USGS-NWQL: O-9125-94: Chlorinated pesticides in aquatic tissue by dual capillary-column gas chromatography with electron-capture detection

Summary
Analytes
Revision
Data and Sites

Official Method Name

Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory - Determination of Chlorinated Pesticides in Aquatic Tissue by Capillary-Column Gas Chromatography with Electron-Capture Detection

Current Revision

1994

Media

ANIMAL TISSUE

Instrumentation

Gas Chromatography with Electron Capture Detection

Method Subcategory

Organic

Method Source

USGS-NWQL

Citation

Leiker, T.J., J.E. Madsen, J.R. Deacon and W.T. Foreman, 1995, Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of chlorinated pesticides in aquatic tissue by capillary-column gas chromatography with electron-capture detection: U.S. Geological Survey Open-File Report 94-710.

Brief Method Summary

Whole-body-fish or corbicula tissue is homogenized into a single composite. A 10-g sample aliquot of homogenized tissue material is Soxhlet extracted and the extract is reduced to a volume of 5.0 mL. A 1-mL aliquot is removed for percentage lipid determination. A 2-mL aliquot of the extract is injected into a gel permeation chromatograph (GPC) to separate the lipid material and other interferences from the method compounds. After the compounds have been collected from the GPC, the extract is solvent exchanged into hexane, separated into two fractions on a column packed from top to bottom with 1 cm of sodium sulfate, 5 g of 8.5 percent water-deactivated alumina, 3 g of 2 percent water-deactivated silica, and 0.5 cm of sodium sulfate. The first fraction contains the PCBs, DDE, and other nonpolar organics. The second fraction contains toxaphene, chlordane compounds, DDT, DDD, and other more polar organic compounds. Each fraction is concentrated to a volume of 1 mL and analyzed by dual capillary column gas chromatography with electron-capture detection.

Scope and Application

This method is suitable for the determination of 28 organochlorine-containing pesticides and industrial chemicals in whole-body fish and corbicula tissue at concentrations of 5 ug/kg for chlorinated pesticides, 50 ug/kg for PCBs, and 200 ug/kg for toxaphene. The method is applicable for those hydrophobic compounds that exhibit Log K_OW >4.

Applicable Concentration Range

Organochlorine pesticides at 5 ug/kg, PCBs at 50 ug/kg, and toxaphene at 200 ug/kg

Interferences

Compounds recovered from a sample matrix, which have chemical and physical properties that are similar to but are not chromatographically resolved from the compounds of interest, can interfere.

Quality Control Requirements

Calibration standards, surrogate standards, Retention time marker solution, Continuous calibration verification (CCV) standards, Performance evaluation mix (PEM) standards, GPC system performance verification standard.

Sample Handling

Collect fish and corbicula samples according to guidelines set forth by Crawford and Luoma (1993). Briefly, collect fish samples by electroshocking, wrap in aluminum foil, freeze, and ship frozen to NWQL. Collect corbicula samples, depurate for 22 hours, wrap in aluminum foil, and ship frozen to NWQL.

