SECTION 302 Pesticide Analytical Manual Vol I Cleanup(C Cl (p. 302-21) Florisil column(4 g)cleanup, with relatively nonpolar one methylene chloride eluant residues (P. 302-28) Charcoal/Celite/magnesium oxide polar residues column cleanup C3 (p. 302-25) Charcoal/silanized Celite column before HPLC cleanup determination for N-methylcarbamates C4(p.30227 C-18 cartridge cleanup before hPlc determination for N-methylcarbamates C5 (p. 302-29) Florisil column cleanup, with latively olaI mixed ether eluants 2 C6 (P. 302-31) SAX/PSA cartridge cleanup polar and nonpolar Determination(D) Recommended Use DG 1(p. 902-33) GLC, 100% methyl siloxane residues with halogen column. 200. EC detector moities DG 2(P. 302-95) GLC, 100% methyl siloxane residues with column,200°,FPDP DG 3(P. 302-97) GLC, 100% methyl siloxane residues with halogen column,200°, ELCD-X DG 4(P. 302-99) GLC, 100% methyl siloxane residues witn nitrogen column,200°, ELCD-N DG 5(P. 302-41) GLC, 100% methyl siloxane residues with nitrogen column, 200, N/P detecto or phosphorus DG 6(P. 302-43) GLC, 100% methyl siloxane column,160°,FID o-phenylphenol DG 7(P. 302-45) GLC, 100% methyl siloxane early eluting residues column, i30 eC detector with halogen, sulfur, other moieties dG8(P. 302-417) GLC, 100% methyl siloxane early eluting residues column,l30°,FPDP with phosphe DG 9(p. 302-419) GLC, 100% methyl siloxane early eluting residues column,l30°, ELCD-X with halogen DG10(P. 302-51) GLC, 100% methyl siloxane late eluting residues column, 280, EC detector with halogen, sulfur, DGll(p. 302-53) GLC, 100% methyl siloxane late eluting residues column,230°,FPDP DG12(P. 302-55) GLC, 100% methyl siloxane late eluting residues column,230°, ELCD-X with halogen DG13(P. 302-57) GLC, 50% phenyl, 50% methyl siloxane column. 200%eC detector su r moieties
SECTION 302 Pesticide Analytical Manual Vol. I 302–2 Transmittal No. 2000-1 (10/1999) Form FDA 2905a (6/92) Cleanup (C) C1 (p. 302-21) Florisil column (4 g) cleanup, with relatively nonpolar one methylene chloride eluant residues C2 (p. 302-23) Charcoal/Celite/magnesium oxide polar residues column cleanup C3 (p. 302-25) Charcoal/silanized Celite column before HPLC cleanup determination for N-methylcarbamates C4 (p. 302-27) C-18 cartridge cleanup before HPLC determination for N-methylcarbamates C5 (p. 302-29) Florisil column cleanup, with relatively nonpolar mixed ether eluants residues C6 (p. 302-31) SAX/PSA cartridge cleanup polar and nonpolar residues Determination (D) Recommended Use DG 1 (p. 302-33) GLC, 100% methyl siloxane residues with halogen. column, 200°, EC detector sulfur, other moities DG 2 (p. 302-35) GLC, 100% methyl siloxane residues with column, 200°, FPD-P phosphorus DG 3 (p. 302-37) GLC, 100% methyl siloxane residues with halogen column, 200°, ELCD-X DG 4 (p. 302-39) GLC, 100% methyl siloxane residues with nitrogen column, 200°, ELCD-N DG 5 (p. 302-41) GLC, 100% methyl siloxane residues with nitrogen column, 200°, N/P detector or phosphorus DG 6 (p. 302-43) GLC, 100% methyl siloxane biphenyl, column, 160°, FID o-phenylphenol DG 7 (p. 302-45) GLC, 100% methyl siloxane early eluting residues column, 130°, EC detector with halogen, sulfur, other moieties DG 8 (p. 302-47) GLC, 100% methyl siloxane early eluting residues column, 130°, FPD-P with phosphorus DG 9 (p. 302-49) GLC, 100% methyl siloxane early eluting residues column, 130°, ELCD-X with halogen DG10 (p. 302-51) GLC, 100% methyl siloxane late eluting residues column, 230°, EC detector with halogen, sulfur, other moieties DG11 (p. 302-53) GLC, 100% methyl siloxane late eluting residues column, 230°, FPD-P with phosphorus DG12 (p. 302-55) GLC, 100% methyl siloxane late eluting residues column, 230°, ELCD-X with halogen DG13 (p. 302-57) GLC, 50% phenyl, 50% methyl residues with halogen, siloxane column, 200°, EC detector sulfur, other moieties
Pesticide Analytical Manual Vol. I SECTION 302 DG14(p. 302-59)GLC, 50% phenyl, 50%0 methyl residues with phosphorus siloxane mn,200°,FPDP DG15 (P. 302-61)GLC, 50% phenyl, 50% methyl residues with sulfur siloxane column, 200, FPD-S DG16(P. 302-63) GLC, 50% phenyl, 50% methyl residues with halogen siloxane column. 200% ELCd-X DG17(P. 302-65)GLC, 50% phenyl, 50% methyl residues with nitrogen siloxane column, 200, N/P or phosphorus detector DG18(P. 302-67)GLC, 50% cyanopropylphenyl residues with halogen 6o% methyl siloxane column sulfur. other moieties 00°, EC detector DG19(P. 302-69)GLC, 50% cyanopropylphenyl residues with phosphorus 50% methyl siloxane column 200°,FPDP
