EPA/600/A-93/013 ISOLATION AND PURIFICATION OF BACTERIAL DNA FROM SOIL William E. Holben Center for Microbial Ecology and Department of Crop and Soil Sciences Michigan State University This is a preprint of a chapter to be published in "Methods of Soil Analysis" published by the Agronomy Society of America, Inc.; 1992 (in press) ------- ISOLATION AND PURIFICATION OF BACTERIAL DNA FROM SOIL William E. Holben Center for Microbial Ecology and Department of Crop and Soil Sciences Michigan State University ------- INTRODUCTION Recently, new methods for monitoring specific bacterial populations8 in environmental samples have become available. These methods employ the techniques of molecular biology to distinguish, enumerate and monitor individual bacterial populations within a microbial community by the detection of DNA sequences specific to those populations using appropriate molecular probes. DNA-based detection of bacterial populations helps to overcome a major limitation of microbial ecology and soil microbiology; the difficult task of specifically monitoring an individual population of microbes in the environment, and in the presence of the entire microbial community. Such capabilities are essential to understanding the complex interactions between the environment, other microorganisms and the population(s) of interest. Prior to the development of these methods, microbial ecologists generally monitored specific microbial populations using methods that included developing mutant derivatives that could be recovered on selective media (e.g., spontaneous antibiotic resistance), or polyclonal or monoclonal antibodies raised against individual populations that were conjugated to a Quorecent dye to facilitate detection by direct microscopic analysis. DNA-based detection of microbial populations thus represents a new tool to expand the capabilities of investigators to detect and quantify microorganisms in environmental samples. Among the advantages of DNA-based microbial monitoring methods are that a particular DNA sequence is detected directly; thus gene expression is not required. Marker genes and selectable phenotypes are also not required. This is potentially important to microbial ecologists in that it obviates the need to a For the purposes of this chapter, an individual population of bacteria is defined as a group of organisms having identical, or nearly identical, genotype (genetic makeup). ------- demonstrate that genetic manipulations of organisms required for detection by alternate strategies have not compromised the competitiveness of the organism. Thus, DNA-based detection methodologies can be used for monitoring either genetically engineered or wild-type indigenous populations. In fact, very little information about the genetic make-up of the population of interest is required since highly specific probes for detection can be generated by simply subcloning random pieces of DNA from the organism of interest and screening for specificity (Salyers et al., 1983). Alternatively, the probe sequence can be based on regions of the rRNA gene(s) specific to the population of interest which can readily be identified (Barry et al., 1990). Another advantage of DNA-based detection is that bacterial growth is not required for detection allowing non-culturable and non- viable populations to be detected. The importance of this aspect is clear when one considers that typically only about 0.1-1 percent of the bacteria present in a soil sample can readily be cultured under laboratory conditions (Faegri et al., 1977). Having no requirement for culturing also simplifies quantitative and comparative analyses since there is no subsequent increase in the population(s) of interest compared to the other microbial populations in the community and thus relative proportions between populations are maintained. As with any other method for microbial detection, there are limitations to these molecular approaches. Limitations do not preclude the use of this or any other detection strategy, they simply need to be recognized and understood. This will help to avoid ambiguities and potential over-interpretation of data or overestimation of detection capabilities. For example, when using probes for specific functions (e.g., a certain catabolic activity), lack of hybridization signal can only be construed as absence of the sequence used as probe, not absence of the activity. One potentially limiting aspect of DNA-based detection strategies is that ------- protocols for DNA isolation, purification, and subsequent detection and enumeration are relatively sophisticated compared to simpler detection strategies such as culturing on selective media. Relatively few samples (usually 6-24) can be simultaneously processed. This might limit some ecological studies particularly where a large number of variables are to be studied or where statistical analyses are required. The low-end sensitivity of DNA-based detection strategies is relatively poor. Without incorporating additional sophisticated protocols that amplify either the target sequence (e.g., Steffan and Atlas, 1988; Neilson et al.f 1992) or the probe signal, DNA probes can detect about 104 copies of target sequence per gram of soil (Holben et al., 1988). Since there are generally about 109 bacteria in a gram of surface soil, this represents the detection of populations that constitute about 1/100,000 of the total microbial community. This level of detection might be a limitation for some analyses, e.g., risk-assessment for engineered organisms, but certainly suffices for many other kinds of investigations where one is interested in more numerically dominant populations. Recent improvements in DNA isolation protocols and subsequent analyses have made these procedures simpler and more generally useful than as originally published. Two alternate strategies for the isolation of total bacterial community DNA from soil samples will be presented; the first is based on the fractionation of bacteria from soil prior to lysis and the second involves direct lysis of bacteria in the presence of the soil matrix, A comparison of these methodologies is made, and recommendations for the selection of either protocol, depending on sample characteristics and the experimental question being addressed, are given. Other chapters of this volume describe in detail some of the analyses and potential applications possible with bacterial community DNA. For an overview of this emerging DNA-based microbial detection technology, the reader is referred to Holben and Tiedje (1988); Sayler and Layton (1990); and Knight et al. (1992). ------- GENERAL CONSIDERATIONS There are several considerations that will affect the recovery of total bacterial community DNA from the soil environment, regardless of which of the two DNA recovery methods are employed. Biomass The bacterial biomass present in the sample has an impact on the quantity of DNA recovered due to some practical limitations of the methodologies employed. Theoretically, one could recover bacterial DNA from each bacterium present if every important reaction and handling step operated at 100% efficiency. Then, the starting sample size could be adjusted to obtain the desired yield of DNA. This, of course, is not the case. For example, with the direct lysis protocol described here, the starting sample size has been scaled down to 10 g (compared to the original protocol of Qgram et al. [1987], where 100 g samples were used) in order to increase the number of samples that can be processed simultaneously. Using the direct lysis protocol outlined below, 6-10 ng of bacterial community DNA per gram of soil can routinely be obtained for a surface soil (A horizon) that contains about 109 bacteria per gram, for a yield of about 60-100 ug per sample. However, the number of bacteria per gram of soil varies with soil type and depth. At a depth of 1 meter, where microbial populations typically range from 106 to 10? bacteria per gram, one would need to process on the order of 1 kg of soil to obtain a yield of 