United States
Environmental Protection
Agency
&EPA
Toxic Substances
BROAD SCAN ANALYSIS OF
NATIONAL HUMAN
SPECIMENS
VOLUME I - EXECUTIVE SUMMARY
THE FY82
TISSUE SURVEY
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New
England
West North
Central
West South Certra!
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BROAD SCAN ANALYSIS OF HUMAN ADIPOSE TISSUE:
VOLUME 1: EXECUTIVE SUMMARY
by
John S. Stanley
FINAL REPORT
EPA Contract No. 68-02-4252
Work Assignment No. 21
MRI Project No. 8821-A01
December 31, 1986
Prepared For:
National Human Monitoring Program
Field Studies Branch (TS-798)
Design and Development Branch
Office of Toxic Substances
U.S. Environmental Protection Agency
401 M Street, S.W.
Washington, DC 20460
Attn: Ms. Janet Remmers and Mr. Philip Robinson, Work Assignment Managers
Dr. Joseph J. Breen and Ms. Cindy Stroup, Program Managers
U.S. Environmental Protection Agency
Region V, Library
230 South Dearborn Street
Chicago, Winois 60604
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DISCLAIMER
This document has been reviewed and approved for publication by the
Office of Toxic Substances, Office of Pesticides and Toxic Substances, U.S.
Environmental Protection Agency. The use of trade names or commercial
products does not constitute Agency endorsement or recommendation for use.
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PREFACE
This executive summary is the first of a five-volume series that
details the broad scan chemical analysis of composite adipose tissue samples.
These composite samples were prepared from individual specimens obtained from
the Environmental Protection Agency's (EPA) National Human Adipose Tissue
Survey (NHATS) fiscal year 1982 (FY82) repository.
This first volume summarizes data generated from all analysis efforts.
Volumes II through V deal specifically with the chemical analysis of the NHATS
composites. The statistical analyses of the data reported in these volumes
will be reported separately by the EPA's Office of Toxic Substances (OTS)
Design and Development Branch contractor, Battelle Columbus Laboratories.
The entire series of reports are referenced as follows:
Stanley JS. 1986. Broad scan analysis of human adipose tissue:
Volume I: Executive summary. EPA 560/5-86-035.
Stanley JS. 1986. Broad scan analysis of human adipose tissue:
Volume II: Volatile organic compounds. EPA 560/5-86-036.
Stanley JS. 1986. Broad scan analysis of human adipose tissue:
Volume III: Semi volatile organic compounds. EPA 560/5-86-037.
Stanley JS. 1986. Broad scan analysis of human adipose tissue:
Volume IV: Polychlorinated dibenzo-p_-dioxins (PCDDs) and polychlori-
nated dibenzofurans (PCDFs) EPA 560/5-86-038.
Stanley JS, Stockton RA. 1986. Broad scan analysis of human adipose
tissue: Volume V: Trace elements. EPA 560/5-86-039.
These method development, sample analyses, and reporting activities
were completed for the EPA/OTS Field Studies Branch (FSB) broad scan analysis
of human adipose tissue program (EPA Prime Contract Nos. 68-02-3938 and 68-02-
4252, Work Assignments 8 and 21, respectively, Ms. Janet Remmers, Work Assign-
ment Manager, and Dr. Joseph Breen, Project Officer).
The samples were prepared with the assistance of Ms. Leslie Moody
and Mr. Steven Turner. The HRGC/MS methods development and sample analyses
were conducted by Mr. Steven Turner, Ms. Kathy Boggess, Mr. John Onstot, and
Dr. Thomas Sack. The compositing scheme used to prepare the samples from the
NHATS repository was provided by Dr. Gregory Mack, Battelle Columbus Labora-
tories, under contract to the EPA/OTS Design and Development Branch (Mr. Philip
Robinson, Task Manager, and Ms. Cindy Stroup, Program Manager).
MIDWEST RESEARCH, INSTITUTE
/"ป'
aul C. Consl
Program Manager
Jojfn E. Going iii
Director
Chemical Sciences Department
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TABLE OF CONTENTS
Page
I. Introduction 1
A. Broad Scan Analysis Strategy 1
B. Work Assignment Objectives 1
II. Project Summary 2
A. Collection and Storage of NHATS Specimens 2
B. Volatile Organic Compounds 3
C. Semivolatile Organic Compounds 4
D. PCDD and PCDF 16
E. Trace Elements 24
III. Recommendations 27
A. Volatile Organic Compounds 27
B. Semivolatile Organic Compounds 27
C. PCDD and PCDF 28
D. Trace Elements 29
IV. References 30
Appendix A - Glossary of Terms 31
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LIST OF TABLES
Table Page
1 Incidence of Detection of Target Volatile Organic
Compounds in the NHATS FY82 Composite Specimens 5
2 Incidence of Detection of Volatile Organic Compounds
in Composited Human Adipose Tissue from the
Northeast Census Region 6
3 Incidence of Detection of Volatile Organic Compounds
in Composited Human Adipose Tissue from the
South Census Region 7
4 Incidence of Detection of Volatile Organic Compounds
in Composited Human Adipose Tissue from the
North Central Census Region 8
5 Incidence of Detection of Volatile Organic Compounds
in Composited Human Adipose Tissue from the
West Census Region 9
6 Incidence of Detection of Target Semi volatile Organic
Compounds in the NHATS FY82 Composite Specimens 11
7 Incidence of Detection of Semi volatile Organic Compounds
Determined in Composited Human Adipose Tissue from
the West Census Region 12
8 Incidence of Detection of Semi volatile Organic Compounds
Determined in Composited Human Adipose Tissue from
the Northeast Census Region 13
9 Incidence of Detection of Semi volatile Organic Compounds
Determined in Composited Human Adipose Tissue from
the North Central Census Region 14
10 Incidence of Detection of Semivolatile Organic Compounds
Determined in Composited Human Adipose Tissue from
the South Census Region 15
11 Lipid-Adjusted Concentration of PCDD and PCDF in
the NHATS FY82 Composite Specimens 17
12 PCDD and PCDF Detected in the NHATS FY82 Composite
Specimens from the Northeast Census Region 18
13 PCDD and PCDF Detected in the NHATS FY82 Composite
Specimens from the West Census Region 19
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LIST OF TABLES (concluded)
Table Page
14 PCDD and PCDF Detected in the NHATS FY82 Composite
Specimens from the South Census Region 20
15 PCDD and PCDF Detected in the NHATS FY82 Composite
Specimens from the North Central Census Region 21
16 Concentration (M9/g) for Trace Elements in Adipose
Tissue Determined by ICP-AES Analysis 25
17 Summary of Data for Trace Elements (ng/g) Identified in
Nine Human Adipose Tissue Specimens by NAA 26
vn
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LIST OF FIGURES
Figure Page
1 Flow scheme for analysis of semivolatile organic
compounds in human adipose tissue 10
2 PCDD and PCDF distribution in the general U.S.
population by age group 22
3 Comparison of PCDD and PCDF concentration (based on
wet tissue weight) profiles for Sweden, the general
U.S. population, and upstate New York 23
vm
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I. INTRODUCTION
The U.S. Environmental Protection Agency's Office of Toxic Substances
(EPA/OTS) maintains through the National Human Adipose Tissue Survey (NHATS) a
unique program for estimating the general population exposure to toxic organic
chemicals. NHATS is the main operative program of the National Human Monitor-
ing Program (NHMP). The NHMP was first established by the U.S. Public Health
Service in 1967, and was subsequently transferred to EPA in 1970. During 1979
the program was transferred within EPA to the Exposure Evaluation Division of
OTS.
