Pesticide Analytical Manual Vol I TABLE 401-a Table 401-a: Recovery of Chemicals Through Method 401(E1-E2+C1+DL1) (methanol extraction, cleanup with partitioning and charcoal/Celite column, HPLC with post-column derivatization and fluorescence detection) Chemical Recovery RrtI Notes 2.3.5-trimethacarb Ccc 3-hydroxycarbofuran 0.6 3-hydroxymethyl-2, 5-dimethyl= P(70% phenyl methylcarbamate 3-hydroxymethyl-4, 5-dimethyl- C phenyl methylcarbamate 3-ketocarbofuran V(67-110%)0.8 4-hydroxymethyl-3, 5-dimethyl- C phenyl methylcarbamate C 0.8 14 aldicarb sulfoxide P(50-60%) 0.33 bendiocarb bufencarb CCccccc 1.44 Major peak is listed. rboxim 0.7515 l.0 7 carbofuran dioxacarb 0.6715 ethiofencarb P(7082%) 1.1 Breaks down to 2 peaks; other rrt 0.5 1.47 1.1 methiocarb methiocarb sulfone 0.7911 methiocarb sulfoxide methomyl metolcarb CCccccccc 0.46 10 32% recovery from peanuts 0.44 promecarb 1.31 s ng that cause 50% full scale deflection detector response in DL/ h Dy le(approximate percentage when known) Codes: C: complete(>80%); P: Partial (50-80%); S: small (<50%); V: varial R: recovered but no quantitative information available; NR: not recover 2 Retention time relative to carbofuran on c-8 column described Transmittal No. 96-E1 [9/96) Form FDA 2905a(6/92 TABLE 401-a-1
Transmittal No. 96-E1 (9/96) Form FDA 2905a (6/92) TABLE 401-a–1 Pesticide Analytical Manual Vol. I TABLE 401-a Table 401-a: Recovery of Chemicals Through Method 401 (E1-E2 + C1 + DL1) (methanol extraction, cleanup with partitioning and charcoal/Celite column, HPLC with post-column derivatization and fluorescence detection) Chemical Recovery1 Rrt2 ng3 Notes 1 Codes: C: complete (>80%); P: partial (50-80%); S: small (<50%); V: variable (approximate percentage when known); R: recovered but no quantitative information available; NR: not recovered. 2 Retention time, relative to carbofuran, on C-8 column described in DL1. 3 ng that cause 50% full scale deflection detector response in DL1. 2,3,5-trimethacarb C 3,4,5-trimethacarb C 3-hydroxycarbofuran C 0.6 10 3-hydroxymethyl-2,5-dimethyl= P (70%) phenyl methylcarbamate 3-hydroxymethyl-4,5-dimethyl= C phenyl methylcarbamate 3-ketocarbofuran V (67-110%) 0.85 11 4-hydroxymethyl-3,5-dimethyl= C phenyl methylcarbamate aldicarb C 0.83 14 aldicarb sulfoxide P (50-60%) 0.33 9 aldoxycarb C 0.4 9 bendiocarb C 1 10 bufencarb C 1.44 19 Major peak is listed. butocarboxim C 0.75 15 carbaryl C 1.06 7 carbofuran C 1 10 dioxacarb C 0.67 15 ethiofencarb P (70-82%) 1.1 15 Breaks down to 2 peaks; other rrt 0.5. fenobucarb C 1.47 10 isoprocarb C 1.13 8 methiocarb C 1.26 10 methiocarb sulfone C 0.79 11 methiocarb sulfoxide C 0.64 12 methomyl C 0.46 10 32% recovery from peanuts. metolcarb C 0.85 10 oxamyl C 0.44 10 promecarb C 1.31 10
TABLE 401-a Pesticide Analytical Manual Vol I Table 401-a: Recovery Through Method 401(E1-E2+C1+ DL1) Chemical Recover 0.988 P(40460%) 0.99 Recovery C if analytical breakdown product(methomyl)also measured XMC 1.0610 TABLE 401-a-2
TABLE 401-a Pesticide Analytical Manual Vol. I Transmittal No. 96-E1 (9/96) TABLE 401-a–2 Form FDA 2905a (6/92) Chemical Recovery1 Rrt2 ng3 Notes Table 401-a: Recovery Through Method 401 (E1-E2 + C1 + DL1) propoxur C 0.98 8 thiodicarb P (40-60%) 0.99 11 Recovery C if analytical breakdown product (methomyl) also measured. XMC C 1.06 10