100 ug of bacterial community DNA. Samples of this size are not readily be processed by the method outlined below. The procedures, as given, are ------- intended for use with samples such as surface soils, sediments, or sludges with total bacterial counts in the range of 108 to 101° bacteria per g of material. Others have developed modifications of the direct lysis protocol in order to recover useable amounts of DNA from samples with low biomass such as aquifer material (S. Thiem, personal communication; Smith and Tiedje, 1992). Organic/Humic content of soils The amount of organie/humic matter in soil has a dramatic effect on the quality (purity) of the DNA obtained, particularly when the direct lysis method is employed. The humic materials present in soil have a similar molecular weight and net charge to DNA and, thus, are readily copurified. The bacterial fractionation procedure which first separates bacteria from the bulk soil prior to cell lysis reduces, but does not eliminate, this problem. Humic contaminants interfere with subsequent enzymatic digestions of DNA (Ogram et al. 1987; Holben et al., 1988; Steflan et al,, 1988), and potentially other enzymatic reactions such as DNA polymerase and ligase. Humic contaminants also confound precise quantitation of the recovered DNA because they exhibit substantial absorbance of light at 260 nm, the measure of which is generally used to quantitate DNA. It is thus preferable to use soils of moderate organic/humic content for experiments involving the isolation of total bacterial community DNA. Although there may be a correspondingly lower biomass associated with such soils, it is usually sufficient to recover usable amounts of DNA from surface soils. For cases in which high organic content soils are used, methods for more precise quantitation of DNA in the presence of humic contaminants are available. One such method, ------- which is relatively simple and requires no sophisticated equipment, is outlined later in this chapter. Clay Content of Soils Adsorption isotherms indicate that relatively large amounts of DNA can bind to pure clays, soils and sediments (Greaves and Wilson, 1969; Ogram et al., 1988). The binding of DNA to clays in soil can have a profound impact on the amount of bacterial community DNA recovered. For example, in comparing DNA recovered from two soils with similar organic content (2.3 and 2.7% respectively), but different clay content (8.1 and 48% respectively), it was found that the yield of DNA from the high clay soil was only about 15-25% of that from the low clay soil despite both soils having similar bacterial viable counts (unpublished observation). The mechanism of binding of DNA to clay is not well understood. Studies with flavomononucleotide binding to smectite implicate the Fe3+ groups of clay and the phosphate groups of the mononucleotide (Mortland, et al., 1984). However, attempts to block DNA binding to clays in soil by competition with excess phosphate, or altering the pH or ionic environment, have been largely unsuccessful (unpublished data). Thus, no method for effectively blocking the DNA binding sites of clays in soil, or for removing adsorbed DNA from clays (and thus enhancing DNA recovery) has yet been described. As was the case with high organic matter soils discussed above, it is best, if possible, to avoid using high clay soils in experiments where bacterial community DNA is to be recovered. ------- 8 BACTERIAL FRACTIONATION METHOD FOR RECOVERY OF BACTERIAL COMMUNITY DNA Principles The bacterial fractionation method involves the separation of bacterial cells from the bulk of the soil prior to cell lysis and recovery of bacterial community DNA. Briefly, soil particles, debris, fungal cells and bacterial cells are brought into suspension by homogenization in the presence of buffer. Soil particles, fungal cells, and other debris are then removed by a low-speed centrifugation step which leaves the unattached bacterial cells in suspension. High-speed centrifugation is then performed to recover the bacterial cells. This combined low-speed, high-speed centrifugation method for the recovery of bacterial cells from soils was pioneered by Faegri et al. (1977) and is termed differential centrifugation. Generally, multiple rounds of homogenization and differential centrifugation are performed on the same soil or sediment sample to enhance the recovery of bacteria. In the protocol described here, the bacterial fraction is lysed using a protocol which combines the salient features of lysis protocols for various groups of bacteria, including the removal of humic contaminants using polyvinylpolypyrrolidone (PVPP), digestion by lysozyme and pronase, and incubation at high temperature (Holben et al., 1988). Following cell lysis, the bacterial DNA is recovered and purified by cesium chloride-ethidium bromide equilibrium density centrifugation and precipitation in ethanol. As described here, the method includes several modifications of the previously published protocol (Holben et al., 1988) including the deletion and combination of steps to result in a shortened protocol that gives comparable yields and purity of DNA. The yield of DNA from 50 g of agricultural surface soil with 2.3% organic matter ------- and 8.1% clay content is in the range of 50-100 ug, corresponding to 1-2 ug per gram of soil. This protocol allows bacterial community DNA to be purifed from six 50 g soil samples to be processed to the point of purified bacterial community DNA in 3-4 days. With slight additional effort, it is possible to process up to 12 samples simultaneously. The bacterial fractionation and cell lysis portion of the protocol (i.e., "day 1" of the procedure) is labor-intensive but the subsequent purification of DNA is largely "hands-ofT time. Advantages An advantage of the bacterial fractionation method is that the DNA recovered from soils, especially high organic content soils, tends to be less contaminated with humic materials than is DNA recovered by direct lysis since the bacteria are removed from the bulk of the soil prior to lysis. If the analysis of the bacterial community DNA isolated from a particular soil requires subsequent digestion with restriction endonucleases and the organic content of the soil is high, isolation of DNA by bacterial fractionation may be required. The DNA recovered by this method has an average size of 50 kb (Holben et al., 1988) compared to DNA recovered by direct lysis which ranges from 30-40 kb in size (unpublished observation). This might be a consideration if the recovered DNA were to be used in experiments attempting to clone DNA fragments from the bacterial community DNA but is not as important when the DNA is to be used in hybridization experiments. The bacterial fractionation procedure recovers DNA only from bacteria (not fungal, protozoan or free DNA) since the bacteria are separated from the soil prior to lysis and DNA recovery. Initially, this appeared to be an important feature of this protocol (Holben et al., 1988; Steffan et al., 1988), but ------- 10 more recently it appears that the direct lysis protocol also recovers primarily bacterial DNA (see below). Originally (Holben et al., 1988), it was thought that the DNA recovered by the bacterial fractionation method was representative of the entire bacterial community based on indirect evidence (Bakken, 1985), but more recent data from this laboratory indicate that more recently grown cells are preferentially recovered from the soil environment (manuscript in preparation). Bacterial fractionation may preferentially recover rapidly growing bacterial cells because they do not adhere as tightly to soil particles. This can be used to advantage if the bacterial population of interest is rapidly growing; providing a fractionation of actively growing cells from those less active, thereby increasing the sensitivity of detection of the desired population. Another advantage of the bacterial fractionation method is that it yields viable cells from the soil bacterial community in concentrated