NHATS is an annual program to collect and chemically analyze a na-
tionwide sample of adipose tissue specimens for the presence of toxic compounds.
The objective of the program is to detect and quantify the prevalences of toxic
compounds in the general population. The specimens are collected from autopsied
cadavers and surgical patients according to a statistical survey design (Lucas
1981). The design ensures that specified geographic regions and demographic
categories are appropriately represented to permit valid and precise estimates
of baseline levels, time trends, and comparisons across subpopulations.
The NHATS data are used to address part of OTS's mandate under the
Toxic Substances Control Act (TSCA) to assess chemical risk to the U.S. popu-
lation. Historically, organochlorine compounds and polychlorinated biphenyls
(PCBs) have been selected for evaluation.
A. Broad Scan Analysis Strategy
EPA/OTS has developed an aggressive strategy to expand the use of
the NHATS program so as to provide a more comprehensive assessment of TSCA-
related substances that persist in the adipose tissue of the general U.S.
population. The NHATS specimens collected during fiscal year 1982 (FY82) were
selected for a broad scan analysis of volatile and semi volatile organic TSCA-
related chemicals and trace elements (Mack and Stanley 1984).
The initiative to achieve a more comprehensive assessment necessi-
tated either the development of new methods or the modification of the exist-
ing analytical procedures. Data reported on NHATS specimens up to the FY82
collection are limited to organochlorine pesticides and PCBs based on packed
column gas chromatography/electron capture detector (PGC/ECD) analysis.
B. Work Assignment Objectives
The objectives of this work assignment were (1) to identify appro-
priate analytical methods for a broad scan analysis of human adipose tissue
based on high resolution gas chromatography/mass spectrometry (HRGC/MS) detec-
tion for general semivolatile and volatile organic compounds and multielemental
techniques [neutron activation analysis (NAA) and inductively coupled emission
spectrometry (ICP-AES)] for toxic trace elements; (2) to conduct preliminary
evaluation of the analytical procedures; (3) to complete the sample workup
and HRGC/MS analysis of 46 composite samples prepared from the NHATS specimens
collected during FY82 (the target detection range for analytes by the HRGC/MS
as specified in the current NHATS strategy (Mack and Stanley 1984) was 0.05
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to 0.10 ug/g); and (4) to compare the data generated by the two multielemental
techniques through the analysis of nine individual NHATS specimens.
The broad scan analysis approach is necessary to identify additional
compounds or toxic trace elements that may be of concern to EPA under the man-
dates of TSCA. The multielemental analysis techniques were included as screen-
ing procedures to provide information on toxic trace elements that persist in
human adipose tissue.
A summary of the results that were generated from the FY82 NHATS
project is given in Section II. Recommendations for additional methods devel-
opment are presented in Section III. Appendix A provides a glossary of the
terms used throughout this text.
II. PROJECT SUMMARY
The broad scan analysis task has resulted in the development and
preliminary evaluation of HRGC/MS methods for the measurement of volatile and
semivolatile organic compounds at concentrations ranging from 0.001 to 2 ug/g
in human adipose tissues. Procedures based on selected ion monitoring (SIM)
techniques have provided qualitative analysis for complex analytes such as
toxaphene. The sensitivity of the SIM technique has also been applied to the
determination of parts per trillion (picogram/gram) quantities of specific
polychlorinated dibenzo-p_-dioxin (PCDD) and dibenzofuran (PCDF) congeners.
Two multielement analysis techniques were evaluated to determine the levels
of toxic trace elements in adipose tissue.
The results of this broad scan analysis activity have been presented
in part at the American Chemical Society Symposium on "Exposure Measurement
and Evaluation of Methods for Epidemiology Studies," Chicago, IL, September
1985; the Fifth International Dioxin Symposium in Bayreuth, FRG, September
1985 (Stanley et al. 1986); 13th Annual Federation of Analytical Chemistry
and Spectroscopy Society Symposium on "Application of Mass Spectrometry in
Trace Analysis," St. Louis, MO, in October 1986.
In addition to these reports and presentations, a detailed method
protocol for the determination of specific semivolatile organic compounds in
human adipose tissue was prepared and submitted for peer review (Stanley 1985).
This analytical method is undergoing additional validation for implementation
into the NHATS program for routine analysis.
The results of the method development and sample analysis activi-
ties are reported in four separate reports dealing specifically with volatile
(Stanley 1986a), and semivolatile organics (Stanley 1986b), PCDDs and PCDFs
(Stanley 1986c), and trace elements (Stanley and Stockton 1986). A synopsis
of the results based on each analysis effort is presented.
A. Collection and Storage of NHATS Specimens
The adipose tissue specimens were originally collected during FY82
(October 1, 1981, through September 30, 1982) for determination of organo-
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chlorine pesticide and PCB residues. The specimens were collected during
surgical procedures or as part of postmortem examinations. The cooperating
physicians and pathologists were requested to acquire at least 5 g of high
lipid adipose (subcutaneous, perirenal, or mesenteric), taking precautions to
avoid contamination that might result in direct contamination from chemicals
such as solvents, paraffin, disinfectants, preservatives, or plastics. The
cooperators were given no specific instructions to avoid potential contamina-
tion that might arise from background contribution (airborne levels) of sol-
vents or metals.
The adipose tissue specimens were sealed in glass jars and frozen
(-20ฐC) following collection. The specimens were shipped in insulated coolers
packed in dry ice. The FY82 specimens were originally received and stored at
EPA's Toxicant Analysis Center at Bay St. Louis, MS. The NHATS repository
was transferred to Midwest Research Institute (MRI) during September 1982.
The specimens were shipped in insulated coolers and packed on dry ice. The
specimens were inventoried at MRI upon receipt and were then stored in freezers
(-20ฐC). Precautions were taken to ensure that the specimens remained frozen
during all inventory and sample handling procedures. The procedures for prepa-
ration of the composite specimens are presented in detail in the report that
focuses on the volatile organic analyses (Stanley 1986a).
B. Volatile Organic Compounds
An analytical method based on a heated dynamic headspace purge and
trap technique was developed to sample volatile organic compounds from human
adipose tissue. The volatile organic compounds were separated and detected
using HRGC/MS. HRGC was selected to achieve the best possible separation of
volatile components. MS was selected as a detector to provide the necessary
specificity to positively detect the volatile compounds present in adipose
tissue. Target analytes were quantitated based on a multiple internal stan-
dard technique. The method evaluation studies and daily quality control
checks demonstrated that method accuracy was improved for analytes that had a
corresponding deuterated analog as an internal quantitation standard.
Forty-six composite samples were prepared from the FY82 NHATS reposi-
tory according to a study design prepared by the EPA/OTS Design and Development
Branch contractor, Battelle Columbus Laboratories. The composite samples rep-
resent the nine U.S. census divisions stratified by three age groups (0-14,
15-44, and 45 plus).
