Pesticide Analytical Manual Vol. I Chapter 1 Regulatory Op Chapter 2 General Analytical Operations and Information Chapter 3 Chapter 4 Multiclass Selective MRMs MRMS Chapter 5 Chapter 6 Table of Contents page 301: Multiclass MRMs: Concept and application 301 A: Recommended Application of Multiclass MRMs 301-1 1/94 301 B: Capabilities and Limitations of MRMs 1/94 Influence of solvents on methodolo 3014 1/94 Extraction 30l-4 1/94 301-6 1/9 References 1/94 302: Method I for Nonfatty Foods Basic references 3021 l/94 enera 302-1 1/94 Method modules 3021 1/94 Form FDA 2905a(6/92) 300-1
Pesticide Analytical Manual Vol. I SECTION 100 300–1 Transmittal No. 2000-1 (10/1999) Form FDA 2905a (6/92) Table of Contents page date 301: Multiclass MRMs: Concept and Application 301 A: Recommended Application of Multiclass MRMs 301-1 1/94 301 B: Capabilities and Limitations of MRMs 301-4 1/94 Influence of Solvents on Methodology 301-4 1/94 Extraction 301-4 1/94 Cleanup 301-6 1/94 Determinative Steps 301-7 1/94 References 301-7 1/94 302: Method I for Nonfatty Foods Basic References 302-1 1/94 General Principles 302-1 1/94 Applicability 302-1 1/94 Method Modules 302-1 1/94 Validation 302-5 1/94 Chapter 1 Regulatory Operations Chapter 2 General Analytical Operations and Information Chapter 3 Multiclass MRMs Chapter 5 GLC Chapter 4 Selective MRMs Chapter 6 HPLC
Pesticide Analytical Manual Vol I page Extraction with acetone, liquid-liquid partitioning with petroleum ether/ methylene chloride 3027 1/94 E2 Extraction with acetone. removal of water with 40 g Hydromatrix 302-9 1/94 Extraction with acetone. removal of water with 25 g Hydromatrix 302-121/94 E4 Extraction with water/acetone, liquid-liquid partitioning with petroleum ether/ methylene chloride 302131/94 Extraction with acetone, liquid-liquid partitioning with acetone/methylene chloride 302-1510/99 E6 Extraction with water/acetone, liquid-liquid partitioning with acetone/methylene chloride 302-1510/99 E7 Extraction with acetone and solid phase extraction cartridges, liquid-liquid 302-1710/99 methylene chlorid s) cleanup, with one Florisil column (4 302-19 1/94 Charcoal/Celite/magnesium oxide column cleanup 30221 1/94 Charcoal/Silanized Celite column cleanup 302-29 1/94 C-18 cartridge cleanup 1/94 C5 Florisil column cleanup, with mixed ether eluants 302271/94 SAX/PSA cartridge cle 302-2910/99 Determinati 3023110/97 302-32 1/94 DGI GLC, 100% methyl siloxane, 200 C, EC 302331/94 DG2 GLC, 100% methyl siloxane, 2000C, FPD-P 302-95 10/97 DG9 GLC, 100% methyl siloxane, 200 C, ELCD-X 302-97 1/94 DG4 GLC, 100% methyl siloxane, 200 C, ELCD-N 302-39 1/94 DG5 GLC, 100% methyl siloxane, 200 C, N/P 3024 10/9 DG6 GLC, 100% methyl siloxane, 1300 C, FID 302-43 1/94 DG7 GLC, 100% methyl siloxane, 190 C,EC 302-451/94 DG8 GLC, 100% methyl siloxane, 130%C, FPD-P 30247 DG9 GLC, 100% methyl siloxane, 130% C, ELCD-X 302-49 1/94 DG10 GLC, 100% methyl siloxane, 290 C, EC 302511/94 DGll GLC, 100% methyl siloxane, 2300 C, FPD-P 802-53 1/94 DG12 GLC, 100% methyl siloxane, 2300 C, ELCD-X 302-55 1/94 DG18 GLC, 50% phenyl, 50% methyl siloxane, 200°C,EC 302571/94 302 ra2010