form (Holben et al., 1988) which can be used in other types of experiments requiring live bacteria. The bacterial fractionation protocol, as described here, recovers about 33% of the bacterial cells from sandy loam soil after three rounds of homogenization and differential centrifugation (Holben et al., 1988). Additional rounds of homogenization and centrifugation will yield a diminishing return of bacterial cells for the effort involved, but may be necessary to recover more tightly adhered bacterial cells. Disadvantages Perhaps the main disadvantage of this procedure is that it requires a significant amount of "hands-on" activity and time to process samples through the point of cell lysis (typically 6-8 h for six samples). Although there are no particularly sophisticated procedures or specialized equipment involved, care ------- 11 must be taken in handling samples to minimize DNA loss and maximize reproducibiiity of yield. Due to the amount of handling involved, and the limitations of centrifuge rotor configuration and other logistical considerations, it is usually practical for a single person to process six soil samples simultaneously for bacterial community DNA, although up to 12 samples per day can be accommodated. The bacterial fractionation protocol yields 5-6 times less DNA per gram of soil than does the direct lysis procedure. This can be an important consideration, particularly when the samples have low bacterial biomass. As mentioned above, this procedure appears to preferentially recover DNA from rapidly growing and less tightly adhered bacteria. This phenomenon may confound attempts to quantify bacterial populations unless hybridization data are compared to independant measurements using alternate methodologies (Holben et al., submitted). This selectivity would be a disadvantage for experiments in which the objective is to obtain DNA representing the entire bacterial community, for example to assess the diversity of organisms present in the community that contain a certain gene or other target sequence. DIRECT LYSIS METHOD FOR THE RECOVERY OF TOTAL BACTERIAL COMMUNITY DNA. Principles In the direct lysis method, bacterial cells are lysed directly in the presence of the soil matrix. High temperature, high concentrations of detergent and ------- 12 mechanical disruption using minute glass beads are employed for cell lysis using this method. Direct lysis of bacterial cells in soil for the recovery of total bacterial DNA was pioneered by Ogram et al. (1987) and has since been modified by several groups for simplification, increased sample throughput, or specific applications (Steffan et al., 1988; Hilger et al., 1991; Tsai and Olson, 1992; Smith et al, 1992; this manuscript). As originally described, one or two 100 g soil samples could be processed for DNA recovery over the course of 3-4 days and several DNA concentration/precipitation steps were involved. In the protocol described here, the released DNA is subsequently isolated and purified by cesium chloride- ethidium bromide equilibrium density centrifugation and precipitation in ethanol. The time required to obtain purified DNA is 2-3 days which represents an improvement over the original protocol, is less labor-intensive, and greater numbers of samples (12-24) can be processed simultaneously. Advantages A major advantage of the direct lysis approach is that it is less labor intensive and faster than the bacterial fractionation method. The direct lysis protocol allows one person to readily process 8-12 samples simultaneously, and up to 24 samples with extra effort. The time required from the starting point of sieved soil samples to the initiation of cesium chloride gradient centrifugation is only 2-3 h. The direct lysis procedure results in higher yields of DNA, typically 60-100 jig per 10 g soil sample (6-10 ng pef g of soil). This is particularly important in samples having low biomass such as aquifer material where the ability to recover sufficient amounts of DNA can be the limiting factor to success. Bacterial community DNA recovered by direct lysis seems to better represent the bacterial ------- 13 community than DNA recovered by the bacterial fractionation procedure (manuscript in preparation). In fact, it appears that the direct lysis protocol outlined here approaches quantitative recovery of bacterial DNA since there are about 109 bacteria per gram of soil, each having a genome of about 9 x 10-15 g of DNA, resulting in a calculated quantitative yield of 9 \ig DNA per gram of soil. It is also significant that essentially no intact bacterial cells can be found by microscopy in a soil sample following the lysis protocol. This is an important feature for experiments involving populations that are tightly adhered to particles, not rapidly growing, or when DNA representative of the entire bacterial community is of interest. Disadvantages Bacterial community DNA isolated by the direct lysis procedure is generally more contaminated with humic material than is DNA isolated from the same soil by the bacterial fractionation method. However, DNA purified by direct lysis from soils having moderate levels of humic acids is generally of sufficient purity for most subsequent manipulations involving digestion with restriction enzymes, denaturation, or hybridization. If particularly fastidious reactions, such as DNA amplification using the polymerase chain reaction (PCR), are to be performed, or if DNA isolated using this method is refractory to restriction digestion or other manipulations, further purification (e.g., by additional rounds of purification on cesium chloride-ethidium bromide gradients), or isolation of DNA by bacterial fractionation may be required. DNA isolated by direct lysis tends to be oflower molecular weight (i.e. the randomly sheared DNA fragments are, on the average, smaller) than DNA isolated by bacterial fractionation. Presumably, this reflects ------- 14 the more harsh conditions (i.e. higher temperatures and ionic detergents) and mechanical shearing of DNA imposed by this procedure. The average DNA fragment size is still over 25 kb and thus is suitable for most procedures involving size-fractionation of restriction enzyme-digested DNA, It is worthwhile to assess the size range of DNA obtained by this method since excessive shearing will yield smaller DNA and less satisfactory results in hybridization analyses, or if attempting to clone DNA from the microbial community. Size range can be readily determined by agarose gel electrophoresis with DNA fragments of known size included as standards. As mentioned above and elsewhere (Ogram et al., 1987; Steffan et al., 1988), it was thought that, in addition to bacterial DNA, the direct lysis procedure might recover DNA from fungi, protozoa, and cell-free DNA. Recent evidence suggests that these other potential sources of DNA in soil do not contribute significantly to the DNA obtained. Other investigators have made concerted attempts to obtain fungal DNA from soil samples with little success using the direct lysis method and similar approaches (D. Harris, personal communication). It seems likely that the rigid fungal cell wall and the prevalence of "ghost" fungal hyphae containing no DNA account for the difficulty in isolating DNA from fungi. The population levels of protozoa in typical agricultural surface soils are about 105 per gram compared to 109 to 10*0 bacteria. Thus, even accounting for the larger genome size of protozoa, they could not make a significant contribution to the total amount of DNA obtained. Free (extracellular) DNA in the agricultural soils used in this laboratory, if present, does not appear to be extracted by the direct lysis protocol. This is evidenced by the fact that initial extraction of the soil for DNA prior to lysis does not recover DNA; nor does it reduce the DNA yield obtained by direct lysis compared to soil not previously extracted. In sediment samples, the initial extraction of DNA prior to cell lysis recovered about 1 ug of DNA per g of ------- 15 sediment compared