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1、CODEX STAN 229 Page 1 of 35 RECOMMENDED METHODS OF ANALYSIS FOR PESTICIDE RESIDUES CODEX STAN 2291 1. INTRODUCTION 1.1 Scope Hereunder are given analytical methods which can, from practical experience of the Working Group on Methods of Analysis to the Codex Committee on Pesticide Residues, be applie
2、d to the determination of pesticide residues for regulatory purposes. The list, given in par.2, is not exhaustive and methods not mentioned in the list can also be applied, provided that they can be shown to be effective. 1.2 Criteria for the selection of analytical methods Whenever possible, the Wo
3、rking Group used the following criteria when selecting analytical methods: (i) published in books, manuals or open literature; (For some newer compounds, few methods might be available from these sources; in those cases, GIFAP is prepared to supply analytical methods to regulatory authorities as a m
4、atter of routine policy and to other scientists on a case by case basis. Requests can be directed to: GIFAP, Avenue Albert Lancaster 79A, 1180 Brussels, Belgium); (ii) collaboratively studied or known to have been validated in a large number of laboratories; (iii) capable of determining more than on
5、e residue, i.e. multi-residue methods; (iv) suitable for as many commodities as possible at or below the specified MRLs; (v) applicable in a regulatory laboratory equipped with routine analytical instrumentation. Preference was given to gas chromatography or high performance liquid chromatography as
6、 the determinative step for the methods. Under certain conditions however, methods using less sophisticated procedures, such as thin-layer chromatography or spectrophotometry, may be applicable. This may be the case, for example, when an exporting country wants to check whether or not a commodity pr
7、oduced in that country complies with an Codex MRL. In this case, the treatment history of the commodity may be known or assumed, so that the method used need not be as elaborate as in cases where samples of unknown treatment history are under investigation. Also, when the MRL is high compared to the
8、 limit of determination, simpler methodology may be applied in order to arrive at a “pass/no pass“ decision or for quick screening purposes. 1.3 Application of methods It will always be necessary for the analyst to validate a method before it is first applied in a practical situation. There is a fur
9、ther need for regular checks on the performance of the method in use at both the MRL and at the lower limit of determination. For all new pesticide/commodity combinations the 1 Last revised in 1993 CODEX STAN 229 Page 2 of 35 method must be validated following Good Practice in Residue Analysis, (see
10、 reference 4 ). Confirmation of the identity of an indicated residue by an independent technique is also to be regarded as an essential part of Good Practice in Residue Analysis, especially when the initial result suggests that an MRL is exceeded. Mass spectrometry has become for many residues the m
