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U.S. Department of Agriculture
Food Safety and Inspection Service
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NATIONAL RESIDUE PLAN FOR 1998

APPENDIX II

FSIS RESIDUE ANALYTICAL CAPABILITY

|Albendazole - Halofuginone | HCB - Zinc | References|

Compound

Method Description

LDL/MIC

MPL

Species/Tissues

Ref.

Albendazole (amino sulfone metabolite)

Marker residue detected and quantified by HPLC- fluorescence detection

20 ppb

50 ppb

Cattle/liver Cattle/muscle Sheep/muscle

1

Extraction with organic solvents followed by HPLC with UV detection; confirmed by GC/EI/MS

0.05 ppm

NE

Red meat liver, muscle

1

Aldicarb and Metabolites

GPC plus HPLC with post- column fluorescence detection; extracts verified by oxidation to the sulfone

5 ppb

10 ppb

All/liver

1

Aldrin

Micro alumina assay: column chromatography plus GLC

0.02 ppm

NE

All/fat pp

1

GPC plus GLC

0.02 ppm

0.05 ppm

All/fat

1

Mills method: Florisil column chromatography plus GLC

0.02 ppm

0.10 ppm

All/fat pp

1

Extracts from GPC or Mills confirmed by GC/MS.

0.03 ppm

NE

All/fat,PP

1

Compound

Method Description

LDL/MIC

MPL

Species/Tissues

Ref.

Amoxicillin

Trihydrate

Microbiological assay procedure: ability of tissue extracts containing antimicrobial activity to inhibit microbial growth

0.02 ppm

0.02 ppm

Cattle, swine/ kidney,liver, muscle

2

 

Tissue extracts quantified by HPLC using fluorometer

0.01 ppm

0.01 ppm

Cattle, swine/ kidney,liver, muscle

1

 Ampicillin

Ampicillin

Trihydrate

Microbiological assay procedure: ability of tissue extracts containing antimicrobial activity to inhibit microbial growth

 

 

0.01 ppm

0.01 ppm

Cattle, swine/ all

3

Apramycin

Sample extraction TLC; bioautographed using Bacillus subtilis as a test organism

0.05 ppm

0.1 ppm

Swine/kidney ,muscle

1

 Arsanilate sodium Arsanilic acid

Arsenate, Calcium

Arsenate, Copper  Arsenate, Lead Arsenate, Magnesium Arsenate, Sodium Arsenic,Arsenite, Potassium Arsenite,

Dry ashed tissue dissolved and reacted to produce arsine gas, which is quantified by AAS

Dry ashed tissue dissolved and reacted to produce arsine gas, which reacts to form blue complex for colorimetric quantification

0.05 ppm

 

0.05 ppm

NE

 

0.20 ppm

All/kidney, liver,muscle

 

All/kidney, liver, muscle

1

 

1

Atrazine

Fat extracted using C18 columns and quantified by capillary GC with nitrogen/ phosphorous detector.

Extracts confirmed by GC/MS

5 ppb

 

 

5 ppb

NE

 

 

NE

All/fat

 

 

All/fat

1

 

 

1

Bacitracin methylene disalicylate

Bacitracin, zinc

Microbiological assay procedure: ability of tissue extracts containing antimicrobial activity to inhibit microbial growth

0.05 ppm

NE

All/kidney, liver, muscle

4

Bambermycins

Microbiological assay procedure: ability of tissue extracts containing antimicrobial activity to inhibit microbial growth

25 ppb

NE

All/kidney, liver, muscle,

5

Bendiocarb

GPC plus HPLC with post-column fluroescence detection.

5 ppb

10 ppb

All/liver

1

Compound

Method Description

LDL/MIC

MPL

Species/Tissues

Ref.

