AHL LabNote 59-GC/MS-LC/MS multi-residue method

This multi-residue method is a qualitative tool used to screen liver, GI contents and suspect material for possible toxins. It consists of a general extraction method and analysis of the extract by GC/MS (gas chromatography-mass spectrometry) and LC/MS (liquid chromatography-mass spectrometry) methods.

GC/MS is a method suitable for volatile/semi-volatile, heat stable compounds analysed in the gas phase. The GC/MS method is both targeted (looking for specific known compounds) and non-targeted (looking for unknown compounds). This method involves several targeted analyses (see Table 1) and a non-targeted analysis that screen the extract for compounds and subsequent match with a comprehensive mass spectrum library. Matches are based on the specific mass spectral fingerprint produced for a compound based on the standardized ionization energy of the GC/MS instrumentation.

LC/MS is a method suitable for non-volatile compounds analysed in the liquid phase. LC/MS in a targeted method (Table 1). Routine LC/MS is not suitable for non-targeted screening due to various interferences that affect a compound’s ionization.

Table 1 lists the targeted compound included in our GC/MS-LC/MS multi-residue method. Recovery of these compounds in matrix has been confirmed at levels > 2 ppm.

It should also be noted that there are some compounds that we know are not detectable using this method (Table 2)

We will expand the list of targeted compounds as more compound standards are purchased and evaluated using this method.

This is not an all-encompassing toxin screen, but a cost effective way of screen for a large number of potential toxins. Targeted compounds currently include organochloride, organophosphate, carbamate, and other pesticides, barbiturates, tremorgenic mycotoxins, strychnine.

Table 1. List of known compounds currently included in GC/MS-LC/MS multi-residue method.

Standard Name

LC/GC

2,3,5-Trimethacarb

LC

2,4-DDE

GC

2-phenylphenol (O-phenylphenol)

GC

3-Hydroxycarbofuran

LC

4,4'-DDD

GC

Acephate

LC

Acetamiprid

LC

Acetochlor

LC

Acibenzolar-S-methyl

GC

Alachlor

GC

Alanycarb

LC

Aldicarb

LC

Aldicarb Sulfone

LC

Aldicarb sulfoxide

LC

Aldrin

GC

Allethrin

GC

Allidochlor

GC

alpha-BHC (benzene hexachloride)

GC

Ametryn

GC

Aminocarb

GC

Anilofos

LC

Aramite

GC

Aspon (Tetrapropyl thiodiphosphate)

GC

Atrazine

GC

Azaconazole

LC

azinphos-ethyl

GC

Azinphos-Methyl

LC

Azoxystrobin

GC

Baytan (triadimenol )

GC

Benalaxyl

GC

Bendiocarb

GC

Benfluralin

GC

Benfuracarb

LC

Benodanil

GC

Benoxacor

LC

Benzoximate

LC

benzoylprop-ethyl

GC

BHC beta isomer

GC

BHC delta isomer

GC

Bifenazate

LC

Bifenox

GC

Bifenthrin

GC

biphenyl

GC

Bitertanol

LC

Boscalid

LC

bromacil

GC

Bromophos-ethyl

GC

bromophos-methyl (bromophos)

GC

bromopropylate

GC

Bromuconazole

LC

bupirimate

GC

buprofezin

GC

Butachlor

GC

Butafenacil

LC

Butocarboxim

LC

Butocarboxim sulfoxide

LC

Butoxycarboxim

LC

butralin

GC

Butylate

GC

Cadusafos

LC

Captafol

GC

captan

GC

Carbaryl

LC

Carbendazim

LC

Carbetamide

GC

Carbofuran

LC

Carbophenothion

GC

Carboxin

LC

Carfentrazone-ethyl

LC

Chlorantraniliprole

LC

chlorbenside

GC

Chlorbromuron

LC

chlorbufam

GC

Chlordane - Gamma (trans)

GC

chlordane-cis (alpha)

GC

Chlordane-oxy

GC

Chlorfenson (Ovex)