11、ethod of choice for confimatory purposes, but the ultimate choice of a confirmatory test depends upon the technique used in the initial determination and upon the available instrumentation and necessary expertise. 1.4 References to literature Other relevant Codex recommendations in the field of enfo
12、rcement of Codex maximum limits for pesticide residues are as follows: 1. Recommended Methods of Sampling for the Determination of Pesticide Residues (Ref: Codex Alimentarius Vol. 2, Section 3 ). 2. Portion of a Commodities to which Codex Maximum Residue Limits apply and which should be analysed (Re
13、f: Codex Alimentarius Vol. 2, Section 4.1). 3. Explanatory Notes on Codex Maximum Limits for Pesticide Residues (Ref: Codex Alimentarius Vol. 2, Section 1). 4. Codex Guidelines on Good Practice in Pesticide Residue Analysis. (Ref: Codex Alimentarius Suppl 1 to vol, 2. Section 4). In paragraph 3 refe
14、rences can be found to: - general articles on pesticide residue methodology (paragraph 3.1); - manuals (paragraph 3.2); - individual papers (paragraph 3.3). After each reference given in paragraph 3.3, the compounds to which the methods involved apply are indicated by their CCPR-number. CODEX STAN 2
15、29 Page 3 of 35 2. LIST OF METHODS OF ANALYSIS The numbers refer to the manuals and books listed in paragraph 3.2, the names to the (first) author of the papers listed in paragraph 3.3. _ _ CCPR number Compound References 001 aldrin/dieldrin 1a, 1n, 1o, 1p, 2a, 2d, 2f, 3, 4 (XII-5, 6; S1-5, S8-10, S
16、12, S19), 5, 7a (5, 6), 7c (S8-10, S12, S19), 8a, 8b, 8c, 8d, 9a (M1, M12), 10 Ambrus, Abbott (2), Panel (4), Stijve (2, 3) 002 azinphos-methyl 2c, 2d, 2e, 2f, 3, 4 (XII-6; S5, S8, S19; 63, 63A), 7a (6), 7c (S8, S19), 7d(255), 9a (M2, M5, M12), 10 Abbott (1), Ambrus, Panel (3) 003 binapacryl 2a, 2d,
17、 3, 4 (XII-4, 6; S19; 8, 43), 7a (6), 7c (S19), 9b, 10 Baker, PB (2) 004 bromophos 2a, 2c, 2d, 4 (XII-3, 6; S5, S8-10, S13, S17, S19; 210, 210A), 6d, 7a (3, 6), 7c (S8-10, S13, S17, S19), 9a (M2, M5, M12), 10 Abbott (1), Ambrus, Bottomley, Panel (7, 8), Stijve (7) 005 bromophos-ethyl 2a, 2c, 2d, 3,
18、4 (XII-3, 6; S8, S13, S17, S19; 263), 6d, 7a (3,6), 7c (S13, S17, S19), 9a (M2, M5, M12), 10 Abbott (1), Ambrus 006 captafol 2d, 2e, 4 (XII-6; S8, S19, S20; 266, 266A), 6d, 7a (6), 7b, 7c (S8, S19, S20), 9a (M1, M12), 10 Ambrus, Baker, PB (1), Buettler, Gilvydis, Pomerantz 007 captan 2a, 2d, 2e, 3,
19、4 (XII-6; S8, S12, S19, S20; 12, 12A), 7a (6), 7b, 7c (S8, S12, S19, S20), 9a (M1, M12), 10 Ambrus, Baker, PB (1), Buettler, Gilvydis, Pomerantz 008 carbaryl 1q, 2d, 2e, 2f, 2g, 3, 4 (XII-6; 100), 6c, 7a (6), 9a (M2, M13), 10 Brauckhoff, Chaput, Lawrence(1) 009 carbon disulphide 9a (M8) Mestres (2)
20、010 carbon tetrachloride 1d, 9a (M8) Daft, Mestres (2), Panel (5) CODEX STAN 229 Page 4 of 35 CCPR number Compound References 011 carbophenothion 2a, 2c, 2d, 2e, 2f, 3, 3d, 4 (XII-5, 6; S8, S10, S13, S16, S19), 7a (5, 6), 7c (S8, S10, S13, S16, S19), 8b, 8e, 9a (M2, M5, M12), 10 Abbott (1), Ambrus 0
