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 |