to the recovery of 26 |ig of DNA per g of sediment following cell lysis (Ogram et al., 1987). In summary, the direct lysis procedure is simpler, faster and gives higher yields of DNA that is probably more representative of the total bacterial community present in the soil sample than DNA obtained by the bacterial fractionation method. On the other hand, DNA obtained by bacterial fractionation is of higher purity, larger molecular weight and enriched for rapidly growing (and thus, the most active) populations. The method chosen for use thus depends on the nature of the experimental question, the requirements of the subsequent analyses to be performed with the bacterial community DNA, and the characteristics of the environmental sample. Some recommendations for the appropriate bacterial community DNA recovery method based on experimental goals or soil characteristics are given in Table 1. ------- 16 Table 1. Considerations and recommendations for selection of the appropriate protocol for isolating bacterial community DNA from soil. Consideration low biomass high purity of DNA large number (#) of samples high organic/humic content of samples rapidly growing or loosely adhered orgsc tightly bound orgs DNA best represents community Example aquifer material or nutrient poor soil for PCR reactions multi-parameter or high replication rich soils, forest litter addition of specific source of carbon EPSd producers or trait of organism assess diversity or community-level analyses Protocol DLa BFb DL BF BF DL DL Reason(s) better DNA recovery and low humic matter bacteria removed from soil before lysis faster, larger sample #'s possible bacteria removed from soil before lysis enriches for these orgs; > sensitivity lyses adhered cells probably more representative aDL = Direct Lysis protocol t>BF= Bacterial Fractionation protocol corgs = organisms dEPS = exopolysaccharide ------- 17 PROCEDURES L Bacterial Fraetionation Materials NOTE: The materials list is based on the simultaneous processing of six 50 g soil samples from the stage of sieved soil to the final cesium chloride gradient purification step. The list is based on the items used in this laboratory and does not constitute a commercial endorsement of any supplies or equipment. Reasonable substitutions for particular types of centrifuge rotors, tubes and other materials and equipment that maintain, or reasonably approximate, the specified conditions are appropriate. 1. Six standard Waring blenders with 1.2 1 (40 fi. oz.) glass jars 2. Ice/water bath for each of the blender jars 3 Twelve 250 ml centrifuge bottles (for use with a Sorvall GSA rotor) 4, Sorvall superspeed centrifuge (e.g., model RC5B) with an SS34 (8-place) or SAGOO (12-place) rotor and a GSA rotor 5. Six small paint brushes (to facilitate resuspending bacterial pellets) 6. Twelve 50 ml polycarbonate Oak Ridge tubes 7. Vortex mixer 8. Water bath at 37° C 9. Water bath at 65° C 10, Refractometer (to measure the initial density of the cesium chloride gradient for DNA purification. If a refractometer is not available, density can be determined by measuring the specific gravity of the solution). ------- 18 11. Sorvall ultracentrifuge with TV865B rotor or equivalent 12. Twelve ultracentrifuge tubes for the TV865B rotor Recipes NOTE: The recipes presented here are for reagents required from the stage of sieved soil to the point of the final equilibrium gradient centrifugation step. After this point the steps are common to both DNA isolation protocols and can be found in the section titled: "Fractionation of DNA Gradients, Final Purification and Quantitation of Bacterial Community DNA". 1. 10 X Winogradsky's Salt Solution ( 10 X WS) Provides an isotonic environment for bacterial cells during homogenization and differential centrifugation steps. for 2 liters: •Dissolve 5.0 g of K2HP04 in 800 ml of distilled H20. •Dissolve the following in (a separate) 800 ml of distilled H20: MgS04 • 7 H20 5.0 g NaCl 2.5 g Fe2(S04)3 • H20 50 mg MnSC>4 * 4 H2° 50 •Combine the above, then adjust to pH 6.0 with concentrated HCl. •Bring the final volume to 2 1 with distilled H20. ------- 19 •Before use, dilute 1:10 with distilled H20 and then autoclave. 2. Homogenization solution* This solution provides an isotonic environment for bacterial cells and contains ascorbic acid as a reducing agent to prevent further oxidation (which results in polymerization) of humic compounds in the soil. Contains: 1 X Winogradsky's salt solution 0.2 M sodium ascorbate (added as powder to achieve 0.2 M) This should be prepared just prior to use as the reducing power of the sodium ascorbate lessens with time. NOTE: If the bacterial fractionation protocol is being used to recover viable cells, it is recommended that Winogradsky's salt solution alone be used as the homogenization solution as sodium ascorbate appears to reduce the viability of cells during the fractionation process. 3. Acid-washed Polyvinylpolypyrrolidone (PVPP) This insoluble polymer complexes with humic acids in the homogenization stage removing them from the aqueous phase. The acid treatment of PVPP constitutes a pretreatment which optimizes this interaction. ------- 20 •Prepare 4 1 of 3 M HC1. (Most stock concentrated HCl solutions are 12.1 N so slowly add 992.0 ml of concentrated HCl to 3008 ml of distilled H20 in a 4 1 beaker). •Slowly add 300 g of polyvinylpolypyrrolidone with stirring, cover beaker and stir overnight. •Filter suspension through Miracloth or several layers of cheesecloth (use a large Buchner funnel and a 4 1 vacuum flask). •Resuspend the PVPP in 4 1 of distilled H20, mix for 1 hour and again filter through Miracloth or cheesecloth. •Resuspend the PVPP in 4 1 of 20 mm potassium phosphate buffer (pH 7.4) and mix for 1 to 2 h. Check the pH of the PVPP suspension with pH paper. The desired pH is 7.0. •Repeat filtrations of the suspension and washes in 20 mM phosphate buffer until the PVPP suspension has a pH of 7.0. •Following the final filtration, spread the PVPP on lab paper and let air dry overnight. 4. TE Protects DNA by providing buffered environment with EDTA present to chelate divalent cations which are required for the activity of any nucleases which might be present. ------- 21 Contains: 33 mM Tris, pH 8.0 1 mM EDTA, pH 8.0 for 2 1: •Combine the following in 1 1 of distilled H20: 66 ml of 1 M Tris, pH 8.0 4 ml 0.5 M EDTA, pH 8.0 •bring volume to 2 1, then autoclave. NOTE: The disodium form of EDTA is preferred. At high concentrations EDTA will not go into solution until it approaches the appropriate pH. 5. 5 M sodium chloride (NaCl) Sodium chloride is used during the cell lysis stage as a pretreatment for cells with exopolysaccharide capsules to facilitate access of lysozyme to the cell wall for more efficient lysis. for 500 ml: •Add 146.1 g of NaCl to 400 ml distilled H20 and dissolve with stirring. •Bring the volume to 500 ml, then autoclave. ------- 22 6. 20% Sarkosyl This detergent disrupts the membranes of bacterial cells facilitating the release of DNA into solution during the cell lysis stage. for 100 ml: •Add 20 g of n-laurylsarcosine to 50 ml of distilled H20, mix (slight heating will help the sarkosyl go into solution) •Bring the volume to 100 ml, then autoclave. 7. Tris/sucrose/EDTA This solution provides an appropriate environment for bacterial cells that is buffered both for pH and for osmotic potential and inactivates endogenous nucleases (which degrade DNA) by chelating divalent cations which are required for their activity. The EDTA also serves to disrupt the outer membrane of Gram negative organisms allowing lysozyme freer access to the cell wall. Contains: 50 rnM Tris, pH 8.0 0.75 M Sucrose 10 mM EDTA, pH 8.0 ------- 23 for 250 ml: •Combine the following in 200 ml of distilled H20: 12.5 ml of 1 M Tris, pH 8.0 64.2 g sucrose 5.0 ml of 0.5 M EDTA, pH 8.0 •Bring volume to 250 ml with distilled H20, then autoclave. 