 Benomyl

pH extraction with organic solvents; followed by HPLC ppm with UV detection; extracts derivatizedand confirmed by GC/EI/MS

0.05 ppm

NE

Poultry/ liver, muscle

1

BHC

Micro alumina assay: column chromatography plus GLC

0.01 ppm

NE

All/fat,PP

1

GPC plus GLC

0.01 ppm

0.05 ppm

All/fat

1

Beta and delta isomers: GPC plus GLC

0.02 ppm

0.05 ppm

All/fat

1

Mills method: Florisil column chromatography plus GLC

0.02 ppm

0.10 ppm

All/fat, PP

1

Extracts from GPC or Mills confirmed by GC/MS

0.02 ppm

NE

All/fat, PP

1

Bufencarb

GPC plus HPLC with post- column fluorescence detection. Extracts are subjected to reverse phase chromatography, derivativized and confirmed by GC/MS

5 ppb

10 ppb

All/liver

1

Cacodylic acid

Dry ashed tissue is dissolved and reacted to produce arsine gas, which reacts to form bluecomplex for colorimetric quantification

0.05 ppm

0.20 ppm

All/kidney, liver, muscle

6

Cadmium

 

Dry ashed tissue is dissolved and quantified by AAS or by inductively coupled plasma

0.5 ppd

NE

All/kidney , liver, muscle

1

Dry ashed tissue is quantified by anodic stripping voltammetry

4 ppb

1.0 ppb

NE

NE

Poultry, kidney, liver

7

 Calcium  

Tissue is wet ashed and titrated with specific indicator

Wet ashed tissue is quantified by AAS

0.03%

NE

0.03%

NE

All/muscle

All

8

Cambendazole

 

Extraction with organic solvents followed by HPLC with UV detection; extracts confirmed by GC/EI/MS

0.05 ppm

NE

Red meat/ liver, muscle, PP

1

 Captan

 

GPC plus GLC

0.02 ppm

0.05 ppm

Red meat/fat

1

Carbadox

 

 

Tissue extract is hydrolyzed and a derivative is prepared and separated by ion exclusion chromatography, then quantified by GC-ECD

Extracts confirmed by GC/EI/MS

7.5 ppb

 

 

7.5 ppb

30 ppb

 

 

NE

Swine/ liver, muscle

 

 

Swine/ liver, muscle

1

 

 

1

Compound

Method Description

LDL/MIC

MPL

Species/Tissues

Ref.

Carbarsone

Dry ashed tissue is dissolved and reacted to produce arsine gas, which reacts to form blue complex for colorimetric quantification

0.05 ppm

0.20 ppm

All/kidney, liver, muscle

9

 Carbaryl

GPC plus HPLC with post- column fluorescence detection

Extracts are subjected to reverse phase chromatography, derivativized and confirmed by GC/MS

5 ppb

10 ppb

All/liver

1

Carbofuran and metabolite

GPC plus HPLC with post- column fluorescence detection.

Extracts are subjected to reverse phase chromatography, derivativized and confirmed by GC/MS

5 ppb

10 ppb

All/liver

1

Carbophenothion

Tissue extracts are quantified by GLC with flame photometric or nitrogen-phosphorous flame ionization detector

0.10 ppm

NE

All/liver, muscle

 

GPC plus GLC

0.03 ppm

0.20 ppm

All/fat

1

1

GPC extracts are confirmed by CG/EI/MS

0.01 ppm

NE

Red meat/fat

 Chloramphenicol

Tissue extracts are screened by E-Z screen

25 ppb

NE

Calf/ muscle, kidney

10

Tissue extract screened for chloramphenicol by CELIA CA

5ppb

NE

Calf/ muscle

11

Extraction of parent and glucuronide using C18 columnswith GC capillary quantification as the trimethylsilyl derivative

0.15 ppb

NE

Calf/muscle

1

Extracts are confirmed using NICI/MS

0.15 ppb

NE

Calf/muscle

1

C18 cleanup of the hydrolyzed extract with GC capillary quantification as the trimethyl derivative

5 ppb

NE

Calf/urine

1

Extracts are confirmed using NICI/MS

5 ppb

NE

Calf/urine

1

Chlordane

Micro alumina assay: column chromatography plus GLC

GPC followed by GC-ECD

0.15 ppm

0.10 ppm

0.50 ppm

0.30 ppm

All/fat, PP

All/fat

1

1

Mills method: Florisil column chromatography plus GLC

0.15 ppm

0.30 ppm

All/fat, PP

1

Extracts from GPC or Millsare confirmed by GC/MS

NE

NE

All/fat, PP

1

Chlordecone

(Kepone)

GPC plus GLC

0.03 ppm

0.20 ppm

All/fat

1

GPC extracts are confirmed by GC/EI/MS

 

0.05 ppm

(poultry)

0.20 ppm

(cattle)

NE

Poultry, red meat/fat

1

Compound

Method Description

LDL/MIC

MPL

Species/Tissues

Ref.