Transmittal No. 2000-1 (10/1999) 300–2 Form FDA 2905a (6/92) SECTION 100 Pesticide Analytical Manual Vol. I E1 Extraction with acetone, liquid-liquid partitioning with petroleum ether/ methylene chloride 302-7 1/94 E2 Extraction with acetone, removal of water with 40 g Hydromatrix 302-9 1/94 E3 Extraction with acetone, removal of water with 25 g Hydromatrix 302-12 1/94 E4 Extraction with water/acetone, liquid-liquid partitioning with petroleum ether/ methylene chloride 302-13 1/94 E5 Extraction with acetone, liquid-liquid partitioning with acetone/methylene chloride 302-15 10/99 E6 Extraction with water/acetone, liquid-liquid partitioning with acetone/methylene chloride 302-15 10/99 E7 Extraction with acetone and solid phase extraction cartridges, liquid-liquid partitioning 302-17 10/99 C1 Florisil column (4 g) cleanup, with one methylene chloride eluant 302-19 1/94 C2 Charcoal/Celite/magnesium oxide column cleanup 302-21 1/94 C3 Charcoal/Silanized Celite column cleanup 302-23 1/94 C4 C-18 cartridge cleanup 302-25 1/94 C5 Florisil column cleanup, with mixed ether eluants 302-27 1/94 C6 SAX/PSA cartridge cleanup 302-29 10/99 Determination 302-31 10/97 Confirmation 302-32 1/94 DG1 GLC, 100% methyl siloxane, 200° C, EC 302-33 1/94 DG2 GLC, 100% methyl siloxane, 200° C, FPD-P 302-35 10/97 DG3 GLC, 100% methyl siloxane, 200° C, ELCD-X 302-37 1/94 DG4 GLC, 100% methyl siloxane, 200° C, ELCD-N 302-39 1/94 DG5 GLC, 100% methyl siloxane, 200°␣ C, N/P 302-41 10/97 DG6 GLC, 100% methyl siloxane, 130° C, FID 302-43 1/94 DG7 GLC, 100% methyl siloxane, 130° C, EC 302-45 1/94 DG8 GLC, 100% methyl siloxane, 130° C, FPD-P 302-47 1/94 DG9 GLC, 100% methyl siloxane, 130° C, ELCD-X 302-49 1/94 DG10 GLC, 100% methyl siloxane, 230° C, EC 302-51 1/94 DG11 GLC, 100% methyl siloxane, 230° C, FPD-P 302-53 1/94 DG12 GLC, 100% methyl siloxane, 230° C, ELCD-X 302-55 1/94 DG13 GLC, 50% phenyl, 50% methyl siloxane, 200° C, EC 302-57 1/94 page date
Pesticide Analytical Manual Vol. I da DG14 GLC, 50% phenyl, 50% methyl siloxane 200°C,FPD-P 302-5910/97 DG15 GLC, 50% phenyl, 50% methyl siloxane 230°C.FPDS 302611/94 DG16 GLC, 50% phenyl, 50% methyl siloxane, 200°C, ELCD-X 302-63 1/94 DG17 GLC, 50% phenyl, 50% methyl siloxane 200°C.N 3026510/97 DG18 GLC, 50% cyanopropylphenyl, 50% methyl siloxane,200°C,EC 302-671/94 DG19 GLC, 50% cyanopropylphenyl, 50% methy siloxane,200°C,FPD-P 302691/94 303: Method I for nonfatty Foods Basic references 303-1 1/94 General Principles 303-1 1/94 Applicability 303-1 1/94 Method modules 303-1 1/94 Validation 303-3 1/94 El Extraction with acetonitrile, partition into 303-7 l/94 E2 Extraction from eggs with acetonitrile partition into petroleum ether 303-8 1/94 Extraction with 35 water/acetonitrile, partition into petroleum ether 303-9 1/94 E4 Extraction with acetonitrile and water partition into petroleum ether 1/94 Extraction with heated acetonitrile and water,partition into petroleum ether 303-101/94 Florisil column cleanup, with three ethyl ether/petroleum ether eluants 303-111/94 Florisil column cleanup, with three methylene chloride eluants 303-121/94 Determination 303-131/94 303-131/94 304: Method for Fatty Foods Basic reference 304-1 1/94 General Principles 304-1 1/94 Method modules 304-1 1/94 Validation 304-3 1/94 El Extraction of fat with sodium sulfate petroleum ether 04-5 1/94 E2 Small scale extraction of fat with sodiun ulfate, petroleum ether 300-3