Pesticide Analytical Manual Vol I TABLE 401-b Table 401-b: Recovery of Chemicals Through Method 401(E1-E2+C1+ DL2 (methanol extraction, cleanup with partitioning and charcoal/Celite column, HPLC with fluorescence detection/ Recovery!Rrt2 Notes4 l.06 Ex L288 Em L 330. carbofuran Ex 288. Em l330 CGA161149 V(4399%)0.73 Ex L288. EmL330 CGA195654 S(15-132%)0.57 dioxacarb 0.67 Ex L 265. Em L 294 V(60-100%)1.09 Ex L 288. Em L 330. Low level residues may be obscured by matrix interferences. isoprocarb 1.13 370 Ex L264 Em L 292. naphthaleneacetamide P(77%) Ex L288 Em L 320 For C rec.. elute charcoal with additional 100 mL petr ether napropamIde 4ExL288,FmL330. P Cccc Ex L288 Em L 330 phosalone oxygen analog C ExL 288. Em L 330 piperonyl butoxide Ex 288. Em L 330 40ExL276,EmL300 Codes: C: complete (>80%); P: Partial (50-80%); S: small(<50%); V: variable(approximate percentage when known) R: recovered but no quantitative information available; NR: not recovered. Retention time, relative to carbofuran, on C-s column described in DLl/DL2 s ng that cause 50% full scale deflection detector response in DI Excitation (Ex)and emission(Em) wavelengths found optimum for the chemical. Transmittal No. 96-E1 [9/96) orm FDA 2905a(6/92 TABLE 401-b-1
Transmittal No. 96-E1 (9/96) Form FDA 2905a (6/92) TABLE 401-b–1 Pesticide Analytical Manual Vol. I TABLE 401-b Table 401-b: Recovery of Chemicals Through Method 401 (E1-E2 + C1 + DL2) (methanol extraction, cleanup with partitioning and charcoal/Celite column, HPLC with fluorescence detection) Chemical Recovery1 Rrt2 ng3 Notes4 1 Codes: C: complete (>80%); P: partial (50-80%); S: small (<50%); V: variable (approximate percentage when known); R: recovered but no quantitative information available; NR: not recovered. 2 Retention time, relative to carbofuran, on C-8 column described in DL1/DL2. 3 ng that cause 50% full scale deflection detector response in DL2. 4 Excitation (Ex) and emission (Em) wavelengths found optimum for the chemical. carbaryl C 1.06 3 Ex L 288, Em L 330. carbofuran C 1 90 Ex L 288, Em L 330. CGA 161149 V (43-99%) 0.73 10 Ex L 288, Em L 330. CGA 195654 S (15-132%) 0.57 300 Ex L 288, Em L 330. dioxacarb C 0.67 180 Ex L 265, Em L 294. fluometuron V (60-100%) 1.09 50 Ex L 288, Em L 330. Low level residues may be obscured by matrix interferences. isoprocarb C 1.13 370 Ex L 264, Em L 292. naphthaleneacetamide P (77%) 0.75 3 Ex L 288, Em L 320. For C rec., elute charcoal with additional 100 mL petr ether napropamide C 1.36 4 Ex L 288, Em L 330. phosalone C 1.7 90 Ex L 288, Em L 330. phosalone oxygen analog C 1.3 90 Ex L 288, Em L 330. piperonyl butoxide C 1.74 5 Ex 288, Em L 330. propoxur C 0.98 40 Ex L 276, Em L 300
TABLE 401-b Pesticide Analytical Manual Vol I TABLE 401-b-2
TABLE 401-b Pesticide Analytical Manual Vol. I Transmittal No. 96-E1 (9/96) TABLE 401-b–2 Form FDA 2905a (6/92)