Transmittal No. 2000-1 (10/1999) Form FDA 2905a (6/92) 302–3 Pesticide Analytical Manual Vol. I SECTION 302 DG14 (p. 302-59) GLC, 50% phenyl, 50% methyl residues with phosphorus siloxane column, 200°, FPD-P DG15 (p. 302-61) GLC, 50% phenyl, 50% methyl residues with sulfur siloxane column, 200°, FPD-S DG16 (p. 302-63) GLC, 50% phenyl, 50% methyl residues with halogen siloxane column, 200°, ELCD-X DG17 (p. 302-65) GLC, 50% phenyl, 50% methyl residues with nitrogen siloxane column, 200°, N/P or phosphorus detector DG18 (p. 302-67) GLC, 50% cyanopropylphenyl, residues with halogen, 50% methyl siloxane column, sulfur, other moieties 200°, EC detector DG19 (p. 302-69) GLC, 50% cyanopropylphenyl, residues with phosphorus 50% methyl siloxane column, 200°, FPD-P
SECTION 302 Pesticide Analytical Manual Vol I Figure 302 Recommended Approach: Nonfatty Foods >75% water >75% water <75% water E1/E5 E4/E6 c1/c5 c3/c4 DG2/14 DG10 DG6 DL1 DG3/16 pyrethroids biphenyl DG3 DG4/5/17 phenylphenol carbamates DG14 DG15 DG1 residues residues detectable detectable with element element elective selective detectors detectors 302-4 230
SECTION 302 Pesticide Analytical Manual Vol. I 302–4 Transmittal No. 2000-1 (10/1999) Form FDA 2905a (6/92) Figure 302 Recommended Approach: Nonfatty Foods E2/E3 C1/C5 DG10 pyrethroids DG6 biphenyl, o-phenylphenol DL1 N-methylcarbamates DG2/14 DG3/16 DG4/5/17 DG15 DG12 residues detectable with elementselective detectors >75% water E1/E5 E4/E6 C3/C4 >75% water <75% water E7 C6 DG2 DG3 DG14 DG16 residues detectable with elementselective detectors
Pesticide Analytical Manual Vol. I SECTION 302 VALIDATION Many combinations of method modules are possible. The following combinations have undergone interlaboratory validation and are recommended for use: El+DG2 DG3 Validation report: Sawyer, LD.(1985)J. Assoc. Off. Anal. Chem. 68, 64-71. Collaborative study lead-ing to AOAC official final action status for acephate, a-BHC, chlorpyrifos, dieldrin, monocrotophos, and omethoate in lettuce, strawberries, and toma AOACofficial method reference: Oficial Methods ofAnalysis of the AOAC(1990) 15thed.,985.22. El +c3+ DLl Validation report Pardue, J.R(April 1987)"Recoveries of N-Methyl Carbamates Using a Com- bination of the Luke(PAM I, 232. 4)and Krause (PAM I, 24224b, 242.25) Procedures LIB 3138. FDA. Rockville MD E2 Cl temperature programmed GlC systems equivalent to] DGl, DG7, DG10, and DG16 Validation repor Griffitt, K.R., and Szorik, M. M.( Sept 1989)The Analysis of 127 Total Diet Items for Chlorinated Residues Using Luke/ Solid Phase Extracts, "LIB 3366, FDA. Rockville MD 302
Transmittal No. 2000-1 (10/1999) Form FDA 2905a (6/92) 302–5 Pesticide Analytical Manual Vol. I SECTION 302 VALIDATION Many combinations of method modules are possible. The following combinations have undergone interlaboratory validation and are recommended for use: E1 + DG2, DG3 Validation report: Sawyer, L.D. (1985) J. Assoc. Off. Anal. Chem. 68, 64-71. Collaborative study lead-ing to AOAC official final action status for acephate, a-BHC, chlorpyrifos, dieldrin, monocrotophos, and omethoate in lettuce, strawberries, and tomatoes. AOAC official method reference: Official Methods of Analysis of the AOAC (1990) 15th ed., 985.22. E1 + C3 + DL1 Validation report: Pardue, J.R. (April 1987) “Recoveries of N-Methyl Carbamates Using a Combination of the Luke (PAM I, 232.4) and Krause (PAM I, 242.24b, 242.25) Procedures,” LIB 3138, FDA, Rockville, MD E2 + C1 + [temperature programmed GLC systems equivalent to] DG1, DG7, DG10, and DG16 Validation report: Griffitt, K.R., and Szorik, M.M. (Sept 1989) “The Analysis of 127 Total Diet Items for Chlorinated Residues Using Luke/Solid Phase Extracts,” LIB 3366, FDA, Rockville, MD
SECTION 302 Pesticide Analytical Manual Vol I 3026 230
SECTION 302 Pesticide Analytical Manual Vol. I 302–6 Transmittal No. 2000-1 (10/1999) Form FDA 2905a (6/92)