The HRGC/MS analysis of the volatile compounds purged from the human
adipose demonstrated a complex mixture of compounds consisting primarily of
aldehydes, ketones, hydrocarbons, and carboxylic acid esters. Additional com-
pounds that are classified as aromatic, halogenated aliphatic, and halogenated
aromatic compounds were detected as minor constituents.
Quantitative data were determined for 17 specific compounds. The
predominant target analytes that were noted in this study included chloroform,
1,1,1-trichloroethane, benzene, tetrachloroethene, toluene, chlorobenzene,
ethylbenzene, styrene, 1,1,2,2-tetrachloroethane, 1,4-dichlorobenzene, 1,2-
dichlorobenzene, xylenes, and ethylphenol.
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Several compounds, including styrene, the xylene isomers, 1,4-dichlo-
robenzene, and ethylphenol, were detected in all composite samples. Table 1
presents the incidence of detection for the selected target analytes and the
range of concentrations observed. Qualitative summaries of the incidence of
detection based on age group and census division are presented in Tables 2
through 5.
The quantitative data for the 17 target analytes have been submitted
along with all supporting quality control data to Battelle Columbus Division
for statistical analysis. Characterization of additional chromatographic
peaks in the HRGC/MS data to identify other compounds of interest to EPA has
been initiated under a separate work assignment (Contract No. 68-02-4252, Work
Assignment No. 23).
C. Semi volatile Organic Compounds
An analytical method for the broad scan analysis of human adipose
tissue for semivolatile organic compounds was identified and evaluated. The
analytical method is based on gel permeation chromatography (GPC), Florisil
fractionation, and HRGC/MS. Figure 1 is a schematic of the sample preparation
and analysis procedures.
Forty-six composite specimens were prepared from the FY82 NHATS re-
pository according to a study design provided by Battelle Columbus Division,
the EPA Design and Development Branch contractor. The composite specimens
represent the nine U.S. census divisions stratified by three age groups (0-14,
15-44, and 45 plus).
Quantitative data for organochlorine pesticides, PCBs, chlorobenzenes,
phthalate esters, phosphate triesters, and polynuclear aromatic hydrocarbons
were determined for each composite. Table 6 summarizes the incidence of detec-
tion of selected semivolatile organic compounds and the range of concentrations
measured based on extractable lipid content. Tables 7 through 10 qualitatively
demonstrate the incidence of observation based on census divisions and age
group. The feasibility of determining other halogenated aromatic compounds,
including polybrominated biphenyls, polychlorinated terphenyls, and polychlo-
rinated diphenyl ethers, using this method was demonstrated through the analy-
sis of spiked adipose tissue samples.
The samples representing the 45-plus age category were also analyzed
for toxaphene (a complex mixture of polychloroterpenes) by HRGC/MS-SIM. Toxa-
phene was qualitatively identified in 12 of the 14 samples analyzed. Quanti-
tation of toxaphene was not achieved due to the complexity of the response but
was estimated to be less than 0.10 ug/g.
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Table 1. Incidence of Detection of Target Volatile Organic
Compounds in the NHATS FY82 Composite Specimens
Wet tissue
Frequency of concentration
Compound observation (%) (ng/g)
Chloroform
1,1,1-Trichloroethane
Bromodi chl oromethane
Benzene
Tetrachl oroethene
Di bromochl oromethane
1,1,2-Trichloroethane
Toluene
Chlorobenzene
Ethyl benzene
Bromoform
Styrene
1,1,2, 2-Tetrachl oroethane
1 , 2-Di chl orobenzene
1,4-Di chlorobenzene
Xylene0
Ethylphenol
76
48
0
96
61
0
0
91
96
96
0
100
9
63
100
100
100
ND (2)a -
ND (17) -
ND (21)
ND (4) -
ND (3) -
ND (1)
ND (1)
ND (1) -
ND (1) -
ND (2) -
ND (1)
8-350
ND (1) -
ND (0.1)
12-500
18-1,400
0.4-400
580
830
97
94
250
9
280
8
- 2
ND = not detected. Value in parentheses is the estimated limit
, of detection.
The exact isomers were not determined.
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Table 2. Incidence of Detection of Volatile Organic Compounds
in Composited Human Adipose Tissue from
the Northeast Census Region
Census division:
Age group:
Compound
New England
Middle Atlantic
0-14
15-44
45+
0-14
15-44
45+
Chloroform
1,1,1-Trichloroethane
Bromodi chloromethane
Benzene
Tetrachloroethene
Di bromochloromethane
1,1,2-Trichloroethane
Toluene
Chlorobenzene
Ethyl benzene
Bromoform
Styrene
1,1,2,2-Tetrachloroethane
1,2-Dichlorobenzene
1,4-Dichlorobenzene
Xylene3
Ethylphenol
Note: A positive (+) value indicates the compound was detected at a
trace (response greater than 2.5 times S/N but less than 10 times S/N)
or positive quantifiable level (response greater than 10 times S/N).
A negative (-) value indicates the compound was not detected (response
less than 2.5 times S/N). The number of symbols for each age group
indicates the number of composites analyzed.
aThe exact isomers were not determined.
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Table 3. Incidence of Detection of Volatile Organic Compounds
in Composited Human Adipose Tissue from
the South Census Region
Census division:
\ge group:
Compound
South Atlantic
0-14 15-44 45+
East South Central West South Central
0-14 15-44 45+ 0-14 15-44 45+
:hloroform
1,1,1-Trichloroethane
3romodichloromethane
Benzene
Fetrachl oroethene
Dibromochloromethane
1,1,2-Trichloroethane
Toluene
3hlorobenzene
Ethyl benzene
Bromoform
Styrene
1,1,2,2-Tetrachloroethane
1,2-Dichlorobenzene
1,4-Dichlorobenzene
Xylene3
Ethyl phenol
-+ +++- +++- +
++ ++++ ++++ +
-+ -+--
++ ++++ ++++ +
++ ++++ ++++ +
Note: A positive (+) value indicates the compound was detected at a trace (response
greater than 2.5 times S/N but less than 10 times S/N) or positive quantifiable level
(response greater than 10 times S/N). A negative (-) value indicates the compound was
not detected (response less than 2.5 times S/N). The number of symbols for each age
group indicates the number of composites analyzed.
The exact isomers were not determined.
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Table 4. Incidence of Detection of Volatile Organic Compounds
in Composited Human Adipose Tissue from
the North Central Census Region
Census division: East North Central West North Central
Age group: 0-14 15-44 45+ 0-14 15-44 45+
Compound
Chloroform ++
1,1,1-Trichloroethane
Bromodichloromethane
Benzene ++
Tetrachloroethene +-
Dibromochloromethane
1,1,2-Trichloroethane
Toluene ++
Chlorobenzene ++
Ethyl benzene ++
Bromoform
Styrene ++
1,1,2,2-Tetrachloroethane
1,2-Dichlorobenzene ++
1,4-Dichlorobenzene ++
Xylene3 ++
Ethyl phenol ++ +++ +++ + + ++
Note: A positive (+) value indicates the compound was detected at a
trace (response greater than 2.5 times S/N but less than 10 times S/N)
or positive quantifiable level (response greater than 10 times S/N).
A negative (-) value indicates the compound was not detected (response
less than 2.5 times S/N). The number of symbols for each age group
indicates the number of composites analyzed.
aThe exact isomers were not determined.