Maximum Holding Time

Relative Cost

Greater than $400

Sample Preparation Methods

Soxlet extraction, gel permeation chromatography, alumina/silica fractionation

This method has 26 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
2,4' -DDD(53-19-0) 1,1-Dichloro-2,2-bis(2,4'-dichlorophenyl)ethane 1,1-Dichloro-2-(o-chlorophenyl)-2-(p-chlorophenyl)ethane 2,4' -DDD 2,4'-Dichlorodiphenyldichloroethane o,p'-DDD o,p'-TDE	0.300 ug/kg	67% Rec (SL)	6.30 RSD (SL)	2.50 ug/kg
2,4'-DDE(3424-82-6) 1,1-Dichloro-2-(o-chlorophenyl)-2-(p-chlorophenyl) ethylene 1-chloro-2-(2,2-dichloro-1-(4-chlorophenyl)ethenyl)benzene 2,4'-DDE o,p'-DDE	N/A	N/A	N/A	2.50 ug/kg
4,4'-DDD(72-54-8) 1,1-Dichloro-2,2-bis(p-chlorophenyl)ethane 4,4'-DDD Benzene, 1,1'-(2,2-dichloroethylidene)bis[4-ch Benzene, 1,1'-(2,2-dichloroethylidene)bis[4-chloro- Dichloro-2,2-bis(p-chlorophenyl)ethane,1,1- Dichlorodiphenyldichloroethane Ethane, 1,1-dichloro-2,2-bis(p-chlorophenyl)- Rhothane TDE Tetrachlorodiphenylethane p,p'-DDD p,p'-Dichlorodiphenyl dichloroethane p,p'-TDE	1.600 ug/kg	80% Rec (SL)	25.90 RSD (SL)	2.50 ug/kg
4,4'-DDE(72-55-9) 1,1'-(-Dichloroethenylidene)bis(4-chlorobenzene) 4,4'-DDE 4,4'-DDE, DDT, DDD Benzene, 1,1'-(dichloroethenylidene)bis[4-chlo Benzene, 1,1'-(dichloroethenylidene)bis[4-chloro- Ethylene, 1,1-dichloro-2,2-bis(p-chlorophenyl)- bis(p-Chlorophenyl)-1,1-dichloroethylene,2,2- p,p'-DDE p,p'-Dichlorodiphenyldichloroethylene	N/A	64% Rec (SL)	15.60 % RSD (SL)	2.50 ug/kg
Aldrin(309-00-2) Aldrex Aldrin Aldrin-R Aldrite Aldrosol HHDN Hexachlorohexahydro-endo-exo-dimethanonaphthalene Octalene Seedrin liquid	0.200 ug/kg	54% Rec (SL)	3.99 RSD (SL)	2.50 ug/kg
DCPA(1861-32-1) Chlorothal Chlorthaldimethyl DCPA Dacthal Dimethyl tetrachloroterephthalate Dimethyl-2,3,5,6-tetrachlorotephthalate Tetrachloroterephthalic acid, dimethyl ester	0.400 ug/kg	94% Rec (SL)	4.88 RSD (SL)	2.50 ug/kg
Dieldrin(60-57-1) 1,2,3,4,10,10-Hexachloro-6,7-epoxy-1,4,4a,5, 6 1,2,3,4,10,10-Hexachloro-6,7-epoxy-1,4,4a,5, 6,7,8, ... 2,7:3,6-Dimethanonaphth(2,3-b)oxirene, 3,4,5,6 2,7:3,6-Dimethanonaphth(2,3-b)oxirene, 3,4,5,6,9,9- ... Alvit Dieldrin Dieldrin (hexachloroepoxyoctahydro-endo,exo- ... Dieldrin/aldrin Dimethanonaphthalene, 1,2,3,4,10,10-hexachloro-6,7- ... Heod Octalox	0.600 ug/kg	67% Rec (SL)	11.20 RSD (SL)	2.50 ug/kg
Endrin(72-20-8) 2,7:3,6-Dimethanonaphth[2,3-b]oxirene, 3,4,5,6,9,9- ... 3,4,5,6,9,9-Hexachloro-1a,2,2a,3,6,6a,7,7a-oct 3,4,5,6,9,9-Hexachloro-1a,2,2a,3,6,6a,7,7a-octahydro ... Compound 269 Endrin Hexachloroepoxyoctahydro-endo,endo-dimethanonaphthalene Hexadrin Mendrin Nendrin	0.400 ug/kg	89% Rec (SL)	6.02 RSD (SL)	2.50 ug/kg
Heptachlor(76-44-8) 1,4,5,6,7,8,8-Heptachlorotetrahydro-4,7-methanoindene Drinox Heptachlor Heptachlor [1,4,5,6,7,8,8-heptachloro-3a,4,7,7a- ... Heptachlor/Heptachlor epoxide (SARA 110) Heptachlorodicyclopentadiene Heptagran Heptamul Velsicol-104	0.400 ug/kg	68	7.81 RSD (SL)	2.50 ug/kg
Heptachlor epoxide(1024-57-3) Heptachlor epoxide Velsicol 53-CS-17 Vesicol 53-CS-17	1.100 ug/kg	92% Rec (SL)	15.20 RSD (SL)	2.50 ug/kg
Hexachlorobenzene(118-74-1) Anticarie Benzene, hexachloro- Bunt-cure HCB Hexachlorobenzene Perchlorobenzene	0.700 ug/kg	70% Rec (SL)	12.20 RSD (SL)	2.50 ug/kg
