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(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
TABLE 402-a Pesticide Analytical Manual Vol I Table 402-a: Recovery Through 402 (E1-E7+C1+ DG1 or DG3 or DG4) Chemical Notest. 4-chlorobenzoic acid El: S(27-66%) Low temperature column needed to detect methyl E2S(276%) 士-CPA El: S(32-69%) Chromatographs only on wide bore GLC. No ester reference standard 6-chloropicolinic acid Methylates, but methyl ester does not elute from Florisil AC 263.222 ammonium salt R Methyl ester not eluted from Florisil acifluorfen El:P(5469%) Iloxydim-sodium El: NR Does not methylate E2: NR arsanilic acid Compound did not methylate under method conditions benazolin El: NR 28-32% recovered if Florisil eluted with additional 100 ML EE E2: NR Complete recovery if Florisil eluted with additional 100 ML EE bifenox El: C Parent is methyl ether. bromacil E2: NR Complete recovery if Florisil eluted with addi- nal 100 ML EE bromofenoxim El:P(57-86%)No ether reference standard. E2: C br El: P(50-68%) No ether reference standard chloramben E1:S(40-43%) E2:P(4959%) chloroxuron El: NR Does not methylate E2. NR clofencet potassium salt Does not methylate Copra El: P(50-66%) Chromatographs only on wide bore GLC. No ester TABLE 402-a-2
TABLE 402-a Pesticide Analytical Manual Vol. I Transmittal No. 96-E1 (9/96) TABLE 402-a–2 Form FDA 2905a (6/92) Chemical Recovery1-3 Notes4,5 Table 402-a: Recovery Through 402 (E1-E7 + C1 + DG1 or DG3 or DG4) 4-chlorobenzoic acid E1: S (27-66%) Low temperature column needed to detect methyl ester. E2: S (2-76%) 4-CPA E1: S (32-69%) Chromatographs only on wide bore GLC. No ester reference standard. E2: C 6-chloropicolinic acid NR Methylates, but methyl ester does not elute from Florisil. AC 263,222 ammonium salt NR Methyl ester not eluted from Florisil. acifluorfen E1: P (54-69%) alloxydim-sodium E1: NR Does not methylate. E2: NR arsanilic acid Compound did not methylate under method conditions. benazolin E1: NR 28-32% recovered if Florisil eluted with additional 100 mL EE. E2: NR Complete recovery if Florisil eluted with additional 100 mL EE. bifenox E1: C Parent is methyl ether. E2: C bromacil E2: NR Complete recovery if Florisil eluted with additional 100 mL EE. bromofenoxim E1: P (57-86%) No ether reference standard. E2: C bromoxynil E1: P (50-68%) No ether reference standard. E2: C chloramben E1: S (40-43%) E2: P (49-59%) chloroxuron E1: NR Does not methylate. E2: NR clofencet potassium salt NR Does not methylate. cloprop E1: P (50-66%) Chromatographs only on wide bore GLC. No ester reference standard. E2: C
Pesticide Analytical Manual Vol I TABLE 402-a Table 402-a: Recovery Through 402(E1-E7+C1+DG1 or DG3 or DG4) Chemical Recove notes CP106070 Does not methylate CP106077 Some methylation, but does not elute from GPC. CP108064 El: NR nR through method even in 100 mL EE; recovered from GPC only, Florisil onl E2: NR Complete recovery if Florisil eluted with additional 100 mL EE CP108669 NR Some methylation, but does not elute from GPC. CP92429 NR Does not methylate CP95200 Some methylation, but does not elute from GPC CP97290 Does not methylate cyclanilide El: c E2:V(45-67%) dicamba E1:P(71-76%) E2. C dichlorprop E1:C(80%) No ester reference standard E2:C(72-104%) diclofop E1:S(4351%) E2:V(81200%) dinoseb El: NR Does not methylate E2: NR El: NR Does not methylate; parent 50% recovered if Florisil eluted with 100 mLEE E2: NR Does not methylate; complete recovery of parent E1:S(45-50%)Nit detecte tandard El: NR E2: NR fetac E1:C(7492%) Jo ester reference standard E2: C El: NR Methylated product not soluble in hexane E2: NR TABLE 402-8-3
Transmittal No. 96-E1 (9/96) Form FDA 2905a (6/92) TABLE 402-a–3 Pesticide Analytical Manual Vol. I TABLE 402-a Chemical Recovery1-3 Notes4,5 Table 402-a: Recovery Through 402 (E1-E7 + C1 + DG1 or DG3 or DG4) CP 106070 NR Does not methylate. CP 106077 NR Some methylation, but does not elute from GPC. CP 108064 E1: NR NR through method even in 100 mL EE; recovered from GPC only, Florisil only. E2: NR Complete recovery if Florisil eluted with additional 100 mL EE. CP 108669 NR Some methylation, but does not elute from GPC. CP 92429 NR Does not methylate. CP 95200 NR Some methylation, but does not elute from GPC. CP 97290 NR Does not methylate. cyclanilide E1: C E2: V (45-67%) dicamba E1: P (71-76%) E2: C dichlorprop E1: C (80%) No ester reference standard. E2: C (72-104%) diclofop E1: S (43-51%) E2: V (81-200%) dinoseb E1: NR Does not methylate. E2: NR disul-Na E1: NR Does not methylate; parent 50% recovered if Florisil eluted with 100 mL EE. E2: NR Does not methylate; complete recovery of parent with 100 mL EE. DNOC E1: S (45-50%) Nitrogen detector required. No ether reference standard. E2: C dodine E1: NR Does not methylate. E2: NR fenac E1: C (74-92%) No ester reference standard. E2: C flumetsulam E1: NR Methylated product not soluble in hexane. E2: NR
