Asahipak - Hplc.eu

Preparation of Test Samples Used in Simultaneous GC/MS and LC/MS Analysisof Agricultural Chemicals in Livestock and Marine Products (Outline)Extractionliver, kidneyacetone/n-hexane (1:2)GPCmuscle, fat, fish milk, egg honeyGPCacetonitrilesalting-outGPC Clean-up of Pesticide Residues using EV-2000 ACAcrinathrin (5mg/L)(marker pesticide)Tricyclazole (5mg/L)(marker pesticide)Sample pretreatmentcolumnsPurificationfraction-1[*1] [*1] [*1][*2]fraction-2pesticidefractionpesticidefractionmuscle, fat,fish, milk, eggliver, kidneyfraction-1pesticidefractionfraction-2Acrinathrin (5mg/L)GPC Clean-up of Beef TallowGPC Clean-up of Fatty TunaTricyclazole (5mg/L)test sampleGC/MS, LC/MS*1 purification with Ethylenediamine-N-propylsilyled silica gel mini-column*2 purification with silica gel mini-columnGPC Clean-up of Fatty Tuna and Beef Tallow[Extraction]1) Weigh 20.0g of the sample (5.0g for fat).2) Add 20mL of water and homogenize.3) Add 100mL of acetone/n-hexane (1/2)and homogenize.4) Centrifuge (2,500rpm, 5min.) and collectthe organic layer (1).5) Add 50mL of n-hexane to the residueand homogenize.6) Centrifuge (2,500rpm, 5min.) and collectthe organic layer (2).7) Combine (1) and (2) and add anhydroussodium sulfate for dehydration.8) Remove anhydrous sodium sulfate byfiltering and concentrate the filtrate at40˚C or lower.9) Remove the solvent.10) Weigh the residue (extracted fat).11) Dissolve in acetone/cyclohexane (1/4).Column : Shodex CLNpak EV-G AC + EV-2000 ACEluent : Acetone/Cyclohexane=1/4Flow rate : 5.0mL/minDetector : UV(254nm)Column temp. : 40˚CInjection vol. : 5mLFractionation StandardsFluvalinateAcrinathrincurrent elution fractionformer elution fractionSample :40mg/L eachChinomethionateTricyclazole7Columns for GPC Clean-up0 5 10 15 20 25 30 35 minColumn : Shodex CLNpak EV-G AC + EV-2000 ACEluent : Acetone/Cyclohexane=1/4Flow rate : 5.0mL/minDetector : UV(254nm)Column temp. : 40˚CInjection vol. : 5mL0 5 10 15 20 25 30 35 minColumn : Shodex CLNpak EV-G AC + EV-2000 ACEluent : Acetone/Cyclohexane=1/4Flow rate : 5mL/minDetector : UV(254nm)Column temp. : 40˚CInjection vol. : 5mLElution Positions of Phthalic Acid Estersusing PAE-800 ACRI Corn oil SulferH 2 OCO 2GPC clean-up of Carcinogens in DieselDust measured using PAE-800 ACBenzo[a]fluoranthene1,3-DinitropyreneBisphenol ABenzo[a]pyreneHydroxybenzo[a]pyrene mixturePretreatment of PCBs in Waste OilPCBsRIRIRIRIUV(330nm)UV(330nm)Bis(2-ethylhexyl) adipatePhthalic acid esters4-NonylphenolDDTBisphenol AAnthracene0 15 20 25 30 35minColumn : Shodex CLNpak PAE-800 ACEluent : AcetoneFlow rate : 0.5mL/minDetector : UV(330nm), RIColumn temp. : Room temp.10 20 30minCompound Rt(min) Compound Rt(min)AnthraceneChryseneFluorantheneBenzo[a]flucrantheneBenzo[b]flucrantheneBenzo[k]flucranthenePyrene1-Hydroxypyrene16.618.017.117.718.618.417.919.7Benzo[a]pyreneHydroxybenzo[a]pyrenecompoundBisphenol A1,3-Dinitronaphthalene1-Nitropyrene1,3-Dinitropyrene1,6-Dinitropyrene1,8-Dinitropyrene19.923.016.116.218.618.618.918.7Column : Shodex CLNpak PAE-800 ACEluent : AcetoneFlow rate : 0.8mL/minDetector : UV(210nm)Column temp. : Room temp.Data provided by Prof. Kazuichi Hayakawa,Faculty of Pharmaceutical Sciences, Kanazawa University.Time 14 15 16 17 18 19 20 minVolume 56 60 64 68 72 76 80 mLPCBsChlordane, ToxaphenePolychlorinated naphthalenePolybrominated biphenyletherAliphatic hydrocarbonC 19 C 12 MethylanthraceneAnthraceneColumn : Shodex CLNpak PAE-G AC+ PAE-2000 ACEluent : AcetoneFlow rate : 4.0mL/minDetector : UV(213nm)Data provided by Mr. Koichi Sasaki et al.,Analytical Center, Kokan Keisoku Corporation.