Lindane(58-89-9) Cyclohexane, 1,2,3,4,5,6-hexachloro-, (1-alpha Cyclohexane, 1,2,3,4,5,6-hexachloro-, (1-alpha, 2- ... HCH-gamma Hexachlorocyclohexane (gamma) Lindane Lindane ( gamma isomer of benzene hexachloride ) (99 ... gamma-BHC gamma-Benzenehexachloride gamma-HCH gamma-Hcch gamma-Hexachlorocyclohexane	0.500 ug/kg	57% Rec (SL)	10.80 RSD (SL)	2.50 ug/kg
Methoxychlor(72-43-5) 1,1'-(2,2,2-Trichloroethylidene)bis[4-methoxybenzene] 1,1,1-Trichloro-2,2-bis(4-methoxyphenyl)ethane Benzene, 1,1'-(2,2,2-trichloroethylidene)bis[4-methoxy- Dimethoxy DDT Ethane, 1,1,1-trichloro-2,2-bis(p-methoxypheny Ethane, 1,1,1-trichloro-2,2-bis(p-methoxyphenyl)- Marlate Methoxcide Methoxychlor Metox p,p'-Methoxychlor p,p'DMDT	1.700 ug/kg	214% Rec (SL)	9.86 RSD (SL)	2.50 ug/kg
Mirex(2385-85-5) Bichlorendo Cyclopentadiene,hexachloro-, dimer Dechlorane Ferriamicide Hexachloropentadiene dimer Mirex	0.400 ug/kg	114% Rec (SL)	4.72 RSD (SL)	2.50 ug/kg
Oxychlordane(27304-13-8) 1,5,6,8,9,10,11,11-Octachloro-4-oxatetracyclo[6.2.1.0.0]undec-9-ene 2,3,4,4',5,6-Hexachlordiphenylether 2,3,4,5,6,6a,7,7-octachloro-1b,2,5,5a,6,6a-hexahydro-1aH-2,5-methanoindeno[1,2-b]oxirene 2,5-Methano-2H-indeno[1,2-b]oxirene, 2,3,4,5,6,6a,7,7-octachloro-1a,1b,5,5a,6,6a-hexahydro- Oxychlordane	N/A	N/A	23.50 % RSD (SL)	2.50 ug/kg
Pentachloroanisole(1825-21-4) Pentachloroanisole	0.500 ug/kg	67% Rec (SL)	8.95 RSD (SL)	2.50 ug/kg
alpha-BHC(319-84-6) .alpha.-Benzenehexachloride Cyclohexane, 1,2,3,4,5,6-hexachloro-, alpha-isomer HCH-alpha alpha-BHC alpha-HCH alpha-Hexachlorocyclohexane alpha-Lindane	0.300 ug/kg	48% Rec (SL)	7.18 RSD (SL)	2.50 ug/kg
alpha-Chlordane(5103-71-9) 4,7-Methano-1H-indene 1,2,4,5,6,7,8,8-octachlo Methanoindan, 1-alpha,2-alpha,4-beta,5,6,7-beta,8,8- ... Methanoindan,alpha-1,2,4,5,6,7,8,8-octachloro-3a- ... alpha-Chlordane cis-4,7-Methano-1H-indene 1,2,4,5,6,7,8,8-octachloro ... cis-Chlordane	0.500 ug/kg	81% Rec (SL)	7.64 RSD (SL)	2.50 ug/kg
beta-BHC(319-85-7) Cyclohexane, 1,2,3,4,5,6-hexachloro-, beta-isomer HCH-beta beta-BHC beta-Benzenehexachloride beta-HCH beta-Hexachlorocyclohexane beta-Lindane	0.500 ug/kg	71% Rec (SL)	8.20 RSD (SL)	2.50 ug/kg
cis-Nonachlor(5103-73-1) cis-Nonachlor	0.500 ug/kg	88% Rec (SL)	7.45 RSD (SL)	2.50 ug/kg
delta-BHC(319-86-8) .delta.-Benzenehexachloride Cyclohexane, 1,2,3,4,5,6-hexachloro-, delta-isomer HCH-delta delta-BHC delta-HCH delta-Hexachlorocyclohexane delta-Lindane	0.800 ug/kg	91% Rec (SL)	11.60 RSD (SL)	2.50 ug/kg
o,p'-DDT(789-02-6) 2,2-Bis(o,p-chlorophenyl)-1,1,1-trichloroethane 2,4'-DDT 2-(2-Chlorophenyl)-2-(4-chlorophenyl)-1,1,1-trichloroethane o,p'-DDT o,p'-DDT op-DDT ortho,para'-DDT	0.700 ug/kg	60% Rec (SL)	15.90 RSD (SL)	2.50 ug/kg
o,p'-Methoxychlor(30667-99-3) o,p'-Methoxychlor	0.900 ug/kg	164% Rec (SL)	6.79 RSD (SL)	2.50 ug/kg
p,p'-DDT(50-29-3) 1,1,1-Trichloro-2,2-bis(p-chlorophenyl)ethane 4,4'-DDT Benzene, 1,1'-(2,2,2-trichloroethylidene)bis[4-chloro- Chlorophenothane DDT Dichlorodiphenyltrichloroethane Ethane, 1,1,1-trichloro-2,2-bis(p-chlorophenyl)- bis(p-Chlorophenyl)-2,2,2-trichloroethane,1,1- p,p'-DDT p,p'-Dichlorodiphenyltrichloroethane	3.000 ug/kg	92% Rec (SL)	49.00 RSD (SL)	2.50 ug/kg
trans-Chlordane(5103-74-2) AI3-16398 EINECS 225-826-0 Methanoindan, 1,2,3,5,6,7,8,8-octachlor-3a,4,7,7a- ... Methanoindan,1,2,4,5,6,7,8,8-octachloro-3a,4,7,7a- ... trans-4,7-Methano-1H-indene 1,2,4,5,6,7,8,8- ... trans-Chlordan trans-Chlordane	0.500 ug/kg	84% Rec (SL)	7.48 RSD (SL)	2.50 ug/kg
trans-Nonachlor(39765-80-5) trans-Nonachlor	0.400 ug/kg	85% Rec (SL)	6.55 RSD (SL)	2.50 ug/kg