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Table 5. Incidence of Detection of Volatile Organic Compounds
in Composited Human Adipose Tissue from
the West Census Region
Census division:
Age group:
Compound
Mountain
Pacific
0-14
15-44 45+
0-14
15-44
45+
Chloroform
1,1,1-Trichloroethane
Bromodichloromethane
Benzene
Tetrachloroethene
Di bromochloromethane
1,1,2-Trichloroethane
Toluene
Chlorobenzene
Ethyl benzene
Bromoform
Styrene
1,1,2,2-Tetrachloroethane
1,2-Dichlorobenzene
1,4-Dichlorobenzene
Xylene3
Ethylphenol
Note: A positive (+) value indicates the compound was detected at a
trace (response greater than 2.5 times S/N but less than 10 times S/N)
or positive quantifiable level (response greater than 10 times S/N).
A negative (-) value indicates the compound was not detected (response
less than 2.5 times S/N). The number of symbols for each age group
indicates the number of composites analyzed.
The exact isomers were not determined.
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Composite FY82 NHATS
Specimens (BCL Protocol)
Add Stable Isotope Labeled
Surrogate Compounds
Extraction - Tissumizer
Bulk Lipid Removal
Get Permeation Chromatography
10%
90%
HRGC/MS (SIM) for
Specific Compound Class
(Toxaphene PCDD, PCDF)
Quantitation/Data Transfer
to BCL
Florisil Fractionation
HRGC/MS (Scanning)
0.01-0.1/ig/g
(PCBs. OCI Pesticides, Etc.)
' AMOCO PX-21/
Glass Fiber
1 Florisil
Figure I. Flow scheme for analysis of semivolatile organic
compounds in human adipose tissue.
10
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Table 6. Incidence of Detection of Target Semivolatile Organic
Compounds in the NHATS FY82 Composite Specimens
Range of observed
lipid concentration
Compound observation (%)a (ng/g)
Frequency of
observation (%)'
Dichlorobenzene
Trichlorobenzene
Naphthalene
Diethyl phthalate
Tributyl phosphate
Hexachlorobenzene
p-BHC
Phenanthrene
Di-rrbutyl phthalate
Heptachlor epoxide
trans-Nonachlor
p_,p_'-DDE
Dieldrin
P_,P_'-DDT
Butyl benzyl phthalate
Triphenyl phosphate
Di-n-octyl phthalate
Mi rex
tris(2-Chloroethyl )phosphate
Total PCBs
Trichlorobiphenyl
Tetrachlorobiphenyl
Pentachlorobiphenyl
Hexachlorobiphenyl
Heptachl orobiphenyl
Octachlorobiphenyl
Nonachl orobiphenyl
Decachlorobiphenyl
9
4
40
42
2
76
87
13
44
67
53
93
31
55
69
36
31
13
2
83
22
53
73
73
53
40
13
7
ND (9)b
ND (9)
ND (9)
ND (10)
ND (44)
ND (12)
ND (19)
ND (9)
ND (10)
ND (10)
ND (18)
ND (9)
ND (44)
ND (9)
ND (9)
ND (18)
ND (9)
ND (9)
ND (35)
ND (15)
ND (9)
ND (9)
ND (21)
ND (19)
ND (19)
ND (20)
ND (18)
ND (22)
- 57
- 21
- 63
- 970
- 120
- 1,300
- 570
- 24
- 1,700
- 310
- 520
- 6,800
- 4,100
- 540
- 1,700
- 850
- 850
- 41
- 210
- 1,700
- 33
- 93
- 270
- 450
- 390
- 320
- 300
- 150
.Sample size = 46 composites.
ND = not detected. Value in parentheses is the estimated limit of
detection.
11
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Table 7. Incidence of Detection of Semivolatile Organic Compounds
Determined in Composited Human Adipose Tissue from
the West Census Region
Census division:
Age group:
Compound
Mountain
Pacific
0-14
15-44
45+
0-14
45+
Dichlorobenzene
Trichlorobenzene
Naphthalene
Diethyl phthalate
Tributyl phosphate
Hexachlorobenzene
p-BHC
Phenanthrene
Di-n-butyl phthalate
Heptachlor epoxide
trans-Nonach lor
p_,ฃ'-DDE
Dieldrin
p_,p_'-DDT
Butyl benzyl phthalate
Triphenyl phosphate
Di-ji-octyl phthalate
Mi rex
tris(2-Ch1oroethyl) phosphate
Total PCBs
Trichlorobiphenyl
Tetrachlorobiphenyl
Pentachlorobiphenyl
Hexachlorobiphenyl
Heptachlorobiphenyl
Octachlorobiphenyl
Nonachlorobiphenyl
Decachlorobiphenyl
Note: A positive (+) value indicates the compound was detected at a
trace (response greater than 2.5 times S/N but less than 10 times S/N)
or positive quantifiable level (response greater than 10 times S/N).
A negative (-) value indicates the compound was not detected (response
less than 2.5 times S/N). The number of symbols for each age group
indicates the number of composites analyzed.
12
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Table 8. Incidence of Detection of Semivolatile Organic Compounds
Determined in Composited Human Adipose Tissue from
the Northeast Census Region
Census division: New England Middle Atlantic
Age group: 0-14 15-44 45+ 0-14 15-44 45+
Compound
Dichlorobenzene - + -+
Trichlorobenzene - ________
Naphthalene - + ----+-+
Diethyl phthalate + + +-++---
Tributyl phosphate - -
Hexachlorobenzene - +++++++-
p-BHC - ++++++++
Phenanthrene - ____+_
Di-n-butyl phthalate - - + +- ++ ++
Heptachlor epoxide - +-+++++-
trans-Nonachlor - + -+++++-
p_,p_'-DDE + ++++++++
Dieldrin - _______+
p_,p_'-DDT - +++++--+
Butylbenzyl phthalate - ---+++-+
Triphenyl phosphate - ---+-+-+
Di-rroctyl phthalate + +---+--+
Mi rex - ++______
tris(2-Chloroethy1) phosphate - ________
Total PCBs - ++++++++
Trichlorobiphenyl - -
Tetrachlorobiphenyl - + + ++ ++ +-
Pentachlorobiphenyl - ++++++++
Hexachlorobiphenyl - + -++++++
Heptachlorobiphenyl - -___+-_
Octachlorobiphenyl - +
Nonachlorobiphenyl - -
Decachlorobiphenyl - -
Note: A positive (+) value indicates the compound was detected at a
trace (response greater than 2.5 times S/N but less than 10 times S/N)
or positive quantifiable level (response greater than 10 times S/N).
A negative (-) value indicates the compound was not detected (response
less than 2.5 times S/N). The number of symbols for each age group
indicates the number of composites analyzed.