21、12 chlordane 1a, 1o, 2a, 2d, 2f, 3, 4 (XII-5, 6; S9, S10, S12, S19), 5, 7a (5, 6), 7c (S9, S10, S12, S19), 6c, 6d, 8a, 8b, 8c, 8d, 9a (M1, M12), 10 Panel (4), Stijve (3), Veierov 013 chlordimeform 2e, 6a, 9a (M4), 10 014 chlorfenvinphos 2c, 2d, 2e, 2f, 3, 4 (XII-3, 5, 6; S8, S13, S17, S19; 239), 5,
22、7a (3, 5, 6), 7c (S8, S13, S17, S19), 9a (M2, M5, M12), 10 Abbott (1), Ambrus, Panel (7,8), Stijve (7) 015 chlormequat 6a, 9b Sachse, Stijve (5) 016 chlorobenzilate 2a, 2d, 2e, 3, 4 (XII-6; S19), 7a (6), 7c (S19), 10 017 chlorpyrifos 1p, 2a, 2c, 2d, 2e, 2f, 3, 4 (XII-6; S8, S9, S13, S19), 5, 7a (6),
23、 7c (S8, S9, S13, S19), 8b, 8e, 9a (M2, M5, M12), 10 (Ambrus, Stijve (7) 018 coumaphos 2c, 2d, 2e, 3, 4 (XII-6; S19), 7a (6), 7c (S19), 8b, 8e, 9a (M2, M5, M12) Ambrus, Stijve (7) 019 crufomate 2d, 2e, 2f, 4 (XII-6; S19), 7a (6), 7c (S19), 8b, 8e Stijve (7) 020 2,4-D 2b, 2f, 3, 4 (27, 27A-380), 5,7d
24、(27A-28A), 9a (M6) Ebing, Specht (1) 021 DDT 1a, 1n, 1o, 1p, 2a, 2d, 2f, 3, 4 (XII-4, 5, 6; S1-5, S8-10, S12, S19), 5, 6c, 7a (4,5,6), 7c (S8-10, S12, S19), 8a, 8b, 8c, 9a (M1, M12), 10 Abbott (2), Ambrus, Bottomley, Panel (4), Stijve (2, 3), Veierov 022 diazinon 1a, 2a, 2c, 2d, 2f, 3, 4 (XII-5, 6;
25、S5, S8, S10, S13, S17, S19; 35A, 35B), 6c, 7a (5, 6), 7c (S8, S10, S13, S17, S19), 8e, 9a (M2, M5, M12), 10 Abbott (1), Ambrus, Bottomley, Panel (7), Stijve (7) CODEX STAN 229 Page 5 of 35 CCPR number Compound References 023 1,2-dibromoethane 1d, 8f, 9a (M8) Daft, Heikes, Mestres (2), Panel (5), Rai
26、ns 024 1,2-dichloroethane 1d, 9a (M8) Daft, Mestres (2), Panel (5) 025 dichlorvos 2c, 2d, 2e, 2f, 3, 4 (XII-3, 6; S5, S8, S13, S17, S19; 200), 7a (3, 6), 7c (S13, S17, S19), 8b, 8e, 9a (M2, M5), 10 Abbott (1), Ambrus, Bottomley, Panel (1, 3, 7), Stijve (7) 026 dicofol 2a, 2d, 2f, 3, 4 (XII-6; S8, S9
27、, S12, S19; 69, 69A), 7a (6), 7c (S8, S9, S12, S19), 9a (M1, M12), 10 027 dimethoate 2c, 2d, 2f, 3, 4 (XII-3, 6; S5, S8, S13, S17, S19; 42, 236), 5, 7a (3, 6), 7c (S8, S13, S17, S19), 9a (M5, M12), 10 Abbott (1), Ambrus, Panel (3, 7, 8), Stijve (7) 028 dioxathion 2c, 2d, 4 (XII-6; S8, S13, S19), 7a
28、(6), 7c (S8, S9, S19), 8e, 9a (M2, M5, M12), 10 Abbott (1), Stijve (7) 029 diphenyl 2d, 4 (XII-6; 256A), 7a (6), 10 Farrow, Kitada, Lord, Mestres (1), Player, Pyysalo 030 diphenylamine 2d, 2e, 4 (XII-6), 7a (6), 10 Allen (1), Luke 031 diquat 2e, 4 (37), 6d Calderbank (2), King 032 endosulfan 1b, 2a,
29、 2d, 2f, 3, 4 (XII-5,6; S5, S8, S12, S19; 50), 5, 7a (5, 6), 7c (S19), 5, 9a (M1, M12), 10 Abbott (2), Ambrus 033 endrin 1a, 1o, 2a, 2d, 2f, 3, 4 (XII-5, 6; S5, S9, S10, S12, S19), 5, 7a (5, 6), 7c (S9-10, S12, S19), 8a, 8b, 8c, 8d, 9a (M1, M12), 10 Abbott (2), Ambrus, Panel (4) 034 ethion 1a, 2a, 2
30、c, 2d, 2f, 3, 4 (XII-3, 5, 6; S8, S9, S13, S17, S19), 7a (3, 5, 6), 7c (S8, S9, S13, S17, S19), 8e, 9a (M2, M5, M12), 10 Abbott (1), Ambrus, Stijve (7) CODEX STAN 229 Page 6 of 35 CCPR number Compound References 035 ethoxyquin 2d, 2e, 4 (XII-6; 500) Winell 036 fenchlorphos 1a, 2a, 2c, 2d, 2f, 3, 4 (