8. Lysozyme solution (40 mg/ml) Lysozyme enzymatically attacks the cell wall of bacteria allowing rupture of the cell membrane by detergent and the release of DNA into solution. for 5 ml: •Dissolve 200 nig of lysozyme (grade 1 from chicken egg white [Sigma #L6876]) in 5,0 ml of TE. Prepare on same day and store on ice until use. 9. Pronase E (10 mg/ml) Pronase E comprises a mixture of protein degrading enzymes that facilitate the rupture of bacterial cells in the lysis stage. for 5 ml: •Dissolve 50 mg of pronase (type XXV from Streptomyces griseus [Sigma #P6911]) in 5 ml of TE. Preincubate for 30 min at 37° C prior to use to allow the proteases to inactivate any contaminating nucleases in the mixture. ------- 24 10. Ethidium bromide (10 mg/ml) This DNA-binding dye intercalates into DNA molecules and imposes changes in the buoyant density of DNA causing it to form a discrete band in the cesium chloride equilibrium density gradients that can be fractionated and further purified. for 100 ml: Dissolve 1 g of ethidium bromide in 100 ml of TE. Overnight mixing with a magnetic stirrer may be required. NOTE: ethidium bromide is a potent mutagen and should be handled with care. 11. Cesium chloride balance solution (Rf = 1.3885) This solution is used to bring cesium chloride gradient tubes to final volume and to balance the tubes prior to ultracentrifugation. for approximately 300 ml: •Add 250 g of finely ground cesium chloride (CsCi) to 250 ml of distilled H20 (sterile) and mix by inversion until the CsCl is dissolved. •Add 12.5 ml of 10 mg/ml ethidium bromide and mix. ------- 25 'Check the refractive index (Rf) and adjust as necessary to achieve an Rf value of 1.3885 (this corresponds to a density of 1.58) by adding CsCl to increase the refractive index (density) or H20 to decrease the refractive indexi NOTE: As mentioned above, refractive index is a measure of the density of the solution. In lieu of using a refractometer the investigator can determine the specific gravity of the solution and adjust the density of the solution to 1.58. Procedure NOTE: The following protocol describes the steps involved from the stage of sieved soil to the point of the final equilibrium gradient centrifugation step. After this point, the steps are common to both DNA isolation protocols and can be found in the section titled: "Fractionation of DNA Gradients, Final Purification and Quantitation of Bacterial Community DNA". 1. Combine each 50 g soil sample with 200 ml of homogenization solution and 15 g of acid-washed polyvinylpolypyrrolidone (PVPP) in a blender jar. 2. Homogenize for three 1 min intervals with 1 min cooling in an ice/water bath between homogenizations. ------- 26 3. Pour the homogenate into 250 ml centrifuge bottle and pellet soil, fungi and other debris by centrifugation in a Sorvall GSA rotor at 2,500 rpm (640 x g) for 15minat4°C. 4. Carefully pour the supernatant into a clean 250 ml centrifuge bottle and collect the bacterial fraction by centrifugation in a Sorvall GSA rotor at 12,000 rpm (14,740 x g) for 20 min at 4° C. 5. Add 200 ml of homogenization buffer to the soil pellet and repeat the homogenization and differential centrifugation steps two more times (i.e., repeat steps 2-4 combining the bacterial pellets in step 4). 6. Wash the cells by carefully resuspending the cell pellet in 200 ml of TE using a small, clean paint brush. Collect the bacteria by centrifugation in a Sorvall GSA rotor at 12,000 rpm (14,740 x g) for 20 min at 4° C. f 1. Gently resuspend the cell pellet in 20.0 ml of TE (again using a paint brush), transfer the cell suspension to a 50 ml Oak Ridge tube, then add 5.0 ml of 5 M NaCl and 125 uJ of 20% Sarkosyl and incubate at room temperature for 10 min. 8. Collect the cells by centrifugation in a Sorvall SS34 rotor at 12,000 rpm (11,220 x g) for 20 min at 4° C. 9. Gently resuspend the cell pellet in 3.5 ml of Tris/sucrose/EDTA with a paint brush. ------- 27 10. Add 0.5 ml of lysozyme solution, mix by vortexing then incubate at 37° C for 30 min without shaking. 11. Add 0.5 ml of pronase E, mix by vortexing, then incubate at 37° C for 30 min without shaking. 12. Transfer to a 65° C water bath for 10 min, then add 250 ul of 20% Sarkosyl and incubate at 65° C for 40 min. 13. Transfer to ice and let stand for at least 30 min. 14. Clear the lysate of cellular debris by centrifugation in a Sorvall SS34 rotor at 18,000 rpm (25,260 x g) for 1 h at 4° C. 15. Carefully transfer the supernatant to a clean Oak Ridge tube and" add 9.0 ml of sterile distilled H20, 12.7 g of finely ground cesium chloride and 1.5 ml of ethidium bromide (10 mg/ml). Mix by gentle inversion until the cesium chloride is dissolved and adjust the refractive index to 1.3865-1.3885 (these values correspond to a density range of 1.55-1.58) by adding cesium chloride (to increase the value) or distilled H20 (to decrease the value): 16. Transfer the mixture to an ultracentrifuge tube, fill the remaining volume and balance the tubes using cesium chloride balance solution, then seal the tubes and band the DNA by ultracentrifugation in a Sorvall TV865B rotor at 52,000 rpm (255,800 x g) for 9-16 h at 18° C. ------- 28 17. Fractionate the DNA band with a 5 ml syringe and needle (this procedure is detailed below in the section entitled "Fractionation of DNA Bands from Cesium Chloride Gradients"), transfer the solution to a clean ultracentrifuge tube, fill the remainder of the tube with cesium chloride balance solution and repeat the ultracentrifugation step. This second round of ultracentrifugation results in a substantial increase in purity of the DNA obtained by diluting the contaminants (which are dispersed throughout the gradient) without diluting the DNA (which forms a discrete band in a small volume). 18. Fractionate the DNA band and process through isopropanol extraction, desalting and concentrating DNA by ethanol precipitation, and DNA quantitation as described in the appropriate sections below. n. Direct Lysis Materials NOTE: The materials list is based on the simultaneous processing of eight 10 g soil samples from the stage of sieved soil to the point of the final equilibrium gradient centrifugation step. Larger numbers of samples can be accomodated by either staging the ultracentrifuge runs, or by scaling the protocol to allow the use of other rotors such as the Sorvall T1270 rotor which accommodates twelve 12.5 ml samples, or the Sorvall TFT45.6 rotor which accommodates forty 6.0 ml samples. This list is based on the items used in this laboratory and does not constitute a commercial endorsement of any supplies or equipment. Reasonable substitutions for particular types of centrifuge rotors, tubes and other materials and equipment ------- 29 that maintain, or reasonably approximate, the specified conditions are appropriate. 1. Twenty-four 50 ml polycarbonate Oak Ridge tubes 2. Vortex mixer 3. Water bath at 70° C 4. Glass beads: two sizes are used; 0.7-1.0 mm (Sigma #G9393) and 0.2-0.3 mm (Sigma #G9143) 5. Reciprocal platform shaker 6. Sorvall superspeed centrifuge (e.g., model RC5B) with an SS34 (8-place) rotor or an SAGOO (12-place) rotor 7. Refractometer (to measure the initial density of the cesium chloride gradient for DNA purification. If a refractometer is not available, density can be determined by measuring the specific gravity of the solution). 8. Sorvall ultracentrifuge with TV865B rotor 9. Sixteen ultracentrifuge tubes Recipes NOTE: The recipes presented here are for reagents required from the stage of sieved soil to the point of the final equilibrium gradient centrifugation step. After this point the steps are common to both DNA isolation protocols and can be found in the section titled: "Fractionation of DNA Gradients, Final Purification and Quantitation of Bacterial Community DNA". ------- 30 1. Sodium Phosphate buffer (1 mM at pH 7.0) Buffers the soil suspension during the lysis of bacterial cells. •This solution can be made by combining 2.1 ml of 0,2 M NaH2PO4 and 3.3 ml of 0.2 M Na2HP04 in a total of 11 of distilled H20. 