Pesticide Analytical Manual Vol. I SECTION 100 300–3 Transmittal No. 2000-1 (10/1999) Form FDA 2905a (6/92) DG14 GLC, 50% phenyl, 50% methyl siloxane, 200° C, FPD-P 302-59 10/97 DG15 GLC, 50% phenyl, 50% methyl siloxane, 230° C, FPD-S 302-61 1/94 DG16 GLC, 50% phenyl, 50% methyl siloxane, 200° C, ELCD-X 302-63 1/94 DG17 GLC, 50% phenyl, 50% methyl siloxane, 200° C, N/P 302-65 10/97 DG18 GLC, 50% cyanopropylphenyl, 50% methyl siloxane, 200° C, EC 302-67 1/94 DG19 GLC, 50% cyanopropylphenyl, 50% methyl siloxane, 200° C, FPD-P 302-69 1/94 303: Method II for Nonfatty Foods Basic References 303-1 1/94 General Principles 303-1 1/94 Applicability 303-1 1/94 Method Modules 303-1 1/94 Validation 303-3 1/94 E1 Extraction with acetonitrile, partition into petroleum ether 303-7 1/94 E2 Extraction from eggs with acetonitrile, partition into petroleum ether 303-8 1/94 E3 Extraction with 35% water/acetonitrile, partition into petroleum ether 303-9 1/94 E4 Extraction with acetonitrile and water, partition into petroleum ether 303-9 1/94 E5 Extraction with heated acetonitrile and water, partition into petroleum ether 303-10 1/94 C1 Florisil column cleanup, with three ethyl ether/petroleum ether eluants 303-11 1/94 C2 Florisil column cleanup, with three methylene chloride eluants 303-12 1/94 Determination 303-13 1/94 Confirmation 303-13 1/94 304: Method for Fatty Foods Basic Reference 304-1 1/94 General Principles 304-1 1/94 Applicability 304-1 1/94 Method Modules 304-1 1/94 Validation 304-3 1/94 E1 Extraction of fat with sodium sulfate, petroleum ether 304-5 1/94 E2 Small scale extraction of fat with sodium sulfate, petroleum ether 304-7 1/94 page date
Pesticide Analytical Manual Vol I date Es Extraction of fat by filterin 3049 1/94 E4 Extraction of fat with solvents from denatured 30411 1/94 Extraction of fat with solvents 30413 1/94 Florisil column cleanup, three mixed, Acetonitrile-petroleum ether partitioni ether eluants 30415 1/94 C2 Acetonitrile-petroleum ether partitioning, Florisil column cleanup, three methylene chloride eluants 30418 1/94 Acetonitrile-petroleum ether partitioning, Florisil column cleanup, petroleum ether 30419 Acetonitrile-petroleum ether partitioning, Florisil column cleanup, petroleum ether and three methylene chloride eluants 30419 1/94 Gel 304-21 1/94 C6 GPC, Florisil column(4 g)cleanup, three methylene chloride eluants 30424 1/94 C7 Florisil column(4 g) cleanup, two mixed ether eluants, optional alkaline hydrolysis 304-271/94 Dispersion on alumina, Florisil column cleanup, three mixed ether eluants 304-29 1/94 c9 Dispersion on alumina, Florisil column leanup, three methylene chloride eluants Determination 304-33 1/94 Confirmation 304-33 1/94 Fi 1g ures 801-a Recommended Approach to Analysis of Foods 301-2 1/94 Recommended approach: Nonfatty Foods 3024 10/99 3-a Recommended Approach: Nonfatty Foods 804-a Recommended Approach: Fatty Foods 304-3 1/94 804-b Delivery Tube Apparatus 304-12 Tables 302-a: Recovery of Chemicals Through Method 302 (E1E3+DG1-DG19) 302-a-1 802-b: Recovery of Chemicals Through Method 302 (El-E3+C5+ DGl-DG19 302b-19/96 302-C: Recovery of Chemicals Through Method 302 El-E8+C3+ DLl) 302c-19/96 302-d: Recovery of Chemicals Through Method 302 (E2/E3+C1+DG1DG19) 30o4 ra2010