GC

chlorfenvinphos

GC

Chlorflurecol-methyl ester

GC

chloridazon (Pyrazon)

LC

Chlorimuron ethyl

LC

Chlormephos

GC

chlorobenzilate

GC

Chlorodimeform

GC

chloroneb

GC

Chloropropylat

GC

chlorothalonil

GC

Chloroxuron

LC

Chlorprofam

GC

Chlorpyrifos

GC

Chlorpyrifos Methyl

GC

Chlorthal-dimethyl (DCPA, Dacthal)

GC

Chlorthion

GC

Chlorthiophos

GC

Chlortoluron

LC

Chlozolinate

GC

Clethodim

LC

Clodinafop-propargyl

LC

Clofentezine

LC

Clomazone

GC

Clothianidin

LC

coumaphos

LC

Crotoxyphos

LC

Cyanofenphos

LC

cyanophos

GC

Cyazofamid

LC

Cycloate

LC

Cycloxydim

LC

Cycluron

LC

cyfluthrin

GC

Cyhalothrin-lambda-1

GC

cypermethrin

GC

Cyproconazol

GC

Cyprodinil

GC

Cyromazine

LC

ddd-o,p'

GC

dde-p,p'

GC

ddt-p,p'

GC

deltamethrin

GC

Demeton-O

GC

demeton-s

GC

demeton-S-methyl

LC

Demeton-s-methyl sulfone

LC

Demeton-s-methyl sulfoxide

LC

des-ethyl-atrazine

GC

Desmedipham

LC

Desmetryn

GC

Dialifos

GC

Di-allate

GC

Diazinon

GC

diazinon-o-analogue (Diazinon-oxon, Diazoxon)

GC

dichlobenil (Dichlorobenzonitrile, 2,6-)

GC

Dichlofenthion

GC

Dichloran (Dichloran)

GC

Dichlormid

GC

Dichlorvos

GC

diclobutrazole

GC

Diclocymet

LC

Diclofop-methyl

GC

dicofol (Kelthane)

GC

Dicrotophos

LC

Dieldrin

GC

Diethatyl-ethyl

GC

Diethofencarb

LC

Difenoconazol

LC

Diflubenzuron

LC

Dimethachlor

GC

Dimethametryn

LC

Dimethenamid-p

LC

Dimethoate

LC

Dimethomorph

LC

Dimoxystrobin

LC

Diniconazole

LC

Dinitramine

GC

Dioxacarb

LC

Dioxathion

LC

Diphenamid

GC

Diphenylamine

GC

Dipropetryn

LC

disulfoton

GC

disulfoton-sulfone

GC

Diuron

LC

Endosulfan - II (beta)

GC

Endosulfan-1 (alpha)

GC

Endosulfan-Sulfate

GC

Endrin

GC

EPN

GC

Epoxiconazol

LC

EPTC

GC

Erbon

GC

Esfenvalerate

GC

etaconazole

GC

Ethalfluralin

GC

Ethiofencarb sulfoxide

LC

Ethion

GC

Ethiprole

LC

Ethirimol

LC

Ethofumesate

GC

Ethoprophos (Ethoprop)

GC

ethylan (ethyl-DDD, perthane)

GC

Etoxazole

LC

Etridiazol (Terrazole, Echlomezol)

GC

Etrimfos

GC

Famoxadone

LC

Fenamidone

LC

fenamiphos sulfone

GC

Fenamiphos sulfoxide

LC

fenarimol

GC

Fenbuconazol

GC

fenchlorophos (Ronnel)

GC

Fenfurman

LC

Fenhexamid

LC

Fenitrothion

GC

Fenobucarb

LC

Fenoxanil

LC

Fenoxycarb

LC

fenpropathrin

GC

Fenpropidin

LC

Fenpropimorph

LC

fensulfothion

GC

Fenthion

GC

Fentrazamide

LC

Fenuron

LC

Fipronil

LC

Flamprop-isopropyl

GC

Flamprop-methyl

GC

Flonicamid

LC

Fluazifop-butyl

LC

Flubendiamide

LC

Fluchloralin

GC

flucythrinate

GC

Fludioxonil

GC

Flufenacet

LC

flumetralin

GC

Fluometuron

LC

fluorochloridone

GC

Fluorodifen

GC

Fluoxastrobin

LC

Fluquinconazole

LC

Flurtriafol

LC

flusilazole

GC

Flutolanil

LC

fluvalinate-tau

GC

Folpet

GC

Fonofos

GC

Forchlorfenuron

LC

Fosthiazate

LC

Fuberidazol (FUB)