TABLE 402-a Pesticide Analytical Manual Vol I Table 402-a: Recovery Through 402 (E1-E7+C1+ DG1 or DG3 or DG4) Chemical Notest. fluroxypyr El: S(29-30%) Two peaks result; 3-7% more eluted with100 mL EE. No ester ref std E2: P(64-77%) Two peaks result; complete recovery with 100 mL EE. No ester ref std haloxyfop E2:P(54%) Florisil elution with 100 mL eE not tested HOE038182 El: NR Methylation was complete, but ester not recovered E2: S(30-41%) Elution from Florisil only with eluant #2+ 100 mL EE HOE099730 R Does not methylate Methyl ester not eluted fromFlorisil ioxynil El: C(80-87%) No ether reference standard E2: C e urea Methyl ether not eluted from Florisil. MCPA E1:C(78-89%) E2: C MCPB El: C(70-106%) Chromatographs only on wide bore GLC. No ether reference standard E2: C mecoprop C(78-84%) Wide bore GLC recommended. No ester reference standard PB-7 El: NR Complete recovery if Florisil eluted with addi tional 100 mL EE E2: NR pentachlorophenol 70% mean recovery, 31%CV, n=275, nonfat and picloram El: NR 6-10% recovered if Florisil eluted with additional 100 mL EE E2: NR Complete recovery if Florisil eluted with additional 100 mL EE PPG-947 El: P(49-78%) Two peaks from methylation; only one seen by halogen detector pyrithiobac-sodium El: S(7-13%) Additional 31-34% recovered if Florisil eluted with 100 mI EE TABLE 402-a-4 Sonm FDA :2905a (6/92) Transr
TABLE 402-a Pesticide Analytical Manual Vol. I Transmittal No. 96-E1 (9/96) TABLE 402-a–4 Form FDA 2905a (6/92) Chemical Recovery1-3 Notes4,5 Table 402-a: Recovery Through 402 (E1-E7 + C1 + DG1 or DG3 or DG4) fluroxypyr E1: S (23-30%) Two peaks result; 3-7% more eluted with100 mL EE. No ester ref std. E2: P (64-77%) Two peaks result; complete recovery with 100 mL EE. No ester ref std. haloxyfop E2: P (54%) Florisil elution with 100 mL EE not tested. HOE-038182 E1: NR Methylation was complete, but ester not recovered. E2: S (30-41%) Elution from Florisil only with eluant #2 + 100 mL EE. HOE-099730 NR Does not methylate. imazamox NR Methyl ester not eluted fromFlorisil. ioxynil E1: C (80-87%) No ether reference standard. E2: C iprodione urea NR Methyl ether not eluted from Florisil. MCPA E1: C (78-89%) E2: C MCPB E1: C (70-106%) Chromatographs only on wide bore GLC. No ether reference standard. E2: C mecoprop E1: C (73-84%) Wide bore GLC recommended. No ester reference standard. E2: C PB-7 E1: NR Complete recovery if Florisil eluted with additional 100 mL EE. E2: NR pentachlorophenol E1: P 70% mean recovery, 31% CV, n=275, nonfat and fat. E2: P picloram E1: NR 6-10% recovered if Florisil eluted with additional 100 mL EE. E2: NR Complete recovery if Florisil eluted with additional 100 mL EE. PPG-947 E1: P (49-78%) Two peaks from methylation; only one seen by halogen detector. pyrithiobac-sodium E1: S (7-13%) Additional 31-34% recovered if Florisil eluted with 100 ml EE
Pesticide Analytical Manual Vol I TABLE 402-a Table 402-a: Recovery Through 402(E1-E7+C1+DG1 or DG3 or DG4) Chemical Recove notes RPA203328 Small(0-34%)recovery in 100 mL ethyl ether. El: C E2: C triadimenol El: NR Methyl ether not eluted from florisil E2. NR triclopyr El: c Recovery from fatty foods may be <50% E2: C vinclozolin metabolite b El: S(26-48%) Methylated product is parent vinclozolin; 62% recovery through Florisil only E2:S(27-43%) Transmittal No. 96-E1 [9/96) orm FDA 2905a(6/92 TABLE 402-8-5
Transmittal No. 96-E1 (9/96) Form FDA 2905a (6/92) TABLE 402-a–5 Pesticide Analytical Manual Vol. I TABLE 402-a Chemical Recovery1-3 Notes4,5 Table 402-a: Recovery Through 402 (E1-E7 + C1 + DG1 or DG3 or DG4) RPA203328 NR Small (0-34%) recovery in 100 mL ethyl ether. silvex E1: C E2: C triadimenol E1: NR Methyl ether not eluted from Florisil. E2: NR triclopyr E1: C Recovery from fatty foods may be <50%. E2: C vinclozolin metabolite B E1: S (26-43%) Methylated product is parent vinclozolin; 62% recovery through Florisil only. E2: S (27-43%)
TABLE 402-a Pesticide Analytical Manual Vol I TABLE 402-8-6 Transmittal No. 96-E1 [ 295a
TABLE 402-a Pesticide Analytical Manual Vol. I Transmittal No. 96-E1 (9/96)) TABLE 402-a–6 Form FDA 2905a (6/92)