Transmittal No. 2000-1 (10/1999) 300–4 Form FDA 2905a (6/92) SECTION 100 Pesticide Analytical Manual Vol. I E3 Extraction of fat by filtering 304-9 1/94 E4 Extraction of fat with solvents from denatured product 304-11 1/94 E5 Extraction of fat with solvents 304-13 1/94 C1 Acetonitrile-petroleum ether partitioning, Florisil column cleanup, three mixed ether eluants 304-15 1/94 C2 Acetonitrile-petroleum ether partitioning, Florisil column cleanup, three methylene chloride eluants 304-18 1/94 C3 Acetonitrile-petroleum ether partitioning, Florisil column cleanup, petroleum ether and three mixed ether eluants 304-19 1/94 C4 Acetonitrile-petroleum ether partitioning, Florisil column cleanup, petroleum ether and three methylene chloride eluants 304-19 1/94 C5 Gel permeation chromatography (GPC) 304-21 1/94 C6 GPC, Florisil column (4 g) cleanup, three methylene chloride eluants 304-24 1/94 C7 Florisil column (4 g) cleanup, two mixed ether eluants, optional alkaline hydrolysis 304-27 1/94 C8 Dispersion on alumina, Florisil column cleanup, three mixed ether eluants 304-29 1/94 C9 Dispersion on alumina, Florisil column cleanup, three methylene chloride eluants 304-32 1/94 Determination 304-33 1/94 Confirmation 304-33 1/94 Figures 301-a Recommended Approach to Analysis of Foods 301-2 1/94 302 Recommended Approach: Nonfatty Foods 302-4 10/99 303-a Recommended Approach: Nonfatty Foods 303-3 1/94 304-a Recommended Approach: Fatty Foods 304-3 1/94 304-b Delivery Tube Apparatus 304-12 1/94 Tables 302-a: Recovery of Chemicals Through Method 302 (E1-E3 + DG1-DG19) 302-a-1 9/96 302-b: Recovery of Chemicals Through Method 302 (E1-E3 + C5 + DG1-DG19) 302-b-1 9/96 302-c: Recovery of Chemicals Through Method 302 E1-E3 + C3 + DL1) 302-c-1 9/96 302-d: Recovery of Chemicals Through Method 302 (E2/E3 + C1 + DG1-DG19) 302-d-1 9/96 page date
Pesticide Analytical Manual Vol. I page 302-e: Recovery of Chemicals Through Method 302 (El/E4+C4+DLl) 302e-19/96 302-f: Recovery of Chemicals Through Method 302 (E7+C6+ DGl-DG%, DG6-DG7, DG10 DG18-DGl4, or DG16) 302f-1 303-a: Recovery of Chemicals Through Method 303 (El-E5+Cl or C2+DGl-DG19) 303-a-19/96 304-a: Recovery of Chemicals Through Method 304 El-E5+C1-C4+ DG1-Dg19 304-a-19/96 304-b: Recovery of Chemicals Through Method 304 (E1-E5+C6+DG1-DG19) 04b-19/96 304-c: Recovery of Chemicals Through Method 304 (E2+C7+DG1-DG19) 304 9/96 FDA2905a[6/92 3005
Pesticide Analytical Manual Vol. I SECTION 100 300–5 Transmittal No. 2000-1 (10/1999) Form FDA 2905a (6/92) 302-e: Recovery of Chemicals Through Method 302 (E1/E4 + C4 + DL1) 302-e-1 9/96 302-f: Recovery of Chemicals Through Method 302 (E7 + C6 + DG1-DG3, DG6-DG7, DG10, DG13-DG14, or DG16) 302-f-1 10/99 303-a: Recovery of Chemicals Through Method 303 (E1-E5 + C1 or C2 + DG1-DG19) 303-a-1 9/96 304-a: Recovery of Chemicals Through Method 304 (E1-E5 + C1-C4 + DG1-DG19) 304-a-1 9/96 304-b: Recovery of Chemicals Through Method 304 (E1-E5 + C6 + DG1-DG19) 304-b-1 9/96 304-c: Recovery of Chemicals Through Method 304 (E2 + C7 + DG1-DG19) 304-c-1 9/96 page date