2. Cesium chloride balance solution (Rf = 1.3870) This solution is used to bring cesium chloride gradient tubes to final volume and to balance the tubes prior to ultracentrifugation. for approximately 300 ml: •Add 250 g of finely ground cesium chloride (CsCl) to 250 ml of distilled H20 (sterile) and mix by inversion until the CsCl is dissolved. "Add 12.5 ml of 10 mg/ml ethidium bromide. •Check the refractive index and adjust as necessary to achieve an Rf of 1.3870 (this corresponds to a density of 1.56) by adding CsCl to increase the refractive index (density) or H^O to decrease the refractive index. NOTE: Refractive index is a measure of the density of the solution. In lieu of using a refractometer, the investigator can determine the specific gravity of the solution and adjust the density of the solution to 1.56. ------- 31 Procedure NOTE: This protocol describes the steps involved from the stage of sieved soil to the point of the final equilibrium gradient centrifugation step. After this point the steps are common to both DNA isolation protocols and can be found in the section titled: "Fractionation of DNA Gradients, Final Purification and Quantitation of Bacterial Community DNA". 1. Add 20 ml of NaPC>4(1.0 mM, pH 7.0) and 0.25 g of sodium dodecyl sulfate (SDS) to each 10 g soil sample in a 50 ml Oak Ridge tube, mix by vortexing until thoroughly suspended, then incubate for 30 min at 70° C mixing every 5 minutes. 2. Add 5 g of large glass beads (0.7-1.0 mm) and 5 g of small glass beads (0.2-0.3 mm) and shake for 30 min by placing horizontally on a reciprocal platform shaker at high speed (-100 oscillations/min) at room temperature. 3. Pellet soil and cell debris by centrifugation in a Sorvall SS34 rotor at 10,000 rpm (7,796 x g) for 10 min at 10° C. 4. Transfer the supernatant to a clean Oak Ridge tube and incubate on ice. for 15-30 min to precipitate the SDS. Clear the lysate by centrifugation in a Sorvall SS34 rotor at 10,000 rpm (7,796 x g) for 10 min at 10° C, then carefully transfer the cleared lysate to a clean Oak Ridge tube. ------- 32 5. Adjust the volume of the lysate to 15.5 ml with distilled H20, then add 14.5 g of finely ground cesium chloride. Mix by gentle inversion until the cesium chJoride is totally dissolved, then let stand at room temperature for 10-15 min to precipitate proteins. Clear the lysate by centrifugation at 5,000 rpm (1,949 x g) for 10 min at 10° C. The precipitated proteins will form a floating layer that may appear "foamy"; this layer should be discarded. 6. Transfer the mixture to an ultracentrifuge tube containing 0.65 ml of ethidium bromide (10 mg/ml) and mix by gentle inversion. Fill the remainder of the tube with cesium chloride balance solution (Rf = 1.3870), then balance the tubes, seal and band DNA by centrifugation in a Sorvall TV865B rotor at 52,000 rpm (255,800 x g) at 18° C for 9-16 h. 7. Fractionate the DNA band with a 5 ml syringe and needle (this procedure is detailed below in the section entitled "Fractionation of DNA Bands from Cesium Chloride Gradients"), transfer the solution to a clean ultracentrifuge tube, fill the remainder of the tube with cesium chloride balance solution and repeat the ultracentrifugation step. This second round of ultracentrifugation results in a substantial increase in purity of the DNA obtained by diluting the contaminants (which are dispersed throughout the gradient) without diluting the DNA (which forms a discrete band in a small volume). 8. Fractionate the DNA band and process through isopropanol extraction, desalting and concentrating DNA by ethanol precipitation, and DNA quantitation as described in the appropriate sections below. ------- 33 IE. Fractionation of DNA Gradients, Final Purification and Quantitation of Bacterial Community DNA NOTE: At this stage, the total bacterial community DNA has been extracted from soil and is in aqueous solution. Most of the subsequent protocols and analyses are routine molecular biology protocols with some notable differences described elsewhere in this volume. For further information on routine techniques of molecular biology and/or as an additional resource, the reader is referred to the many molecular biology and cloning laboratory manuals that are available (e.g., Ausubel et al., 1990; Sambrook et al, 1989). ITJ a. Fraetionation of DNA Bands From Cesium Chloride Gradients Materials 1. Syringes (5 ml) fitted with 18 gauge needles 2. Hand-held ultraviolet light source (e.g., Blak-ray model B-100A, VWR Scientific Co.) with UV safety glasses or goggles for eye protection Procedure L Stop the ultracentrifuge and carefully remove the tubes from the rotor. Avoid shaking the tubes as this will perturb the gradients. It is best to let the rotor coast to a stop from 3,000 rpm to zero rather than using the brake which may cause some loss of resolution of the DNA band in the gradient. ------- 2, Extract DNA bands in 1-2 ml volume under ultraviolet illumination using a 5 ml syringe and 18 gauge needle as follows: •Poke a hole at the very top of the ultracentrifuge tube to allow air in. •Insert the needle and syringe just below the visible DNA band with the needle orifice pointed up and extract the DNA band by slowly withdrawing the plunger of the syringe, NOTE: Wear gloves and UV goggles or glasses to protect yourself from the ethidium bromide and UV irradiation. 3. Proceed to isopropanol extraction of ethidium bromide as described below or prepare for second banding as described above. EQ b. Isopropanol Extraction of Ethidium Bromide From DNA Materials 1. Six ml Falcon tubes (capped polypropylene tubes) 2. Thirty ml Corex tubes (glass centrifuge tubes) 3. Sorvall superspeed centrifuge with an SS34 (8-place) or an SA600 (12-place) rotor 4. Capacity for drying under vacuum (e.g., lyopholizer) NOTE: air drying can be substituted for drying under vacuum ------- 35 Recipes 1, Isopropanol saturated with 5 M sodium chloride This is used to remove ethidium bromide from DNA following the ultracentrifugation steps, for approximately 1 1: •Prepare 1 1 of 5 M sodium chloride (NaCl) in a 2 1 bottle and autoclave. •After the 5 M NaCl cools, add 1 1 of isopropanol to the bottle, mix thoroughly and let sit until the organic and aqueous phases separate. There will be some volume loss as the water is mixed with the alcohol. •Add additional isopropanol as necessary until there is some NaCl precipitate present after the phases separate. Procedure 1. Fractionate the DNA band (in 1-2 ml volume) as described in the previous section and transfer to a 6.0 ml Falcon tube. 2. Add an equal volume of isopropanol saturated with 5 M NaCl. 3. Mix by gentle inversion and let sit until the phases separate. ------- 36 4, Pipette oft the top layer (isopropanol) using a Pasteur pipet and discard in an appropriate fashion (the isopropanol will be pink in color and contains ethidium bromide). 5. Repeat steps 2-4 until all pink color is gone and then once more (usually a total of 5 extractions). Proceed to desalting and concentration of DNA as described below. HI c. Desalting and Concentration of DNA Materials 1. Pipetman or equivalent pipettors for small volumes 2. Eppendorf or equivalent microfuge and 1.5 ml microfuge tubes Recipes 1. 3 M Sodium Acetate (NaOAc), pH 5.2 Monovalent cations must be present when precipitating DNA in the presence of alcohol to provide for quantitative recovery of DNA, ------- 37 for 250 ml: •Dissolve 61.52 g of anhydrous NaOAc in 150 ml of distilled H20. •Adjust the pH to 5.2 with glacial acetic acid. •Adjust the volume to 250 ml with distilled H2O, then autoclave. Procedure 1. Following the removal of ethidium bromide transfer the DNA solution to a labelled Corex tube, add two volumes of sterile distilled H20, then add 2 volumes of cold (-20° C) 100% ethanol, cover with parafilm and mix thoroughly by inversion or vortexing. e.g., DNA volume 1.5 ml 2 volumes distilled H20 3.0ml 2 volumes (6 x original DNA volume) ethanol 9.0 ml Incubate overnight at -20° C. NOTE: This first precipitation should not be incubated more than 24 h or the cesium chloride may crystallize out complicating further purification. 