13
-------
Table 9. Incidence of Detection of Semi volatile Organic Compounds
Determined in Composited Human Adipose Tissue from
the North Central Census Region
Census division: East North Central West North Central
Age group: 0-14 15-44 45+ 0-14 15-44 45+
Compound
Dichlorobenzene -- --+ - _ __
Trichlorobenzene + - -
Naphthalene -- + ++- + +-
Diethyl phthalate -+ -+- -+- - + ++
Tributyl phosphate -+
Hexachlorobenzene ++- +++ + + +-
p-BHC -+ +++ +++ + + ++
Phenanthrene -+
Di-n-butyl phthalate -+ -+- -++ + -+
Heptachlor epoxide -+ -++ +++ + + ++
trans-Nonachlor -- + -++ - + ++
p_,p_'-DDE ++ +++ +++ + + ++
Dieldrin -- -+- -++ + + +-
p_,p_'-DDT -+ ++- - - +-
Butyl benzyl phthalate ++ -+- +++ + + ++
Triphenyl phosphate -+ -+- -+- - - -+
Di-n-octyl phthalate -- -+- --+ - +-
Mirex -- - -
tris(2-Chloroethy1) phosphate --
Total PCBs -- +++ +++ + + ++
Trichlorobiphenyl -- +++ - - +-
Tetrachlorobiphenyl -+- -++ - + ++
Pentachlorobiphenyl -- -++ -++ + + ++
Hexachlorobiphenyl -- -++ -++ + + ++
Heptachlorobiphenyl -- + -++ - + ++
Octachlorobiphenyl -- +-- -++ - + ++
Nonachlorobiphenyl -- - - +-
Decachlorobiphenyl -- -+- - _ __
Note: A positive (+) value indicates the compound was detected at a
trace (response greater than 2.5 times S/N but less than 10 times S/N)
or positive quantifiable level (response greater than 10 times S/N).
A negative (-) value indicates the compound was not detected (response
less than 2.5 times S/N). The number of symbols for each age group
indicates the number of composites analyzed.
14
-------
Table 10. Incidence of Detection of Semivolatile Organic Compounds
Determined in Composited Human Adipose Tissue from
the South Census Region
ansus division: South Atlantic East South Central West South Central
3e group: 0-14 15-44 45+ 0-14 15-44 45+ 0-14 15-44 45+
impound
ichlorobenzene - - +
richlorobenzene + - -
aphtha! ene ++ +- +-+- - + -+ + +-
iethyl phthalate -++- -+ + + + +-
ributyl phosphate ---- - -
jxachlorobenzene +- ++++ +-++ + + ++ ++ +
-BHC ++ ++++ +-++ + + ++ + ++ +
lenanthrene +-+- + - +- - --
i-n-butyl phthalate -+ -++- -+ + + + +
jptachlor epoxide +- -+++ ++ + + ++ ++ +
rans-Nonachlor +- --++ --+- + + ++ ++ +
n'-QDE ++ ++++ ++++ + + ++ + ++ +
ieldrin -- -+-- ++-- + + +- +
,p_'-DDT ++ +++- ++ + -+ + +
jtylbenzyl phthalate ++ +++- +++- + + + ++ +
riphenyl phosphate -+ -+ -+ + + -+ +
i-n-octyl phthalate -+ --+- - + + +- +
irex +-+- --+- - - --
rjh;(2-Chloroethyl) phosphate - + --
jtal PCBs +- ++++ ++++ + + ++ + ++ +
Trichlorobiphenyl -+-- ++-+ + - +
Tetrachlorobiphenyl -- -+++ -+++ - + ++ +
Pentachlorobiphenyl +- ++++ ++++ - + ++ ++ +
Hexachlorobiphenyl +- ++++ -+++ + + -+ + ++ +
Heptachlorobiphenyl ~ ++++ ++++ + + ++ ++ +
Octachlorobiphenyl --+- ++++ + + ++ + +
Nonachlorobiphenyl + - + ++ --
Decachlorobiphenyl -- -+-+ - - --
Dte: A positive (+) value indicates the compound was detected at a trace (response greater
lan 2.5 times S/N but less than 10 times S/N) or positive quantifiable level (response
"eater than 10 times S/N). A negative (-) value indicates the compound was not detected
^esponse less than 2.5 times S/N). The number of symbols for each age group indicates the
jmber of composites analyzed.
15
-------
This study greatly advances the NHMP's capability to monitor exposure
to toxic organic chemicals. The data base for the number of specific xenobiotic
organic compounds detected in adipose tissue is expanded. Organochlorine pes-
ticides and PCBs have previously been monitored through PGC/ECD techniques.
The HRGC/MS method, however, provides an additional confidence level for de-
termination since identification is based on matching both retention time and
mass spectra. In addition, the detail on PCB levels is expanded as a result
of identifying specific degrees of chlorination (homologs) and providing quan-
titation of individual responses. Previous analyses for PCBs in the NHATS
monitoring program based on the PGC/ECD method had resulted in semi quantita-
tive data based on a single response.
The quantitative data for the target analytes have been submitted
along with all supporting quality control data to Battelle Columbus Division
for statistical analysis. Characterization of additional chromatographic
peaks in the HRGC/MS data to identify other compounds of interest to EPA has
been initiated under a separate work assignment (Contract No. 68-02-4252, Work
Assignment No. 23).
D. PCDD and PCDF
The sample preparation was completed using techniques that isolate
the PCDD and PCDF congeners from potential interferences. The isolation of
the PCDDs and PCDFs was achieved using carbon-based chromatography columns.
Two different carbon materials were used to complete the analysis for the full
range of the tetra- through octachloro-PCDD and PCDF congeners. HRGC/MS oper-
ated in the SIM mode as required to detect compound concentrations ranging
from less than 5 pg/g (for tetra- and pentachloro congeners) to greater than
1,000 pg/g for the octachloro dibenzo-ฃ-dioxin.
Table 11 presents the frequency of detection, mean concentration,
and lipid concentration range of detection for the tetra- through octachloro-
PCDD and PCDF congeners. Tables 12 through 15 present a qualitative summary
for the detection of PCDD and PCDF by census divisions and age groups.
The data in Table 11 indicate that the 2,3,7,8-TCDD was detected in
35 of the 46 composites with an average 1ipid-adjusted concentration of 6.2 ฑ
3.3 pg/g. The average concentration of the other PCDD compounds ranged from
33.5 pg/g for pentachlorodibenzo-]D-dioxin (detected in 91% of the composites)
up to 554 pg/g for octachlorodibenzo-p_-dioxin (detected in 100% of the com-
posites).
The data demonstrated some differences in PCDD levels for the three
age groups evaluated (Figure 2). The PCDFs were generally detected less fre-
quently and were present at lower concentration than the PCDDs. Obvious trends
in the levels of the PCDF congeners with respect to age were not observed.
The mean values for the PCDD and PCDF data from this study are comparable to
work that has been reported for other studies on adipose tissue samples from
the United States (Schecter and Ryan 1986; Ryan 1986) and Sweden (Nygren et al.
1985) (Figure 3).
16
-------
Table 11. Lipid-Adjusted Concentration of PCDD and PCDF in
the NHATS FY82 Composite Specimens
Frequency of Mean concentration Range of
Compound detection (%) (pg/g) detection (pg/g)
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
HxCDDb
1,2,3,4,7,8,9-HpCDD
OCDD
2,3,7,8-TCDF
2,3,4,7,8-PeCDF
HxCDFb
1,2,3,4,6,7,8-HpCDF
OCDF
76
91
98
98
100
26
89
72
93
39
6.2 ฑ 3.3
43.5 ฑ 46.5
86.9 ฑ 83.8
102 ฑ 93.5
694 ฑ 355
15.6 ฑ 16.5
36.1 ฑ 20.4
23.5 ฑ 11.6
20.9 ฑ 15.0
73.4 ฑ 134
ND (1.3)C
ND (1.3) -
ND (13) -
ND (26) -
19 - 3,700
ND (1.3) -
ND (1.3) -
ND (3.0) -
ND (3.5) -
ND (1.2) -
- 14
5,000
620
1,300
660
90
60
79
890
.Mean concentration calculated using trace and positive quantifiable values.
