Pesticide Analytical Manual Vol. I APPENDⅨ SUGGESTONS FOR PRODUCING QUALITY DATA The following suggestions were developed in response to data received and to pecific questions that have been raised Decisions on what Protocols to follow As directed in the first step of the Decision Tree, review existing data on the chemical before performing experiments Examine PAM I Index to Methods for entries, then review the details in appropriate Chapter 8 or 4 table(s); review Appendix I for available GLC data. If these sources reveal gaps in the data, perform the tests necessary to provide missing data, but do not repeat experiments unless specifically asked to do so or unless current data reflect variability Develop glC data(Protocol C) with system(s) likely to detect the chemi- cal ie. of the dg modules listed. choose at least one whose detector selective to elements in the molecule. The electron capture detector may not be suitable to examine uncleaned extracts from Section 302 Protocol D), so DGl, 19, and 18 are often insufficient. If an electron capture detector is the only one that responds to the chemical, apply caution when injecting extracts from Section 302 Choose the GlC system that provides the best chromatography and sensitivity for examining solutions from recovery studies; it is not nec. essary to re-examine the extracts by multiple glc systems The Decision Tree provides basic criteria for making decisions about which methods to test Where situations exist that make testing or con- tinuation of testing illogical, suspend testing and report the reasons Examples If previous studies with radiolabelled chemical clearly show that the residue will partition into the(discarded) water layer of the method, nethod recovery tests need not be run; however, collection of GLC data should still be attempted If the only commodity of interest is fatty, do not attempt to perform tests on the product with methods designed for nonfatty foods. If the lodity is ly Section 304 El(Protocol F)or, if the hemical is an acid or phenol, Section 402 El(Protocol B) Suspend testing if the GlC tests(Protocol C) indicate that even the most sensitive GLC system is insensitive to the compound As a gen- eral rule, suspend testing if the minimum weight of compound that causes 10% full scale deflection(FSD) is equivalent to 210 times the tolerance for jection of the normal mg sample equivalent de- scribed in the method If the method being tested proves not amenable to analysis of a particular commodity, as evidenced by severe emulsions, failure to form distinct phases, etc, suspend testing ppendix l-3Pesticide Analytical Manual Vol. I APPENDIX II Transmittal No. 94-1 (1/94) Form FDA 2905a (6/92) Appendix II–3 SUGGESTIONS FOR PRODUCING QUALITY DATA The following suggestions were developed in response to data received and to specific questions that have been raised. Decisions on What Protocols to Follow • As directed in the first step of the Decision Tree, review existing data on the chemical before performing experiments. Examine PAM I Index to Methods for entries, then review the details in appropriate Chapter 3 or 4 table(s); review Appendix I for available GLC data. If these sources reveal gaps in the data, perform the tests necessary to provide missing data, but do not repeat experiments unless specifically asked to do so or unless current data reflect variability. • Develop GLC data (Protocol C) with system(s) likely to detect the chemi￾cal; i.e., of the DG modules listed, choose at least one whose detector is selective to elements in the molecule. The electron capture detector may not be suitable to examine uncleaned extracts from Section 302 (Protocol D), so DG1, 13, and 18 are often insufficient. If an electron capture detector is the only one that responds to the chemical, apply caution when injecting extracts from Section 302. • Choose the GLC system that provides the best chromatography and sensitivity for examining solutions from recovery studies; it is not nec￾essary to re-examine the extracts by multiple GLC systems. • The Decision Tree provides basic criteria for making decisions about which methods to test. Where situations exist that make testing or con￾tinuation of testing illogical, suspend testing and report the reasons. Examples: – If previous studies with radiolabelled chemical clearly show that the residue will partition into the (discarded) water layer of the method, method recovery tests need not be run; however, collection of GLC data should still be attempted. – If the only commodity of interest is fatty, do not attempt to perform tests on the product with methods designed for nonfatty foods. If the commodity is meat, use only Section 304 E1 (Protocol F) or, if the chemical is an acid or phenol, Section 402 E1 (Protocol B). – Suspend testing if the GLC tests (Protocol C) indicate that even the most sensitive GLC system is insensitive to the compound. As a gen￾eral rule, suspend testing if the minimum weight of compound that causes 10% full scale deflection (FSD) is equivalent to ≥10 times the tolerance for an injection of the normal mg sample equivalent de￾scribed in the method. – If the method being tested proves not amenable to analysis of a particular commodity, as evidenced by severe emulsions, failure to form distinct phases, etc., suspend testing