2. Pellet the DNA by centrifugation in a Sorvall SS34 (or SAGOO) rotor at 7,500 rpm (4,385 x g) at 4° C for 1 h. Position the tube so that label is toward the outside of the rotor as a reference for the location of the DNA pellet which may not be readily visualized at this stage. ------- 38 3. Discard (pour off) supernatant being careful not to disturb the pellet. Invert the tube on a paper towel and drain dry (5 min), 4. Complete drying under vacuum. Complete air drying may be substituted for vacuum drying. 5. Add 400 ul of sterile distilled H2O, mix by vortexing to dissolve the DNA (it may be helpful to use a Pipetman P1000 to aid in resuspending the DNA pellet by pipetting the 400 ^1 of distilled H20 up and down along sides of tube). 6. Transfer the DNA solution to a labelled 1.5 ml Eppendorf tube. 7. Collect the remaining liquid in the Corex tube by brief centrifugation and transfer to the Eppendorf tube. 8. Add 40 til of 3 M sodium acetate (pH 5.2) and 880 ul of cold (-20° C) ethanol to the tube, mix thoroughly by vortexing and incubate at -20° C for at least I h (DNA may be stored for extended periods in 70% ethanol in the presence of monovalent cations). 9, Collect the DNA by centrifugation in the microfuge for 15-30 min at 4° C. 10. Remove the supernatant with a Pasteur pipette and discard, wash the DNA pellet once with cold (-20° C) 70% ethanol by gentle inversion, centrifuge briefly (2 min), remove the supernatant with a Pasteur pipette and discard, then dry under vacuum. Resuspend in a small volume (usually 100 |il). Proceed to quantitation of DNA as described below. ------- 39 in dL Spectrophotometric Quantitation of DNA Materials 1. Speetrophotometer with UV capabilities and quartz cuvette(s) Procedure The concentration of DNA in the sample can be measured by monitoring the absorbance of a dilute solution of the sample at 260 and 280 nm as follows: 1. Dilute 5 ul of the DNA sample with 995 ul of distilled 2. Measure the absorbance of this solution at 260 and 280 nm. 3, Calculate the concentration of DNA in the sample based on the value of 1.0 Aaeo unit = 50 jig/ml of DNA, and taking into account the 1:200 dilution factor of the sample. 4. Calculate the ^260/^280 ra^io- This ratio indicates the degree of contamination of the DNA with humic (phenolic) compounds and proteins since these molecules exhibit strong absorbance at 280 nm. Pure DNA has a ------- 40 A260/A280 rat»° of 2,0 with a value of 1.7-2.0 indicating relatively pure DNA. DNA solutions can be stored at 4° C but, preferably, at -20° C. NOTE: As mentioned previously, the precise quantitation of bacterial DNA isolated from the soil environment can be problematic due to the copurification of humic contaminants which also absorb light in the UV range. If there is a distinct brownish tinge to the DNA solution, or if the ^2B(^^28Q ratio is low this indicates that there is significant contamination of the DNA with compounds from the soil. If such contaminants are present and precise quantitation is desirable, alternate methods of quantitation must be employed. Perhaps the simplest way to precisely quantitate DNA in the presence of humic contaminants is to measure the UV fluorescence of the DNA in the presence of ethidium bromide. This is readily accomplished using agarose gel electrophoresis by the protocol described in the next section. IH e. Quantitation of DNA by UV Fluorescence in the Presence of Ethidium Bromide NOTE; For this analysis a relatively high agarose concentration of 1.2% is used. This allows the contaminants to migrate significantly far into the gel while the randomly sheared (but generally large) DNA fragments migrate as essentially a single band near the origin. ------- 41 Materials 1. Submarine agarose gel apparatus. There are a wide variety of these available commercially. It is appropriate to obtain one that will also be useful for subsequent analyses of the bacterial community DNA. A gel with minimum dimensions of 15 x 15 cm is recommended to allow sufficient resolution of differently sized DNA fragments and longer gels (e.g., 15 x 25 cm) might be more useful since more than one set of wells can be cast into a single gel as is desirable for this analysis. 2. Power supply for agarose gel electrophoresis 3. Microwave oven or heated stirring plate 4. Access to a camera set-up suitable for photographing gels under ultraviolet illumination such as a transilluminator/Polaroid camera set-up which is basic equipment in most molecular biology laboratories 5. Access to equipment for densitometric analysis of the gel photograph is desirable, as it will allow more precise quantitation, but not essential. Recipes 1. TAB (Tris-acetate-EDTA) Buffer This buffer has appropriate characteristics of pH, buffering capacity and ionic strength which will result in clearly resolved DNA bands in an agarose gel. ------- 42 Contains: 40 mM Tris-acetate 1 mM EDTA for 1 1 of 20 X stock: •Combine the following in 800 ml of distilled H20: 96.8 g Tris-base 22.84 ml glacial acetic acid 40 ml 0.5 M EDTA (pH 8.0) Adjust to pH 8.0, if necessary, using glacial acetic acid, bring to 1 1 final volume with distilled H20 2. 5 X sample loading dye (for agarose gels) This dye allows tracking of the progress of electrophoresis by monitoring the dye front and also makes the DNA samples sufficiently dense to sink to the bottom of the wells in the submarine gel. Contains: 100 mM EDTA 50% glycerol 0.15% bromophenol blue 0.15% xylene cyanole ------- 43 for 10 ml; •Combine the following: 2 ml of 0.5 M EDTA, pH 8.0 5.0 ml of 100% glycerol 0.75 ml of 2% bromophenol blue 0.75 ml of 2% xylene cyanole 1.5 ml of distilled H20 Procedure 1. Combine an appropriate volume of 1 X TAB buffer with an appropriate amount of agarose in an Ehrlenmeyer flask (these values are determined based on the gel dimensions and the desired percentage of agarose; 1.2% for this analysis). 2. Swirl the flask to evenly distribute the agarose. 3. Heat the solution until the agarose is completely dissolved; undissolved agarose will appear as flecks in an otherwise clear solution. If using a microwave, heat at high power for 2 min or until the mixture bubbles. Remove the flask from oven (before it boils over), carefully swirl again, and reheat until all of the agarose goes into solution. 4. Place the flask containing the molten agarose in a 55-65° C water bath or on the benchtop to cool. The gel should be poured when the temperature of the solution is 55-65° C (almost too hot to hold). ------- 44 5, Prepare the gel apparatus for casting the gel while the agarose is cooling. There are several different types of gel boxes and these preparations will depend on the particular one you are using. 6. Just prior to pouring the gel, add ethidium bromide to a final concentration of 0.5 ug/ml to the dissolved agarose and swirl to mix (for agarose gels it is convenient to have a 1 mg/ml stock solution of ethidium bromide which can be made by dilution from the 10 mg/ml stock described above). 7. Pour the agarose solution into the gel casting tray and adjust the well- forming comb(s) to keep the wells properly aligned. Allow the agarose to cool and solidify (-20-30 min) prior to use. 8. To prepare gel for running: •Fill the electrophoresis tank (apparatus) with buffer solution (IX TAB containing 0.5 (ig/mJ ethidium bromide) and place the gel (still in the casting tray) on the tank platform. The buffer must cover the gel by 1-2 mm. •Carefully (to avoid breaking the walls of the wells) remove the comb. ------- 45 9. To prepare samples for loading: •In a microfuge tube bring ~1 ug of total bacterial community DNA solution (as determined spectrophotometrically) to a total volume of 20 ul with distilled H20. Add 5.0 ul of 5 X sample dye to the sample and mix. •A set of DNA standards should be prepared by serial dilution of a known amount of ultrapure DNA (an appropriate source would be to purchase undigested phage lambda DNA commercially). The dilution range should be from 3.0 ug to 0.1 ug in 20 ul volume since the concentration of humic-contaminated DNA is generally overestimated. Add 5.0 ul of 5 X sample dye to each sample and mix. 10. Load the samples and standards into the gel wells using the Pipetman pipettor. Stick the tip below the surface of the buffer but above the well bottom, and dispense the sample slowly. The sample will sink through the buffer and settle in the well. It is recommended that the DNA samples and standards be run near each other in the same gel for more precise quantitation. An appropriate way to accomplish this is to cast two sets of wells into the gel; the upper one (nearer the origin) for the DNA standard dilution series and the lower for the DNA samples of unknown concentration. 