Reference compounds not available to specify isomers.
ND = not detected. Value in parentheses is the estimated limit of detection.
17
-------
Table 12. PCDD and PCDF Detected in the NHATS FY82 Composite
Specimens from the Northeast Census Region
Census division: New England Middle Atlantic
Age group: 0-14 15-44 45+ 0-14 15-44 45+
Compound
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
HxCDD
1,2,3,4,7,8,9-HpCDD
OCDD
2,3,7,8-TCDF
2,3,4,7,8-PeCDF
HxCDF
1,2,3,4,6,7,8-HpCDF
OCDF
Note: A positive (+) value indicates the compound was detected at a
trace (response greater than 2.5 times S/N but less than 10 times S/N)
or positive quantifiable level (response greater than 10 times S/N).
A negative (-) value indicates the compound was not detected (response
less than 2.5 times S/N). The number of symbols for each age group
indicates the number of composites analyzed.
18
-------
Table 13. PCDD and PCDF Detected in the NHATS FY82 Composite
Specimens from the West Census Region
Census division: Mountain Pacific
Age group: 0-14 15-44 45+ 0-14 15-44 45+
Compound
2,3,7,8-TCDD - + + + +
1,2,3,7,8-PeCDD + + - + + +
HxCDD + + + + + +
1,2,3,4,7,8,9-HpCDD + + + + +
OCDD + + + + + +
2,3,7,8-TCDF + - + +
2,3,4,7,8-PeCDF + + + + + +
HxCDF - + + - +
1,2,3,4,6,7,8-HpCDF + + + + +
OCDF + + +
Note: A positive (+) value indicates the compound was detected at a
trace (response greater than 2.5 times S/N but less than 10 times S/N)
or positive quantifiable level (response greater than 10 times S/N).
A negative (-) value indicates the compound was not detected (response
less than 2.5 times S/N). The number of symbols for each age group
indicates the number of composites analyzed.
19
-------
Table 14. PCDD and PCDF Detected in the NHATS FY82 Composite
Specimens from the South Census Region
Census division:
Age group:
Compound
South Atlantic
East South Central West South Central
0-14 15-44 45+ 0-14 15-44 45+ 0-14 15-44 45+
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
HxCDD
1,2,3,4,7,8,9-HpCDD
OCDD
2,3,7,8-TCDF
2,3,4,7,8-PeCDF
HxCDF
1,2,3,4,6,7,8-HpCDF
OCDF
++
+-+- +-++
++ ++-+ +-+-
++ ++++
++++
-+-- +
++ +++-
+- ++--
+-+-
++++
++ ++++ +-++
++
Note: A positive (+) value indicates the compound was detected at a trace
(response greater than 2.5 times S/N but less than 10 times S/N) or positive
quantifiable level (response greater than 10 times S/N). A negative (-) value
indicates the compound was not detected (response less than 2.5 times S/N). The
number of symbols for each age group indicates the number of composites analyzed.
20
-------
Table 15. PCDD and PCDF Detected in the NHATS FY82 Composite
Specimens from the North Central Census Region
Census division: East North Central West North Central
Age group: 0-14 15-44 45+ 0-14 15-44 45+
Compound
2,3,7,8-TCDD -+
1,2,3,7,8-PeCDD ++
HxCDD ++
1,2,3,4,7,8,9-HpCDD ++
OCDD ++
2,3,7,8-TCDF ++
2,3,4,7,8-PeCDF ++
HxCDF -+
1,2,3,4,6,7,8-HpCDF ++
OCDF ++
Note: A positive (+) value indicates the compound was detected at a
trace (response greater than 2.5 times S/N but less than 10 times S/N)
or positive quantifiable level (response greater than 10 times S/N).
A negative (-) value indicates the compound was not detected (response
less than 2.5 times S/N). The number of symbols for each age group
indicates the number of composites analyzed.
21
-------
800
700
600
500
400
300
a
8
100
o
o
50
ซ 50
1
o
I
PCDD from NHATS FY82
Composite Specimens
Wet Tissue Concentration
III 0-14 years
fpj 15 44 years
I I 45+ years
LJpid Adjusted Concentration
PCDF from NHATS FY82
Composite Specimens
TCOF
PeCDF
HxCDF
HpCDF
OCDF
Figure 2. PCDD and PCDF distribution in the general U.S. population
by age group.
22
-------
420 r-
400f
Sweden, 1985
140 -
120 -
100 -
80 -
30 -
40 -
20-
0
TCDF PeCDF HxCDF HoCDF QCDF
TCDD PsCDD HxCDD HoCDD OCOD
c
a
o
O
560 p
540 U
t-
140
2 120
3
"i
100
80
60
General U.S. population
SPA NHATS FY 82 Composite Specimens
TCDF PeCDF HxCCF HoCDF OCDF
-
_
f$&
li%
te-
X': <
wi-
[?>;'^>
, . , , -^ j^^';:
r
I
V
v*
';;'
^;
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**x
^
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>*'
x<
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TCDO PeCOD HxCDD HoCDD OCCD
o
O
SOOJ-
580 t-
140
120
100
ao -
so
40 -
20 -
ofi
Uostate New York
Schecter, A. and J.J. Ryan, 1986
TCDF PeCDF HxCDF HpCDF OCDF
TCDD
HXCDD HDCDD occo
Figure 3. Comparison of PCDD and PCDF concentration (based on wet tissue
weight) profiles for Sweden, the general U.S. population, and upstate
New York (from top to bottom, respectively).
(Source: Stanley 1986; Schecter and Ryan 1986; Nygren et al. 1985)
23
-------
The results of this phase of the broad scan analysis program demon-
strate that the EPA NHATS program is an effective vehicle for documenting the
exposure of the general U.S. population to PCDDs and PCDFs. The analysis of
the 46 composite samples prepared from the FY82 NHATS repository establishes
the prevalence of the 2,3,7,8,-substituted tetra- through octachloro-PCDD and
PCDF congeners in the U.S. population.
The quantitative data for the PCDD and PCDF congeners presented in
this report have been submitted along with all supporting quality control data
to the OTS Design and Development Branch contractor, Battelle Columbus Divi-
sion, for statistical analysis. These data will be analyzed to determine the
significance of differences in PCDD and PCDF levels based on major demographic
factors.
E. Trace Elements
The objective of this task was to provide EPA/OTS with (1) a prelim-
inary assessment of multielement analytical techniques that are applicable for
determining trace elements in adipose tissues and (2) a qualitative assessment
of the level of the specific tissue elements that were present in selected
specimens.
The analyses of nine selected adipose tissue specimens from the FY82
NHATS repository were completed using multielement techniques ICP-AES and NAA.
A total of 18 elements were detected using the two techniques and the estimated
tissue levels are reported. Tables 16 and 17 provide the results generated
by ICP-AES and NAA for the nine adipose tissue specimens.