LC

Furalaxyl

LC

Griseofulvin

LC

Halofenozide

LC

Haloxyfop

LC

heptachlor

GC

heptachlor-epoxide-endo

GC

Heptanophos

GC

hexachlorobenzene

GC

hexaconazole

GC

Hexaflumuron

LC

Hexazinone

GC

Imazalil

LC

Imazamethabenz-methyl

LC

Imidacloprid

LC

Indoxacarb

LC

iodofenphos (Jodfenphos)

GC

Ipconazole

LC

iprobenfos

GC

Iprodione

GC

Iprovalicarb

LC

Isazophos (Miral, Isazofos)

GC

Isofenphos

GC

Isoprocarb

LC

Isopropalin

GC

Isoprothiolane

GC

Isoproturon

LC

Isoxathion

LC

kresoxim-methyl

GC

Leptophos

GC

Lindane (gamma-HCH, BHC-gamma)

GC

Linuron

LC

Malaoxon (metabolite of Malathion)

GC

Malathion

GC

Mandipropamid

LC

Mecarbam

GC

Mefenacet

LC

Mepanipyrim

LC

Mephosfolan

LC

Mepronil

LC

Metaflumizone

LC

Metalaxyl

GC

Metazachlor

GC

Metconazole

LC

Methabenzthiazuron

LC

Methidathion

LC

Methiocarb

LC

Methiocarb sufone

LC

Methiocarb Sulfoxide

LC

Methomyl

LC

methoprotryn

GC

methoxychlor

GC

Methoxyfenozide

LC

methyl-trithion (Carbophenothion-Methyl)

GC

Metobromuron

LC

Metolachlor

GC

Metolcarb

LC

Metoxuron

LC

Metribuzin

GC

Mevinphos(phosdrin)

GC

mirex

GC

Molinate

LC

Monceren (Pencycuron)

LC

monocrotophos

LC

Monolinuron

LC

myclobutanil

GC

Napropamide (Devrinol)

LC

Naptalam

LC

Neburon

LC

Nitenpyram

LC

Nitralin

GC

Nitrapyrin

GC

Nitrofen

GC

Nitrothal-isopropyl

GC

norflurazon

GC

nuarimol

GC

o,p - DDT

GC

octhilinone

GC

Ofurace

LC

Omethoate

LC

oxadiazon

GC

Oxadixyl

GC

Oxamy oxime

LC

oxamyl

LC

oxycarboxin

LC

Paclobutrazol

LC

paraoxon

GC

Parathion

GC

parathion-methyl

GC

Pebulate

GC

Penconazol

GC

Pendimethalin (Prowl) (Penoxaline)

GC

Penoxsulam

LC

permethrin

GC

Phenmedipham

LC

phenthoate

GC

Phorate

GC

Phorate-Sulfone

GC

Phosalone

GC

Phosmet

GC

Phosphamidon

GC

piperonyl butoxide

GC

Piperophos

LC

pirimicarb

GC

pirimiphos-ethyl

GC

pirimiphos-methyl

GC

Pretilachlor

LC

Primisulfuron-methyl

LC

Prochloraz

LC

procymidone

GC

Prodiamine

LC

Profenofos

GC

Profluralin

GC

Promecarb

GC

prometon

GC

Prometryne

GC

Propachlor

GC

Propamocarb

LC

Propanil (DCPA)

GC

propargit

GC

Propetamphos (Safrotin)

GC

Propham

GC

Propiconazole

GC

Propoxur

LC

Propyzamid (Pronamide)