31、XII-3, 5, 6; S8-10, S13, S17, S19), 7a (3, 5, 6), 7c (S8-10, S13, S17, S19), 8b, 8e, 9a (M2, M5), 10 Abbott (1), Ambrus, Panel (7, 8), Stijve (7) 037 fenitrothion 2a, 2c, 2d, 2f, 3, 4 (XII-3, 6; S5, S8, S13, S17, S19; 58), 6a, 8e, 9a (M2, M5), 10 Abbott (1), Ambrus, Bottomley, Desmarchelier, Panel (
32、7,8), Stijve (7) 038 fensulfothion 2c, 2d, 2e, 3, 4 (XII-3, 6; S8, S13, S16, S17, S19), 6a, 7a (3, 6), 7c (S8, S13, S16, S17, S19), 9a (M2, M5), 10 039 fenthion 2c, 2d, 2e, 2f, 3, 4 (XII-3, 6; S5, S8, S13, S16, S17, S19), 7a (3, 6), 7c (S8, S13, S16, S17, S19), 8e, 9a (M2, M5), 10 Abbott (1), Ambrus
33、, Hill 040 fentin 2e, 4 (S24; 55A, 55B), 6e Baker, PG (1) 041 folpet 2a, 2c, 2d, 3, 4 (XII-6; S8, S12, S19, S20; 91, 91A), 7a (6), 7b, 7c (S8, S12, S19, S20), 9a (M1, M12), 10 Ambrus, Baker, PB (1), Buettler, Gilvydis, Pomerantz 042 formothion 2d, 4 (XII-6; S5, S8, S19; 236), 6b, 7a (6), 7c (S8, S19
34、), 9a (M2, M5, M12), 10 Abbott (1), Ambrus 043 heptachlor 1a, 1n, 1o, 2a, 2d, 2f, 3, 4 (XII-5, 6; S 1-4, S8-10, S12, S19), 5, 6c, 6d, 7a (5, 6), 7c (S8-10, S12, S19), 8a, 8b, 8c, 8d, 9a (M1, M12), 10 Abbott (2), Ambrus, Stijve (2, 3), Veierov 044 hexachlorobenzene 1k, 1o, 2a, 2d, 3, 4 (XII-1, 5, 6;
35、S9, S10, S12, S19), 5, 6c, 7a (1, 5, 6), 7c (S9, S10, S12, S19), 8a, 8b, 8c, 8d, 9a (M1, M12), 10 Ambrus, Panel (4), Stijve (2, 3), Veierov, Zimmerli 045 hydrogen cyanide 2e, 4 (11), 9b Darr 046 hydrogen phosphide 2e, 4 (13), 9a (M8) Scudamore (2) CODEX STAN 229 Page 7 of 35 CCPR number Compound Ref
36、erences 047 inorganic bromide 2e, 4 (S18; 149), 7c (S18), 9b Panel (2), Roughan, Stijve (1,4), VanWees 048 lindane 1a, 1o, 2a, 2d, 3, 4 (XII-5, 6; S1-5, S8-10, S12, S19), 5, 7a (5, 6), 7c (S8-10, S12, S19), 8a, 8b, 8c, 8d, 9a (M1, M12), 10 Abbott (2), Ambrus, Panel (4), Stijve (2,3), Veierov 049 mal
37、athion 1a, 2a, 2c, 2d, 2f, 3, 4 (XII-3, 5, 6; S5, S8, S10, S13, S17, S19; 72), 7a (3, 5, 6), 7c (S8, S10, S13, S17, S19), 8e, 9a (M2, M5, M12), 10 Abbott (1), Ambrus, Bottomley, Desmarchelier, Panel (1, 3, 7, 8), Stijve (7) 050 mancozeb see 105: dithiocarbamates 051 methidathion 2a, 2c, 2d, 2e, 3, 4
38、 (XII-6; S5, S8, S13, S19; 232), 6b, 7a (6), 7c (S8, S13, S19), 9a (M2, M5, M12), 10 Ambrus 052 methyl bromide 9a (M8) Mestres (2), Panel (5) 053 mevinphos 2c, 2d, 2f, 3, 4 (XII-3, 6; S5, S8, S13, S17, S19; 93), 7a (3, 6), 7c (S8, S13, S17, S19), 9a (M2, M5, M12), 10 Abbott (1), Ambrus 054 monocroto
39、phos 1p, 2c, 2d, 2e, 2f, 4 (XII-6; S19), 7c (S19), 9a (M2, M5), 10 Ambrus 055 omethoate 1p, 2c, 2d, 4 (XII-6; S13, S17, S19; 236), 5, 7a (6), 7c (S13, S17, S19), 9a (M2, M5), 10 Abbott (1), Panel (3) 056 ortho-phenylphenol 2d, 2e, 10 Farrow, Kitada, Lord, Mestres (1), Player, Pyysalo 057 paraquat 2e
40、, 4 (134), 6d, 7b Calderbank (1), Khan, King, Lott 058 parathion 1a, 2a, 2c, 2d, 2f, 3, 4 (XII-3, 4, 5, 6; S5, S8, S10, S13, S17, S19; 87A, 87B), 7a (3, 4, 5, 6), 7c (S8, S10, S13, S17, S19), 8e, 9a (M2, M5, M12), 10 Abbott (1), Ambrus, Panel (3) CODEX STAN 229 Page 8 of 35 CCPR number Compound Refe