 2-Chloro-1-(2,4,-di- chlorophenyl) vinyl diethyl phosphate

(chlorfenvinphos)

GPC plus GLC

GPC extracts are confirmed by CG/EI/MS

0.03 ppm

0.01 ppm (poultry)

0.10 ppm (red meat)

0.10 ppm

NE

Cattle, sheep/fat

Poultry, red meat/fat

1

1

2-Chloro-1-(2,4,5-tri-vinyl dimethyl phosphate

(stirophos)

GPC plus GLC

0.05 ppm

0.30 ppm

All/fat

1

 

GPC extracts are confirmed by GC/EI/MS

0.05 ppm (poultry)

0.10 ppm (cattle)

NE

Poultry, red meat/fat

1

Chlorpyrifos

GPC followed by GC-ECD

0.05 ppm

0.20 ppm

All/fat

1

GPC extracts are confirmed by GC/EI/MS

0.05 ppm (poultry)

0.50 ppm (swine)

NE

Poultry,swine/ fat

1

Chlortetracycline

Antibiotic screen test (Swab): ability of tissue fluids containing anti- microbial activity toinhibit microbial growth

0.01 ppm

NE

All/kidney

12

Microbiological assay procedure: ability of tissue extracts containing antimicrobial activity to inhibit microbial growth 

0.01 ppm

NE

All/kidney liver, muscle

13

Extraction using C18 columns followed by HPLC with UV detection

0.15 ppm

0.25 ppm

All/kidney liver, muscle

1

Chromium

Dry ashed tissue is extracted with organic reagent and quantified using AAS

NE

NE

All/kidney liver, muscle

1

Clopidol

Organic solvent extraction with HPLC-UV detection

0.1

NE

Poultry/liver ppm

1

Organic solvent extraction with GC-EC detection

0.1 ppm

NE

Poultry/liver

1

 Clorsulon

Tissue extracts are quantified by HPLC-UV detection

Tissue extracts for HPLCare derivatized and confirmed by GC/MS

0.25 ppm

0.5 ppm

 

0.50 ppm

NE

Red meat kidney, muscle, liver,PP

Red meat/ kidney, muscle, liver, PP

1

1

Cloxacillin

Antibiotic screen test(Swab): ability of tissue fluids containing anti- microbial activity to inhibit microbial growth

Microbiological assay combined with HPLC separation andquantified by microbial inhibition

0.16 ppm

 

 

0.02 ppm

NE

 

 

NE

All/kidney

 

 

Dairy cows/ kidney, liver, muscle

16

 

 

17

Cobalt

Dry ashed tissue is dissolved and quantified by AAS or by inductively coupled plasma

6 ppb

6 ppb

NE

NE

All/kidney, liver, muscle

All/kidney, liver, muscle

 

Compound

Method Description

LDL/MIC

MPL

Species/Tissues

Ref.

Copper

Dry ashed tissue is dissolved and quantified by AAS or by inductively coupled plasma

1 ppb

3 ppb

NE

NE

All/kidney, liver, muscle

All/kidney, liver, muscle

1

Coumaphos and oxygen analog

Tissue extracts are quantified by GLC with flame photometric or nitrogen-phosphorous flame ionization detector

0.10 ppm

NE

All/liver, muscle

1

GPC followed by GC-ECD

GPC extracts are confirmed by CG/EI/MS

0.15 ppm

0.20 ppm

0.30 ppm

0.30 ppm

All/fat

Red meat/fat

1

1

Cresylic acid

Tissue extracts are derivatized and determined by GC-EC

NE

NE

Poultry/fat

1

Crufomate (Ruelene)

Tissue extracts are quantified by GLC with flame photometric or nitrogen-phosphorous flame ionization detector