Elements determined by ICP-AES (Table 16) were aluminum, boron,
calcium, iron, magnesium, sodium, phosphorus, tin, and zinc. The estimated
detection limits for 20 additional elements determined by ICP-AES were also
reported. Elements determined by NAA (Table 17) were bromine, chlorine,
cobalt, iron, iodine, potassium, sodium, rubidium, selenium, silver, and zinc.
The estimated detection limits for 56 additional elements determined by NAA
were also reported. The results reported for iron, zinc, and sodium are com-
parable for the two methods.
The results of this study are compared with tissue data reported in a
monograph prepared for the International Commission in Radiological Protection
(ICRP) (Snyder et al. 1975). Data in the ICRP report are based on multiple
sample analyses by single element techniques. The ICRP data were generated
in the mid-1950s through the mid-1960s. The data for the FY82 NHATS specimens
are generally comparable with the levels presented in the ICRP summary with
the exception of tin. Tin was detected at concentration levels estimated to
range from 4.6 to 15 ug/g in the NHATS specimens compared to 0.047 ug/g for
the values reported for the ICRP report. These tin levels were generated by
the ICP-AES analyses but were not confirmed by NAA.
24
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III. RECOMMENDATIONS
Specific recommendations based on analyte classification are dis-
cussed below.
A. Volatile Organic Compounds
Further analytical method development should be pursued to improve
the determination of volatile organic compounds in human adipose tissue sam-
ples. These improvements should specifically include smaller sample sizes
(1.0 to 5.0 g), more efficient transfer of volatile organics onto the HRGC
column, and further development of the isotope dilution quantitation technique.
These modifications can possibly be achieved by using widebore HRGC columns
and/or cryofocusing techniques.
The analytical method should be modified to provide quantitative
information on compounds of greater volatility than chloroform (such as meth-
ylene chloride, vinyl chloride, etc.). This possibly could be accomplished
by conducting two analyses on each tissue sample. The first analysis should
be conducted for the more volatile compounds with the sample heated in the
range of 50-80ฐC and the headspace sampled for 15 min or less. The second
sample analysis should be conducted with the procedures specified in this re-
port to provide quantitative data for compounds ranging in volatility from
chloroform through the dichlorobenzene isomers.
Stability studies should be conducted to determine the effects of
long-term storage at subzero temperature, and repeated thawing and freezing
on the integrity of the volatile organic content in the sample. The results
of the sample analysis conducted for the FY82 composites indicate considerable
differences in the absolute quantities of the major volatile constituents
(hydrocarbons, aldehydes, ketones, etc.) for samples analyzed within 6 mo of
collection and the NHATS specimens that had been archived prior to analysis
for up to 2 yr.
B. Semi volatile Organic Compounds
The analytical method should be fully validated through additional
intra- and interlaboratory analyses. This is necessary to fully define the
method's limitations [accuracy, precision, limits of detection (LOD), and
limits of quantitation (LOQ)], and quality control (QC) requirements for re-
porting valid data. The method LOD and LOQ for individual analytes should be
determined experimentally through replicate analysis of spiked tissue samples.
The HRGC/MS and PGC/ECD methods should be evaluated using homogenized split
samples to determine the comparability of data for the organochlorine pesti-
cides and PCB data. This is necessary to determine whether trend lines can
be extended from existing PGC/ECD data from previous NHATS analysis programs.
Before proceeding with the validation and comparability studies,
the analytical method should be modified to include at least two more internal
standards for quantitation. Surrogate compounds that will fractionate in the
more polar Florisil fractions are needed to fully evaluate method performance
on a per sample basis. Deuterated phthalate esters that are commercially
27
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available should be considered as surrogates in further evaluation of the ana-
lytical method.
There is a need to establish sufficient characterized reference sam-
ples for continued broad scan analysis projects for use as QC samples. These
QC samples should be available in quantities comparable to the 20-g composited
tissue samples. This type of QC sample could be developed from lipid materials
extracted from human adipose tissues. The lipid materials should be thoroughly
homogenized and the background levels of semivolatile organic analytes estab-
lished through replicate analysis. Once this reference material has been char-
acterized, it could be spiked with additional analytes for positive documenta-
tion of method performance.
Additional method development is needed to identify a more expedient
means of removing bulk lipid from the samples. The current analytical method-
ology, although effective, requires considerable time and cost to prepare the
samples.
There is a need to develop HRGC/selective detector analysis methods
to generate data for target analytes on a routine basis. Specifically, HRGC/
BCD analysis of adipose tissue could supply EPA/OTS with data for chloroben-
zenes, organochlorine pesticides, and specific PCB isomers. This approach
would require smaller sample sizes and result in more expedient sample prepa-
ration while maintaining the sensitivity to achieve 1-10 ng/g (ppb) detection
levels. The approach of HRGC/selective detector analysis could also be used
to monitor phosphate triesters on a routine basis.
Some consideration should be given to evaluation of alternate HRGC/MS
techniques including SIM, negative chemical ionization MS, and mass spectrometry
mass spectrometry (MS/MS) to lower detection limits and increase specificity for
compound classes such as organochlorine pesticides, polychlorinated biphenyls,
polybrominated biphenyls, polychlorinated terphenyls, polychlorinated diphenyl
ethers, and polychlorinated naphthalenes.
C. PCDD and PCDF
The methods described for PCDD and PCDF analysis were developed in
conjunction with the HRGC/MS broad scan analysis method for determination of
general semivolatile organic compounds in human adipose tissues. A continued
effort in following PCDD and PCDF trends will require that the analytical method
as described be fully validated through intra- and interlaboratory studies.
Certified standards other than the 2,3,7,8-TCDD are not currently
available. It is imperative that the additional 2,3,7,8-substituted PCDD and
PCDF congeners be made available as certified materials for future studies to
allow accurate comparison of residue levels in the general population.
The analytical method should be modified to include additional
carbon-13 labeled internal standards to improve the accuracy of the quantita-
tion of the tetra- through octachloro PCDD and PCDF.
28
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The time required for preparation of 10- to 20-g tissue samples by
the method is time intensive as a result of bulk lipid removal by GPC. This
procedure was necessary to achieve the overall objective of the broad scan
analysis program. However, future studies that focus on PCDD and PCDF levels
will require the development of more expedient sample preparation techniques.
D. Trace Elements
The study compared ICP-AES and NAA analysis for multielement determin-
ation in adipose tissue. It is recommended that the sensitivity, selectivity,
and cost of each analysis technique be considered with respect to the trace
elements of interest before proceeding with analysis of additional samples.
The data collected from this preliminary scan of metals in adipose tissue dem-
onstrate that ICP-AES has sufficient sensitivity to allow analysis of large
numbers of adipose samples for multiple elements at a reasonable cost. However,
modifications of the method are necessary to lower the detection limits. These
modifications should include increasing the sample size and incorporating an
acceptable approach for correcting background resulting from overlapping spec-
tral interferences.
NAA has the advantage of detecting some elements not possible by
ICP-AES such as the halogens, rubidium, and cesium. Although multielement
analysis by NAA is much more expensive, it may provide the sensitivity and
specificity needed to identify elements of interest.
One other analytical technique that should be considered is high
temperature graphite furnace atomic absorption spectrometry. This technique
can provide lower levels of detection but is limited to single element mea-
surements. This technique can be evaluated for elements of special interest.
