FDAC标准汇编.pdf
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1、Pesticide Analytical Manual Vol. I APPENDIX I Transmittal No. 2000-1 (10/1999) Form FDA 2905a (6/92) Appendix I1 APPENDIX I: PESTDATA Caution: Use this table only as a quick reference for tentative identification of residues found in samples analyzed by the most com- monly used PAM I multiresidue me
2、thods. Always compare the residue to a standard chromatographed in your own gas chromatograph. Apply appropriate confirmatory tests to verify tentative identification. Note that PESTDATA cannot and does not contain all details; consult PAM I tables that accompany each method for more definitive info
3、rmation about the behavior of the compound through the steps of the methods. NOTATIONS AND ABBREVIATIONS USED IN PESTDATA (In all categories a hyphen indicates absence of data) Name Preferred name for each chemical. “*” indicates chemicals with multiple GLC peaks. Chlordane, Strobane, toxaphene and
4、all Aroclors are listed only in the table ordered by name and do not appear in the tables ordered by relative retention times. Molecular Formula Numbers are not subscripted. Averages are used for multicomponent chemicals. RRT/c Columns list retention times (relative to chlorpyrifos) on GLC column in
5、dicated. Conditions under which these data were gathered are described in these Section 302 DG modules: GLC ColumnSection 302 DG modules OV-101DG1-DG5 OV-17DG13-DG17 OV-225DG18, DG19 Note that headers in these tables refer to GLC columns by the names used for packed columns, despite DG1-DG19s descri
6、ptions of wide bore capillary column systems, because so many of these rrts were developed using packed columns. Rrt data for equivalent packed and capillary columns are expected to be essentially identical and are combined in PESTDATA. Pesticide Analytical Manual Vol. I APPENDIX I Transmittal No. 2
7、000-1 (10/1999) Form FDA 2905a (6/92) Appendix I2 Responses Data specify column and detector used. Numbers refer to weight (ng) that causes detector response of approximately 50% full scale deflection (FSD) on the recording device. Response values collected when the detector was combined with a wide
8、 bore capillary column include the notation “(WB).” Codes refer to detectors and operating conditions described in these Section 302 DG modules, except that all response values are based on detector sensitivity of 50% FSD to 1.5 ng chlorpyrifos: CodeDetectorSection 302 DG modules TRtritium electron
9、capturenone - obsolete detector TIthermionic (KCl)none - obsolete detector FPflame photometric, phosphorusDG2, DG14, DG19 FSflame photometric, sulfurDG15 NI 63Ni electron capture DG1, DG13, DG18 NPnitrogen/phosphorusDG5, DG17 HXelectroconductivity (halogen mode)DG3, DG16 HNelectroconductivity (nitro
10、gen mode)DG4 MCmicrocoulometricnone - obsolete detector NOTES: Response values are approximate and can vary dramatically on different chromatographs. Most response values represent rounded-off or averaged values; some were collected under conditions different from those suggested in references. Reco
11、veries Data on the recovery of the compound through several PAM I methods are listed in columns with the following headings. See the appropriate PAM I table(s) for more details, such as partial recoveries through Florisil. HeadingCommon NamePAM I SectionPAM I Table 302Luke (Los Angeles)302 E1-E3, no
12、 cleanup302-a 303Mills, Onley, Gaither303 E1-E5 + C1 or C2303-a 304Mills fatty food304 E1-E5 + C1-C4304-a EthersFlorisil elution system303 C1, 304 C1 and C3303-a, 304-a CH2Cl2alternative Florisil elution303 C2, 304 C2 and C4303-a, 304-a Recovery codes have the following meanings: C: complete (80%);
13、P: partial (50-80%); S: small (5% FSD. It is not necessary to evaporate the solvent from the fortification solution once it has been added to the sample, unless there is some reason to expect it to interfere with the analysis. It is preferable for the fortifying solution to be made from the same sol
14、vent used to extract the sample. Use only the 60/100 mesh PR grade Florisil specified by Sections 303 and 304 (Protocols E and F). Other grades of commercially available Florisil are likely to result in different elution patterns. During tests of elution from Florisil, do not add reference material
15、to the Florisil column in a polar solvent, which will affect elution pattern. Test Florisil elution by both ethyl ether/petroleum ether (Sections 303 C1, 304 C1 and C3) and methylene chloride (303 C2, 304 C2 and C4) elution systems when following the steps of Protocols E and F. Even when Florisil el
16、ution tests with reference standards indicate no elu- tion with later eluants, examine by GLC all the Florisil eluates of the recovery test from the fortified sample. Sometimes the presence of extract changes the Florisil elution pattern. Pesticide Analytical Manual Vol. IAPPENDIX II/PROTOCOL A APPE
17、NDIX II5 Transmittal No. 94-1 (1/94) Form FDA 2905a (6/92) PROTOCOL A: PROCEDURE FOR TESTING CHEMICALS THROUGH SECTION 401 BACKGROUND Methods: Section 401 E1 + C1 + DL1 or DL2 Chemical Type: Applicable to chemicals with N-methylcarbamate structure (DL1) and to some chemicals that are naturally fluor
18、escent (DL2). Commodity Type: Applicable to nonfatty foods and to certain fatty foods such as soybeans and nuts. PAM I Tables: Tables 401-a, 401-b DATA DEVELOPMENT HPLC Analytical Behavior N-Methylcarbamates: Set up HPLC with post-column fluorescence labeling and fluorescence detector, as described
19、in Section 401 DL1; check for proper opera- tion using system suitability test described. Fluorescent Pesticides: Set up HPLC and fluorescence detector, as described in Section 401 DL2. Develop information on test chemical(s) as follows: Dissolve reference standard in methanol to prepare stock solut
20、ions. Dilute with methanol for HPLC working standards. Determine amount (ng) of chemical that causes detector response of 50% full scale deflection (FSD) on recorder or printer/plotter. Note peak shape of response to determine adequacy of chromatography. Determine linear response range of detector t
21、o chemical. Determine stability of chemical in methanol: Short term. Prepare 1 g/mL methanol solution of chemical. Use actinic glassware. Inject 5-10 L injections of this solution into HPLC system over 8 hr to measure short term stability of chemical in solu- tion. Report results as peak height (mm)
22、 response. Long term. Using same solution as above, inject 10 L into system once a day for 1-2 wk to measure long term stability of solution. Store solution on laboratory bench during day and in refrigerator over- night. Report results as peak height (mm) response to test chemical, normalized to pea
23、k height for carbofuran standard injected on same day. APPENDIX II/PROTOCOL APesticide Analytical Manual Vol. I Transmittal No. 94-1 (1/94) Form FDA 2905a (6/92)APPENDIX II-6 Calculate retention time of chemical relative to carbofuran on the HPLC system. Recovery of Chemical Through Cleanup Column P
24、repare fortification solution by diluting stock solution with methanol. Initially determine that charcoal/silanized Celite column has proper elu- tion characteristics as described in Section 401 C1. In duplicate, add 25 g pesticide to newly prepared charcoal/silanized Celite column. Then elute as de
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