Shodex Catalogue 2013-2015.pdf - Analytics Shop

Sample preparation outline for simultaneous GC/MS and LC/MS analysis ofagricultural chemicals in livestock and marine productsExtractionLiver, KidneyAcetone/n-Hexane (1/2)GPCMuscle, Fat, Fish Milk, Egg HoneyGPCAcetonitrileSalting-outGPC Clean-up of residual pesticides using EV-2000 ACAcrinathrin (5mg/L)(marker pesticide)Tricyclazole (5mg/L)(marker pesticide)Sample PretreatmentColumnsPurificationFraction-1[*1] [*1] [*1][*2]Fraction-2PesticidefractionTest sampleGC/MS, LC/MSPesticidefraction*1 Purification with ethylenediamine-N-propylsilyled silica gel mini-column*2 Purification with silica gel mini-columnGPC Clean-up of fatty tuna and beef tallowmuscle, fat,fish, milk, eggliver, kidneyfraction-1pesticidefractionfraction-2Column : Shodex CLNpak EV-G AC + EV-2000 ACEluent : Acetone/Cyclohexane=1/4Flow rate : 5.0mL/minDetector : UV(254nm)Column temp. : 40˚CInjection vol. : 5mLPCB and insulating oil using PAE-800Columns for GPC Clean-up0Sample : 5mLBeef tallowFatty tuna1. Acrinathrin 5mg/L2. Tricyclazole 5mg/LGPC Clean-up of beef tallowGPC Clean-up of fatty tuna1 25 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. : 5mL[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).Sample : 30μLPCB std. KC-mixtureInsulating oildissolved by hexaneMethanolAcetoneHexane400mg/L5,000mg/LInsulating oilPCB0 10 20 30Retention time (min)Column : Shodex CLNpak PAE-800Eluent : Methanol, Acetone, HexaneFlow rate : 0.8mL/minDetector : Photodiode array(209nm)Column temp. : 40˚CSource:Mr. Tetsuya Sawatsubashi (Mitsubishi Heavy Industries, Ltd.) etal., Search of Liquid Chromatographic Clean-up Materials forRapid PCB Analysis and Evaluation of Their SeparationCharacteristics. Journal of Environmental Chemistry, 2007,Vol. 17, No. 3, p. 471-481.Pretreatment of PCBs in waste oilGPC Clean-up of carcinogens in dieseldust measured using PAE-800 ACElution positions of phthalic acid estersusing PAE-800 ACPCBsBenzo[a]fluoranthene1,3-DinitropyreneBisphenol ABenzo[a]pyreneHydroxybenzo[a]pyrene mixtureRI Corn oil SulferH 2 OCO 2Time 14 15 16 17 18 19 20 minVolume 56 60 64 68 72 76 80 mLAliphaticC 19Chlordane,hydrocarbonC 12PCBsToxaphenePolychlorinatedPolybrominatedMethylanthracenenaphthalenebiphenyletherAnthraceneColumn : 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.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 Kazuichi Hayakawa Ph.D.,Faculty of Pharmaceutical Sciences, Kanazawa University.RIRIRIRIUV(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.63