0.10 ppm

NE

All/liver, muscle

1

Cyanide salts

Aqueous extraction followed by a colori- metric determination

0.5 ppm

NE

All/all

1

For confirmation, cyanogen chloride is produced and determined by GC/EC

0.5 ppm

NE

All/all

1

Cyano (3-phenoxy chlorophenyl) methyl- 4-a-(methylethyl) - benzeneacetate

[fenvalerate]

Organic solvent extracts are quantified as the sum of both isomers by GC/EC; extracts areconfirmed by GC/EI/MS

0.03 ppb

NE

All/fat

1

DDE (metabolites of DDT collectively reported as DDT)

Micro alumina assay:column chromatography plus GLC

GPC followed by GC-ECD

0.02 ppm

0.02 ppm

0.50 ppm

0.05 ppm

All/fat, PP

All/fat

1

1

Mills method: Florisil column chromatographyplus GLC

0.02 ppm

0.10 ppm

All/fat, PP

1

Extracts from GPC or Mills are confirmed by GC/MS (LRC)

0.02 ppm

NE

All/fat,PP

1

DDT

(isomers of DDT collectively reported as DDT)

Micro alumina assay: column chromatography plus GLC

GPC followed by GC-ECD

0.30 ppm

0.04 ppm

0.50 ppm

0.15 ppm

All/fat, PP

All/fat

1

1

Mills method:Florisil column chromatographyplus GLC

0.04 ppm

0.15 ppm

All/fat,PP

1

Decoquinate

Zymark Pytechnology System; organic solvent extraction followed by HPLC with fluorescence detection

0.20ppm

0.50 ppm

Cattle, poultry/ liver, muscle

14

Compound

Method Description

LDL/MIC

MPL

Species/Tissues

Ref.

Deltamethrin

Organic solvent extracts are quantified by GC/EC;

Solvent extraction followed by a competitive ELISA determination

0.025 ppm

0.5 ppm

NE

NE

All/fat

All/fat

1

Diazinon

Tissue extracts are quantified by GLC with flame photometric or nitrogen-phosphorous flame ionization detector

0.1 ppm

NE

All/liver, muscle

1

Dibutyltin dilaurate

Tissue extraction acidhydrolysis-morin derivatization--HPLC-UV

0.25 ppm

NE

Turkey/liver

1

Dieldrin

Micro alumina assay: column chromatographyplus GLC

GPC plus GLC

0.01 ppm

0.01 ppm

NE

0.05 ppm

All/fat,PP

All/fat

1

1

Mills method: Florisil column chromatography

0.01 ppm

0.10 ppm

All/fat,PP

1

Extracts from GPC or Mills are confirmed by GC/MS

0.02 ppm

NE

All/fat,PP

1

Diethylstilbestrol (DES)

Solid phase extraction technique using an internal standard followed by methylsilation for GC/MS quantification and confirmation

0.1 ppb

0.2 ppb

Cattle, sheep liver, muscle

1

Dihydrostreptomycin

Antibiotic screen test (Swab): ability of tissue fluids containing anti-microbial activity to inhibit microbial growth

0.25 ppm

NE

All/kidney

12

Microbiological assay procedure: ability of tissue extracts containing antimicrobial activity toinhibit microbial growth

0.25 ppm

NE

All/kidney, liver, muscle

18

3, 5-Dimethyl-4-(methylthio)phenyl methylcarbamate and metabolite

GPC plus HPLC with post- column fluorescence detection Extracts are subjected to reverse phase chromatography, derivatized and confirmedby GC/MS

5 ppb

10 ppb

All/liver

1

Dimetridazole and hydroxy metabolite

Extracts are quantified by HPLC/UV

Tissue extracts from HPLC are confirmed by GC/NICI/MS

1.0ppb

1.0 ppb

NE

NE

Turkey, swine/ muscle

Turkey, swine/ muscle

14

14

Dioxacarb

GPC plus HPLC with post- column fluorescence detection

Extracts are subjected to reverse phase chromatography, derivativized and confirmed by GC/MS

5 ppb

10 ppb

All/liver

1

Dioxathion

Tissue extracts are quantified by GLC with flame photometric or nitrogen-phosphorous flame ionization detector

0.10 ppm

NE

All/liver, muscle

 

 Dodecachloro- octahydro-1,3,4- metheno-2H- cyclobuta(cd)- pentalene[Mirex]

Micro alumina assay: column chromatography plus GLC

GPC plus GLC

Mills method: Florisil column chromatography plus GLC

Extracts from GPC or Mills are confirmed by GC/MS

0.04 ppm

0.04 ppm

 

0.04 ppm

 

0.05 ppm

NE

0.10 ppm

 

0.10 ppm

 

NE

All/fat, PP

All/fat

 

All/fat,PP

 

All/fat,PP

1

 

 

1

 

1

Compound

Method Description

LDL/MIC

MPL

Species/Tissues

Ref.

