United States Prevention, Pesticides EPA712-C-96-176
Environmental Protection and Toxic Substances August 1996
Agency (7101)
&EPA Residue Chemistry
Test Guidelines
OPPTS 860.1360
Multiresidue Method
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INTRODUCTION
This guideline is one of a series of test guidelines that have been
developed by the Office of Prevention, Pesticides and Toxic Substances,
United States Environmental Protection Agency for use in the testing of
pesticides and toxic substances, and the development of test data that must
be submitted to the Agency for review under Federal regulations.
The Office of Prevention, Pesticides and Toxic Substances (OPPTS)
has developed this guideline through a process of harmonization that
blended the testing guidance and requirements that existed in the Office
of Pollution Prevention and Toxics (OPPT) and appeared in Title 40,
Chapter I, Subchapter R of the Code of Federal Regulations (CFR), the
Office of Pesticide Programs (OPP) which appeared in publications of the
National Technical Information Service (NTIS) and the guidelines pub-
lished by the Organization for Economic Cooperation and Development
(OECD).
The purpose of harmonizing these guidelines into a single set of
OPPTS guidelines is to minimize variations among the testing procedures
that must be performed to meet the data requirements of the U. S. Environ-
mental Protection Agency under the Toxic Substances Control Act (15
U.S.C. 2601) and the Federal Insecticide, Fungicide and Rodenticide Act
(7U.S.C. I36,etseq.).
Final Guideline Release: This guideline is available from the U.S.
Government Printing Office, Washington, DC 20402 on The Federal Bul-
letin Board. By modem dial 202-512-1387, telnet and ftp:
fedbbs.access.gpo.gov (IP 162.140.64.19), internet: http://
fedbbs.access.gpo.gov, or call 202-512-0132 for disks or paper copies.
This guideline is also available electronically in ASCII and PDF (portable
document format) from the EPA Public Access Gopher (gopher.epa.gov)
under the heading "Environmental Test Methods and Guidelines."
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OPPTS 860.1360 Multiresidue method.
(a) Scope—(1) Applicability. This guideline is intended to meet test-
ing requirements of the Federal Insecticide, Fungicide, and Rodenticide
Act (FIFRA) (7 U.S.C. 136 et seq.) and the Federal Food, Drug, and Cos-
metic Act (FFDCA) (21 U.S.C. 301 et seq.)
(2) Background. The source material used in developing this har-
monized OPPTS guideline is OPP 171-4 Results of Tests on the Amount
of Residue Remaining, Including a Description of the Analytical Method
Used (Pesticide Assessment Guidelines, Subdivision O: Residue Chem-
istry., EPA Report 540/9-82-023, October 1982). This OPPTS guideline
should be used in conjunction with OPPTS 860.1000, Background.
(b) Purpose. Analytical methods capable of determining many pes-
ticide residues in a single analysis have been developed by the Food and
Drug Administration (FDA). In order to assess the incidence of the resi-
dues remaining on foods and feeds, EPA uses the monitoring data com-
piled by FDA employing these multiresidue methods in its residue enforce-
ment programs. By using the data generated under this guideline, FDA
chemists can confirm the presence or absence of many pesticides and their
metabolites in commodities, and identify many unidentified analytical re-
sponses (UARs) in samples of unknown treatment history.
(c) Method. (1) Specific directions for each multiresidue method used
by FDA are published in that Agency's Pesticide Analytical Manual, Vol.
I (PAM I)(see paragraph (d)(l) of this guideline). A compilation of data
on the analytical behavior of pesticides and related chemicals is also pub-
lished in PAM I. The data compiled in this way include: Relative retention
times of the compounds on a variety of gas-liquid chromatographic (GLC)
columns, responses of various GLC detectors to the compounds, recovery
of the compound through complete methods, and sometimes through im-
portant steps within the methods. The large amount of effort spent on the
testing of multiresidue methods and compilation of results is justified by
the advantages such compilations offer the analytical chemist. When ana-
lytical response for numerous compounds is known, the analyst is better
equipped to recognize the residues that are present in samples of unknown
treatment history. In situations where the likelihood of some particular res-
idue is known, the data lists for several methods can be consulted to help
choose which method should be used.
(2) An updated compilation of multiresidue methods is provided in
Appendix I of PAM I under paragraph (d)(l) of this guideline. All petition-
ers/registrants are expected to provide recovery data for parent pesticide
and all metabolites of concern through these methods. They are expected
to follow the directions for the protocols found in PAM I, Appendix II
under paragraph (d)(l) of this guideline, starting with the decision tree
for multiresidue methods testing and the accompanying guidance found
in the suggestions for producing quality data; i.e. decisions on what proto-
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cols to follow and proper application of methods. If the decision tree indi-
cates that recovery is likely, the registrant should consult the data develop-
ment section of the proper protocols and follow the guidance offered pre-
cisely to generate quality data. It is imperative that all laboratories generat-
ing multiresidue methods recovery data follow the directions as written
so that EPA can determine how a chemical behaves when analyzed accord-
ing to a precisely defined method. When data have been generated, the
registrants are to use the reporting forms found in PAM I, Appendix II
for presenting these data to the Agency. From the completed reports the
appropriate recovery data will be extracted and incorporated for a future
up-date of Appendix I.
(3) If the recovery is considered to be complete through any of the
multiresidue protocols, registrants are encouraged to use that protocol as
their primary enforcement method. However, registrants need to develop
a separate single analyte confirmatory method for publication in PAM II
(under paragraph (d)(2) of this guideline).
(d) References. The following references should be consulted for ad-
ditional background material on this test guideline.
(1) Pesticide Analytical Manual (PAM), Volume I. Food and Drug
Administration, Washington, DC. Available from National Technical In-
formation Service, Springfield, VA (1994).
(2) Pesticide Analytical Manual (PAM), Volume II. Food and Drug
Administration, Washington, DC. Available from National Technical In-
formation Service, Springfield, VA (1994).
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