11. After the gel has been loaded, gently place the cover on the apparatus and hook up the power leads. DNA is negatively charged and will migrate toward the positive (red lead and jack in power supply) electrode. Adjust the power to 50 volts (constant voltage). Run the gel until the leading dye front ------- 46 (bromophenol blue) has migrated two-thirds the length of the gel or two- thirds of the way to the second set of wells. 12. Photograph the gel under ultraviolet illumination either from a transilluminator or by even distribution of UV illumination from a hand- held source. 13. Determine the concentration of the DNA in the original sample by comparison to the known standards using a densitometer or by visual examination. The DNA will fluoresce bright orange and be found relatively near the origin of the gel. The humic contaminants, if significant amounts are present, will fluoresce blue-green and should migrate well ahead of the DNA in the agarose gel. ACKNOWLEDGEMENTS The author's work has been supported by U.S. Environmental Protection Agency Agreement CR 814575 and National Science Foundation Science and Technology Grant No. DIR 8809640. Although the research described in this article has been funded in part by the EPA, it has not been subjected to the Agency's review and therefore does not necessarily reflect the views of the Agency, and no official endorsement should be inferred. The author gratefully acknowledges the technical support provided by Bernard M. Schroeter and Robert A. Laymen. ------- 47 BIBLIOGRAPHY Ausubel, P.M., R. Brent, R.E. Kingston, D.D. Moore, J.G. Seidman, J.A. Smith, and K. Struhl. 1990. Current protocols in molecular biology, Vol. 2, Greene Publishing Assoc. and Wiley-Interscience, New York, New York. Bakken, L.R. 1985. Separation and purification of bacteria from soil. Appl. Environ. Microbiol. 49:1482-1487. Barry, T., R. Powell, and F. Gannon. 1990. A general method to generate DNA probes for microorganisms. Bio/Tech. 8:233-236. Faegri, A., V.L. Torsvik, J. Goksoyr. 1977. Bacterial and fungal activities in soil: separation of bacteria and fungi by a rapid fractionated centrifugation technique. Soil Biol. Biochem. 9:105-112. Greaves, M.P., and M.J. Wilson. 1969. The adsorption of nucleic acids by montmorillonite. Soil Biol. Biochem. 1:317-323. Hilger, A.B., and D.D. Myrold. 1991. Method for extraction of Frankia DNA from soil, p. 107-113. In D.A. Crossley Jr., D.C. Coleman, P.F. Hendrix, W. Cheng, D.H. Wright, M.H. Beare and C.A. Edwards (eds.), Modern techniques in soil ecology. Elsevier Science Publishing Co., New York, New York. Holben, W.E., B.M. Schroeter, V.G.M. Calabrese, R.H. Olsen, J.K. Kukor, V.O. Biederbeck, A.E. Smith and J.M. Tiedje. 1992. Analysis by gene probes of soil ------- 48 microbial communities selected by treatment with 2,4-dichIorophenoxyacetic acid (2,4-D). Appl. Environ. Microbiol. (submitted). Holben, W.E., and J.M. Tiedje. 1988. Applications of nucleic acid hybridization in microbial ecology. Ecology 69:561-568. Holben, W.E., J.K. Jansson, B.K. Chelm, and J.M. Tiedje. 1988. DNA probe method for the detection of specific microorganisms in the soil bacterial community. Appl. Environ. Microbiol. 54:703-711. Knight, I.T., W.E. Holben, J.M. Tiedje, and R.R. Colwell. 1992. Nucleic acid hybridization techniques for detection, identification, and enumeration of microorganisms in the environment, p. 65-91. In M.A. Levin, R.J. Seidler, and M. Rogul (eds.), Microbial ecology: principles, methods, and applications. McGraw-Hill, Inc., New York, New York. Mortland, M.M., J.G. Lawless, H.Hartman, and R. Frankel. 1984. Smectite interactions with flavomononucleotide. Clays and Clay Minerals 32:279-282. Neilson, J.W., K.L. Josephson, S.D. Pillai, and I.L. Pepper. 1992, Polymerase chain reaction and gene probe detection of the 2,4-dielorophenoxyacetic acid degradation plasmid, pJP4. Appl. Environ. Microbiol., 58:1271-1275. Ogram, A., G.S. Sayler, D. Gustin, and R.J. Lewis. 1988, DNA adsorption to soils and sediments. Environ. Set Technol. 22:982-984. ------- 49 Ogram, A., G.S. Sayler, and T. Barkay. 1987. The extraction and purification of microbial DNA from sediments. J. Microbiol. Methods 7:57-66. Salyers, A.A., S,P. Lynn, and J.F. Gardner. 1983. Use of randomly cloned DNA fragments for identification of Bacteroides thetaiotaomicron. J. Bacteriol. 154:287-293. Sambrook, J., E.F. Fritsch, and T. Maniatis. 1989. Molecular cloning, a laboratory manual, 2nd ed., Cold Spring Harbor Laboratory Press, Cold Spring Harbor, New York. Sayler, G.S., and A.C. Layton. 1990. Environmental application of nucleic acid hybridization, p. 625-648. In L.N. Ornston, A. Balows, E.P. Greenberg (eds.), Annual review of microbiology. Annual Reviews, Inc., Palo Alto, California. Smith, G.B., and J.M. Tiedje. 1992. Isolation and characterization of a nitrite reductase gene and its use as a probe for denitrifying bacteria. Appl. Environ. Microbiol. 58:376-384. Steffan, R.J., J. Goks0yr, A.K. Bej, and R.M. Atlas. 1988. Recovery of DNA from soils and sediments. Appl. Environ. Microbiol. 54:2908-2915. Steffan, R.J., and R.M. Atlas. 1988. DNA amplification to enhance detection of genetically engineered bacteria in environmental samples. Appl. Environ. Microbiol. 54:2185-2191. ------- 50 Tsai, Y-L, and B.H. Olson. 1991. Rapid method for direct extraction of DNA from soil and sediments. Appl. Environ. Microbiol. 57:1070-1074. ------- _ TECHNICAL REPORT UATA (ftcfftt ntd Imttruttions on tht nvtnt it/art eomptei i. REPORT NO. EPA/600/A-.93/013 2. 4. TITLE AND SUStlTLE Isolation and purification of bacterial DNA from soil PATE I. PERPORMINB ORBANIZATION CODE 7. AVTHOMS) William E. Holben , PERFORMING ORBANIEATiON REPORT NO. ORGANIZATION NAMI AND ADDRUC tO. PROORAM ELEMENT NO. Michigan State Univ. , East Lans ing , MI Tl. CONTRACT/BRANT NO, 13. SPONSORING AGENC* NAMI AND ADDRESS US Environmental Protection Agency Environmental Research Laboratory 200 SW 35th Street Corvallis, OR 97333 11. TVfi Of HtfJDftT AND PIMIOD COVERED Book Chapter i«. SPONSORING AOENCV CODE EPA/600/02 16.SUFPLSMENTA*Y NOTEfS 1992 Chapter in: Methods of Soil Analysis Society of America) (pub. Agronomy Recently, new methods for monitoring specific bacterial populations in environmental samples have become available. These methods employ the techniques of molecular biology to distinguish, enumerate and monitor individual bacterial populations within a microbial community by the detection of DNA sequences specific to those populations using appropriate molecular probes. DNA-based detection of bacterial populations helps to overcome a major limitation of microbial ecology and soil microbiology; the difficult task of specifically monitoring an individual population of microbes in the environment, and in the presence of the entire microbial community. Such capabilities are essential to understanding the complex interactions between the environment, other microorganisms and the population(s) of interest^-— DNA-based detection of microbial populations thus represents a new tool to expand the capabilities of investigators to detect and quantify microorganisms in environmental samples. KEY WORDS AND DOCUMENT ANALYSIS MsemrroRS fc.!DENTiFtEMft/OPEN ENDED TERM* C. COfATI F*ld/Gl0up DNA, monitoring, bacterial populations, I. DISTMlSI/TiON STATEMENT Release to Public . nclassifie It. NO. OF PACES 51 B SECURITY CLASS (TMtmttl Unclassified 33. PRICE •PA uae-i c»-»i) ------- |