Endosulfan I

GPC plus GLC

GPC extracts are confirmed by GC/EI/MS

0.01ppm

0.02ppm

0.10ppm

NE

All/fat

Red meat/fat

1

Endosulfan II

GPC plus GLC

0.02ppm

0.20 ppm

 

All/fat

 

1

 

Endrin

Micro alumina assay: column chromatography plus GLC

0.03 ppm

NE

All/fat,PP

1

Mills method: Florisilcolumn chromatography plus GLC

0.03 ppm

0.10 ppm

All/fat, PP

1

Extracts from GPC or Mills are confirmed by GC/MS

0.05 ppm

NE

All/fat,PP

1

Erythromycin

Antibiotic screen test (Swab): ability of tissue fluids containing antimicrobial activity to inhibit microbial growth

25 ppb

NE

All/kidney

12

Microbiological assay procedure: ability of tissue fluids containing antimicrobial activity to inhibit microbial growth

25 ppb

NE

All/kidney, liver, muscle

19

Ethion and oxygen analog

Tissue extracts are quantified by GLC with flame photometric or nitrogen-phosphorous flame ionization detector

0.10 ppm

NE

All/liver, muscle

1

Tissue extracts are quantified by GLC with flame photometric or nitrogen-phosphorous flame ionization detector

NE

NE

All/liver muscle

1

Ethylene dibromide

Residue is co-distilled from aqueous suspension and quantified by GLC

0.5 ppb

1.0 ppb

All/fat

1

MS by NICI to determine bromine

1 ppb

NE

All/fat

1

Fenbendazole

Extraction with organic solvents followed by HPLC with UV detection; extracts derivatized and confirmed by GC/EI/MS

0.10 ppm

NE

Red meat/ liver, muscle

1

Tissue extracts are quantifiedby HPLC

200 ppb

400 ppb

Cattle, calf/ liver

20

Quantification extract purified by TLC, derivatized and identified by HPLC fluorescence

200 ppb

NE

Cattle, calf/ liver

20

Compound

Method Description

LDL/MIC

MPL

Species/Tissues

Ref.

Fenitrothion

Tissue extracts are quantified by GLC with flame photometric or nitrogen- phosphorous flame ionization detector

0.10 ppm

NE

All/liver, muscle

1

Fenpropathrin

Solvent extraction followed by a competitive ELISA determination

1.0 ppm

NE

All/fat

14

Flucythrinate

Organic solvent extracts are quantified as the sum of both isomers by GC/EC; extracts are confirmed by GC/EI/MS

1 ppm

NE

All/fat

1

Solvent extraction followed by a competitive ELISA determination

1.0 ppm

NE

All/fat

1

Gasoline

 Fat from product is heated in a sealed vial and gasoline components are identified by pattern recognition using GC/flame ionization detection

0.1 ppm

NE

All/muscle

1

Gentamicin sulfate

Tissue extracts are screened by E-Z Screen

Microbiological assay procedure: ability of tissue extracts containing antimicrobial activity to inhibit microbial growth

50 ppb

 

NE

NE

 

NE

All/muscle liver, kidney

 

Swine/kidney

21

 

22

Extraction followed by detection by HPLC with fluorescence detector

0.2 ppm

0.4 ppm

Swine/kidney

1

Halofuginone

Tissue extracts are quantified by HPLC-UV

0.05 ppm

0.05 ppm

Chicken/liver, muscle

1

Tissue extracts are confirmed by GC/MS/MS

0.05 ppm

NE

Chicken/liver, muscle

23

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URL: http://www.usda.gov/fsis/ophs/bluebook/racahal.htm
Last Updated On 03/09/1998.