41、rences 059 parathion-methyl 1a, 2a, 2c, 2d, 2f, 3, 4 (XII-3, 5, 6; S5, S8, S13, S17, S19; 88A, 88B), 7a (3, 5, 6), 7c (S8, S13, S17, S19), 8e, 9a (M2, M5, M12), 10 Abbott (1), Ambrus, Panel (3) 060 phosalone 2a, 2c, 2d, 2e, 3, 4 (XII-5, 6; S8, S19), 5, 6a, 7a (5, 6), 7c (S8, S19), 9a (M2, M5, M12),
42、10 Abbott (1), Ambrus, Stijve (7) 061 phosphamidon 2c, 2d, 2e, 3, 4 (XII-6; S5, S13, S19), 7a (6), 7c (S13, S19), 9a (M5, M12), 10 Abbott (1), Ambrus, Bottomley 062 piperonyl butoxide 2e, 4 (XII-6; S19, S22; 163), 7a (6), 7c (S19), 9b Krause (2) 063 pyrethrins 2a, 2d, 2e, 4 (XII-6; S19, S22), 6b, 7a
43、 (6), 7c (S19), 9b 064 quintozene 2a, 2d, 2f, 3, 4 (XII-4, 5, 6; S8, S9, S12, S19; 99), 7a (4, 5, 6), 7c (S8, S9, S12, S19), 9a (M1, M12), 10 065 thiabendazole 2d, 2e, 2h, 4 (XII-6; 256A, 256B),7d (256A, 256B), 8g, 9a (M3), 10 Farrow, Kitada, Mestres (1, 3), Rajzman, Yamada 066 trichlorfon 2c, 2d, 2
44、e, 2f, 3, 4 (XII-6; S5, S13, S19; 112), 5, 7a (6), 7c (S13, S19), 8e, 9a (M2, M5, M12) Abbott (1), Ambrus, Bottomley 067 cyhexatin 2e, 4 (S24), 6a, 9b Moellhoff (2) 068 azinphos-ethyl 2c, 2d, 4 (XII-3, 5, 6; S5, S8, S13, S17, S19; 62, 62A), 7a (3, 5, 6), 7c (S8, S13, S17, S19), 9a (M2, M5, M12), 10
45、Abbott (1), Ambrus 069 benomyl see 072: carbendazim 070 bromopropylate 2a, 2d, 4 (XII-6; S19), 7a (6), 7c (S19), 9a (M12), 10 Stijve (6) 071 camphechlor 2a, 2d, 2e,4 (XII-5, 6; S9, S19), 7a (5, 6), 7c (S9, S19) Stijve (2) CODEX STAN 229 Page 9 of 35 CCPR number Compound References 072 carbendazim 2e
46、, 2h, 4 (261, 378), 6a, 6d,7d (261, 370, 378) 9a (M3), 10 Ambrus, Farrow, Mestres (3), VanHaver 073 demeton-S-methyl 2d, 2f, 4 (XII-6; S5, S13, S16, S19), 7a (6), 7c (S13, S16, S19),9a (M2, M5), 10 Abbott (1), Ambrus, Hill, Wagner 074 disulfoton 2a, 2c, 2d, 2e, 2f, 3, 4 (XII-3, 6; S5, S8, S13, S16,
47、S17, S19), 7a (3, 6), 7c (S8, S13, S16, S17, S19), 8e, 9a (M2, M5) Abbott (1), Ambrus, Panel (7) 075 propoxur 1e, 2d, 2g, 4 (XII-6; S19; S25; 216), 6a, 7a (6), 7c (S19), 9a (M2, M13), 10 Ambrus, Brauckhoff, Chaput, Lawrence (1) 076 thiometon 2d, 4 (XII-6; S13), 6b, 7a (6), 7c (S13), 9a (M2, M5, M10,
48、 M12) Abbott (1), Ambrus, Hill 077 thiophanate-methyl 2e, 2h, 4 (261), 5, 7d(261, 370, 378), 9a (M3), 10 Ambrus, Mestres (3), VanHaver 078 vamidothion 4 (XII-3,6; S17), 6a, 7a (3,6), 7c (S17), 9a (M2, M5, M10) 079 amitrole 2e(4A), 7d(4A) Galoux, Lokke (1), v.d.Poll 080 chinomethionate 2d, 2e, 4 (XII
49、-6; S19; 189), 7a (6), 7c (S19), 9b, 10 Ambrus, Francoeur, Krause (1), Tjan 081 chlorothalonil 2a, 2d, 2e, 3, 4 (XII-6; S19), 6b, 7a (6), 7c (S19), 9a (M1, M12), 10 Ambrus, Lokke (2) 082 dichlofluanid 2a, 2d, 4 (XII-6; S8, S12, S19; 203; 203A, 203 -(371), 7a (6), 7c (S8, S12, S19), 7d(203, 371, 203A, 371A), 9a (M1, M12), 10 Ambrus, Lokke (2), Brennecke (4) 083 dicloran 2d, 3, 4 (XII-6; S19), 7a (6), 7c (S19), 9a (M1), 10 Ambrus 084 dodine 2e Newsome (1) CODEX STAN 229 Page 10 of 35 CCPR number Compound