Precision Descriptor Notes:	Method performance was evaluated by analyzing samples of nonspiked homogenized whole-body fish tissue, homogenized corbicula tissue, as well as samples of the same tissues spiked at two different concentrations. Each sample was evaluated using seven replicates. In addition, seven replicates at two concentrations of a reagent spike were analyzed. Seven replicates of NIST SRM-1588 cod liver oil were analyzed as part of the evaluation of method accuracy. To further validate the analytical method, two samples from the U.S. Fish and Wildlife Service round-robin evaluation were analyzed in duplicate, and a USEPA quality-control sample was analyzed in quadruplicate.
Detection Level Note:	Method detection limits were estimated with data from the 2.5-ug/kg reagent spikes and homogenized fish tissue that were fortified at the 2.0-ug/kg level. Matrix based method detection limits were determined on a fish homogenate chosen from submitted samples that contained low levels of contaminants. The method detection limits listed in the report are single calibration MDLs determined in two matrices. These detection limits are not used as method reporting limits. They neither account for the range of lipid composition, lipid concentration, and variety of aquatic tissues that are routinely analyzed, nor the day-to-day variation in instrument performance. The method detection limits were determined according to the U.S. Environmental Protection Agency (1992).

Precision Descriptor Notes:

Method performance was evaluated by analyzing samples of nonspiked homogenized whole-body fish tissue, homogenized corbicula tissue, as well as samples of the same tissues spiked at two different concentrations. Each sample was evaluated using seven replicates. In addition, seven replicates at two concentrations of a reagent spike were analyzed. Seven replicates of NIST SRM-1588 cod liver oil were analyzed as part of the evaluation of method accuracy. To further validate the analytical method, two samples from the U.S. Fish and Wildlife Service round-robin evaluation were analyzed in duplicate, and a USEPA quality-control sample was analyzed in quadruplicate.

Detection Level Note:

Method detection limits were estimated with data from the 2.5-ug/kg reagent spikes and homogenized fish tissue that were fortified at the 2.0-ug/kg level. Matrix based method detection limits were determined on a fish homogenate chosen from submitted samples that contained low levels of contaminants. The method detection limits listed in the report are single calibration MDLs determined in two matrices. These detection limits are not used as method reporting limits. They neither account for the range of lipid composition, lipid concentration, and variety of aquatic tissues that are routinely analyzed, nor the day-to-day variation in instrument performance. The method detection limits were determined according to the U.S. Environmental Protection Agency (1992).

Revision	PDF/Link
1994

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USGS-NWQL: O-9125-94: Chlorinated pesticides in aquatic tissue by dual capillary-column gas chromatography with electron-capture detection

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