A study of possible interest to EPA would be the determination of
elements directly associated with the lipid materials rather than the whole
tissue. This could be accomplished by rendering the adipose tissue followed
by multielement analysis of the oily materials. Based on the results of these
studies further evaluation may be necessary to determine speciation of elements.
A national survey of human adipose tissue to determine prevalence
of toxic trace elements will require stringent quality assurance practices.
This will require method validation for each element of interest, development
of a representative reference material, and integration of a minimum QC pro-
gram that specifies the frequency of analysis of blanks, spiked tissues, and
reference materials. A representative reference material can be generated by
isolating and homogenizing lipid materials from tissues collected through the
NHATS program. Repetitive analysis of such a reference material (spiked and
unspiked) can provide the necessary data to document method precision and ac-
curacy for all samples analyzed.
29
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IV. REFERENCES
Lucas RM, Pierson SA, Myers DL, Handy RW. 1981. RTI. National Human Adipose
Tissue Survey Quality Assurance Program Plan. Preliminary Draft. RTI/1864/
21-11.
Mack GA, Stanley J. 1984. Preliminary strategy on the National Human Adipose
Tissue Survey. Washington, DC: Office of Toxic Substances. Contracts 68-01-
6721 (Task 21) and 68-02-3938 (Work Assignment 8).
Nygren M, Hansson M, Rappe C, Domellof L, Hardell L. 1985. Analysis of poly-
chlorinated dibenzo-ฃ-dioxins and dibenzofurans in adipose tissue from soft-
tissue sarcoma patients and controls. 189th National ACS Meeting Symposium
on Chlorinated Dioxins and Dibenzofurans in the Total Environment III, Miami,
Florida, 1985. Washington, DC: ACS. 25:160-163 Paper No. 55.
Ryan JJ. 1986. Variation of dioxins and furans in human tissues and organ
by country. Chemosphere 15:1585-1593.
Schecter A, Ryan JJ. 1986. Chlorinated dioxin and dibenzofuran levels in
human adipose tissue from exposed and control populations. In: Chlorinated
dioxins and dibenzofurans in perspective. Rappe C, Choudhary G, Keith LH,
eds. Chelsea, MI: Lewis Publishers, pp. 51-66.
Snyder WS, Cook MJ, Nasset ES, Karhausen LR, Howe!Is GP, Tipton IH. 1975.
Report of the task group on reference man. Elmsford, NY: Pergamon Press.
International Commission Radiological Protection (ICRP) Report No. 23.
Stanley JS. 1986a. Broad scan analysis of human adipose tissue: Volume II:
Volatile organic compounds. EPA 560/5-86-036.
Stanley JS. 1986b. Broad scan analysis of human adipose tissue: Volume III:
Semi volatile organic compounds. EPA 560/5-86-037.
Stanley JS. 1986c. Broad scan analysis of human adipose tissue: Volume IV:
Polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans
(PCDFs). EPA-560/5-86-038.
Stanley JS. 1985. MRI. Analytical method for the determination of semi-
volatile organic compounds in human adipose tissue. Interim Report, Revision
No. 2. Washington, DC: Office of Toxic Substances. Contract 68-02-3938
(Work Assignment 8).
Stanley JS, Boggess KE, Onstot J, Sack TM, Remmers JC, Breen J, Kutz FW,
Curra J, Robinson P, Mack GA. 1986. PCDDs and PCDFs in human adipose tissue
from the EPA FY82 NHATS repository. Chemosphere 15:1605-1612.
Stanley JS, Stockton RA. 1986. Broad scan analysis of human adipose tissue:
Volume 6: Trace elements. EPA-560/5-86-039.
30
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APPENDIX A
GLOSSARY OF TERMS
31
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FY82
HpCDD
HpCDF
HRGC
HxCDD
HxCDF
ICP-AES
ICRP
MS
NAA
NHATS
NHMP
OCDD
OCDF
OTS
PCDD
PCDF
PeCDD
PeCDF
SIM
TCDD
TCDF
Fiscal year 1982
Heptachlorodi benzo-ฃ-di oxi n
Heptachlorodibenzofuran
High resolution gas chromatography
Hexachlorodibenzo-ฃ-dioxin
Hexachlorodibenzofuran
Inductively coupled plasma-atomic emission spectroscopy
International Commission Radiological Protection
Mass spectrometry
Neutron activation analysis
National Human Adipose Tissue Survey
National Human Monitoring Program
Octachl orodi benzo-p_-di oxi n
Octachlorodibenzofuran
Office of Toxic Substances
Polychlorinated dibenzo-ฃ-dioxin
Polychlorinated dibenzofuran
Pentachlorodibenzo-ฃ-dioxin
Pentachlorodibenzofuran
Selected ion monitoring
Tetrachl orodi benzo-p_-di oxi n
Tetrachlorodibenzofuran
32
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TECHNICAL REPORT DATA
(Please read fnanicnons on :lie reverse before completing)
i. ae?ORT NO.
EPA-560/5-86-035
3. RECIPIENTS ACCฃSSlQN>NO.
A. TITLE ANO SUBTITLE
Broad Scan Analysis of Human Adipose Tissue
Volume 1 - Executive Summary
5. REPORT OATS
1 December 1986
6. P_ERFORMING ORGANIZATION CODE
Midwest Research Institute
7. AUTHOR(S)
John S. Stanley
8. PERFORMING ORGANIZATION REPORT NO
8821-A(01)
9. PERFORMING ORGANIZATION NAME ANO AOORESS
Midwest Research Institute
425 Volker Boulevard
Kansas City, Missouri 64110
10. PROGRAM ELEMENT NO.
11. CONTRACT/GRANT NO.
68-02-3938
68-02-4252
PONSOR1NG AGENCY NAME ANO AOORESS
v,i. Environmental Protection Agency
ffice of Toxic Substances
Field Studies Branch (TS-798)
Design Development Branch/Exposure Evaluation Division
13. TYPE OF REPORT ANO PERIOD COVERED
Final
14. SPONSORING AGENCY CODE
15. SUPPLEMENTARY NOTES
J. Remmers and P. Robinson, Work Assignment Managers
J. Breen and C. Stroun. Pronram
16. ABSTRACT
The National Human Adipose Tissue Survey (NHATS) provides the U.S. EPA with a
unique capability for monitoring human exposure to potentially toxic substances that per
sist in the environment. NHATS is an annual program to collect and chemically analyze
adipose tissues from a cross-section of the general U.S. population. Historically,
the^analysis of the tissues has focused on PCBs and organochlorine pesticides. EPA's
Office of Toxic Substances (QTS) has developed an aggressive approach to provide a com-
prehensive assessment of potentially toxic substances in human adipose tissue.
A broad scan analysis concept was introduced beginning with specimens col-
lected in fiscal year 1982. The tissues were analyzed as composites based on the nine
U.S. Census divisions and three age groups. The composites were analyzed for volatile
and semivolatile organics at the parts per billion level and PCDD and PCDF at the
parts per trillion level. Several tissue samples were analyzed by individually coupled
plasma-atomic emission spectroscopy (ICP-AES) and neutron activation analyses (NAA).
This report provides a synopsis of each of these analytical efforts.
17.
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