Pesticide Analytical Manual Vol I TABLE 402-a Table 402-a: Recovery of Chemicals Through Method 402 (E1-E7+C1+ DG1 or DGS or DG4) extraction from acidified mixture, GPC, methylation, and Florisil cleanup determination by GLC] Recovery 2. 3.5.6-tetrachlorotere= El: NR ethylated completely, but did not elute from phthalic acid GPO E2: NR 2.3.5-triiodobenzoic acid El: V(6686%) No ester reference standard. E2:V(79-138%) 2,3,6TBA El: c E2: C 2, 3-dihydro-3, 3-methyl-2-oxo- El: NR Chemical did not methylate 5-benzofuranyl methyl sulfonate E2: NR 24.5-T P 79% mean recovery, 31%CV, n=270, nonfat and 2:P 24-D El: P 72% mean recovery, 34% CV, n=186, nonfat and E2: P 24-DB El: c E2: C 2-hydroxy-2, 3-dihydro-3, 3-methyl- El: NR Chemical did not methylate 5-benzofuranyl methyl sulfonate E2: NR 3,5, 6-trichloro-2-pyridinol NR Some(<20%)recovered in 100mL ethyl ether. 3,5-dibromo-A-hydroxy S(0-42%) benzoic acid g-carboxy-5-ethoxy-l, 2, 4-thiadiazole NR Methyl ester not eluted from Florisil column 8-chlorosulfonamide acid Complete recovery from Florisil only, 14% from B-methyl--nitrophenol Methyl ether completely eluted from Florisil, but only 30%from GPC. I Codes: C: complete(>80%); P: partial (50-80%); S: small (<50%); V: variable(approximate percentage when known) R: recovered but no quantitative information available; NR: not recovered. 2 Extraction module used during testing(eg, El)is indicated with each result. Florisil eluted with Eluant I and Eluant 2 only; chemicals eluted in ethyl ether (EE)are considered NR through basic method as normally performed. a Ester/ether elutes from Florisil with Eluant 2 unless otherwise noted. s When no reference material available for ester/ether, recoveries calculated against acid/phenol methylated per method Transmittal No. 96-E1 [9/96) Form FDA 2905a(6/92 TABLE 402-8-1
Transmittal No. 96-E1 (9/96) Form FDA 2905a (6/92) TABLE 402-a–1 Pesticide Analytical Manual Vol. I TABLE 402-a Table 402-a: Recovery of Chemicals Through Method 402 (E1-E7 + C1 + DG1 or DG3 or DG4) (extraction from acidified mixture, GPC, methylation, and Florisil cleanup, determination by GLC) 1 Codes: C: complete (>80%); P: partial (50-80%); S: small (<50%); V: variable (approximate percentage when known); R: recovered but no quantitative information available; NR: not recovered. 2 Extraction module used during testing (e.g., E1) is indicated with each result. 3 Florisil eluted with Eluant 1 and Eluant 2 only; chemicals eluted in ethyl ether (EE) are considered NR through basic method as normally performed. 4 Ester/ether elutes from Florisil with Eluant 2 unless otherwise noted. 5 When no reference material available for ester/ether, recoveries calculated against acid/phenol methylated per method. Chemical Recovery1-3 Notes4,5 2,3,5,6-tetrachlorotere= E1: NR Methylated completely, but did not elute from phthalic acid GPC. E2: NR 2,3,5-triiodobenzoic acid E1: V (66-86%) No ester reference standard. E2: V (79-138%) 2,3,6-TBA E1: C E2: C 2,3-dihydro-3,3-methyl-2-oxo- E1: NR Chemical did not methylate. 5-benzofuranyl methyl sulfonate E2: NR 2,4,5-T E1: P 79% mean recovery, 31% CV, n=270, nonfat and fat. E2: P 2,4-D E1: P 72% mean recovery, 34% CV, n=186, nonfat and fat. E2: P 2,4-DB E1: C E2: C 2-hydroxy-2,3-dihydro-3,3-methyl- E1: NR Chemical did not methylate. 5-benzofuranyl methyl sulfonate E2: NR 3,5,6-trichloro-2-pyridinol NR Some (<20%) recovered in 100mL ethyl ether. 3,5-dibromo-4-hydroxy= S (0-42%) benzoic acid 3-carboxy-5-ethoxy-1,2,4-thiadiazole NR Methyl ester not eluted from Florisil column. 3-chlorosulfonamide acid NR Complete recovery from Florisil only, 14% from GPC. 3-methyl-4-nitrophenol Methyl ether completely eluted from Florisil, but only 30% from GPC