GC

Prothioconazole

LC

Prothiophos

GC

Pymetrozine

LC

Pyracarbolid

GC

Pyraclostrobin

LC

Pyraflufen-ethyl

LC

Pyrazophos

GC

Pyridaben

GC

Pyridaphenthion

LC

Pyrifenox

LC

Pyrimethanil

LC

Pyroxsulam

LC

Quinalphos

GC

quinomethionate

GC

Quinoxyfen

LC

Quintozene

GC

Quizalofop ethyl

LC

Ruelene (Crufomate)

GC

Schradan

LC

secbumeton

GC

Siduron

LC

Simazine

GC

Simetryn

GC

Sulfentrazone

LC

Sulfollate

GC

sulfotep

GC

sulprophos

GC

TCMTB (Benthiazole)

GC

Tebuconazol/Folicur

GC

Tebufenozide

LC

Tebuthiuron

LC

tecnazene (TCNB)

GC

Temephos

LC

Tepraloxydim

LC

Terbacil

GC

Terbufos

GC

Terbumeton

GC

terbutryn

GC

Terbutylazine

GC

tetrachlorvinphos

GC

Tetraconazole

LC

Tetradifon

GC

Tetraiodoethylene

GC

Tetramethrin

GC

Tetrasul

GC

Thiabendazole

LC

Thiacloprid

LC

Thiamethoxam

LC

Thiazopyr

LC

Thidiazuron

LC

thiobencarb (Benthiocarb)

GC

Thiodicarb

LC

Thiofanox

LC

Thiofanox sulfone

LC

Thiofanox sulfoxide

LC

Thionazin (zinophos)

LC

Thiophanate-methyl

LC

Tolclofos-methyl

GC

Tolylfluanid

GC

Tralkoxydim

LC

trialate

GC

Triazophos

GC

tribufos (DEF)

GC

Trichlorfon

LC

Tricyclazol (beam)

LC

Trietazine

LC

Trifloxystrobin

GC

Trifloxysulfuron

LC

Triflumizole

GC

Triflumuron

LC

Trifluralin

GC

Triforine

LC

Triticonazole

LC

Vamidothion

LC

Vernolate

GC

vinclozolin

GC

Zectran (mexacarbate)

LC

Zoxamide

LC

Strychnine

LC

Roquefortine

LC

Penitrem A

LC

Butalbital

GC

Amobarbital

GC

Pentobarbital

GC

Secobarbital

GC

Phenobarbital

GC

Table 2. List of known compounds that cannot be detected by the  GC/MS-LC/MS multi-residue method.

Standard Name

LC/GC

Aclonifen

LC

Carbosulfan

GC

Chlorfluazuron

LC

Chlorthiamid

LC

Cloquintocet-mexyl

LC

Cyanazine

GC

Cymoxanil/zymoxanil

LC

Cyprazine

GC

Dichlofluanid

GC

Dinotefuran

LC

Dodemorph

LC

edifenphos

GC

Emamectin Benzoate

LC

Ethiofencarb

LC

Ethiofencarb sufone

LC

Etofenprox

LC

Fenamiphos (Phenamiphos)

GC

Fenazaquin

LC

Fenpyroximate

LC

fenson

GC

Flucarbazone-sodium

LC

Flufenoxuron

LC

Formetanate

LC

Furathiocarb

LC

Hexythiazox

LC

Hydramethylnon

LC

Isocarbamide

LC

Lufenuron

LC

Methamidiphos

LC

Novaluron

LC

Oxyflurofen

GC

Picolinafen

LC

Picoxystrobin

LC

Propazine

GC

Pyridalyl

LC

Pyridate

LC

Pyriproxyfen

LC

Quizalofop

LC

Spinetoram

LC

Spinosad

LC

Spirodiclofen

LC

Spiromesifen

LC

Spirotetramat

LC

Spiroxamine

LC

Tebufenpyrad

LC

Tebupirimfos

LC

Teflubenzuron

LC

Tolfenpyrad

LC

triadimefon

GC

Atenolol

GC

Metolprolol

GC

Bisprolol

GC

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