12112567890520505l ll i l l051205 Chiral SeparationCoumn / Pretreatment Coumn for itchngMethod / noitcartxEnoitac■iruPnoitcartxEnoitac■iruPCoumnSwGPCCean-upCoumnsSample : 10 µLEpinephrine hydrochloride 20 µg/mL (in *Solution A)1. (R)-Epinephrine2. (S)-Epinephrine10*Solution A : 0.75 g/L Ammonium acetate aqueous solution adjusted to pH4.0 with Glacial acetic acidColumn Eluent Flow rate Detector Column temp. : 25 ˚C: Shodex ORpak CDBS-453: *Solution A/CH3CN = 99/1: 0.3 mL/min: UV (280 nm)Liver, KidneyAcetone/n-Hexane (1/2)GPCFraction-1Fraction-2[*1][*2]GPC column : Shodex CLNpak EV-2000 AC + EV-G AC*1 Puri■cation with ethylenediamine-N-propylsilyled silica gel mini-column *2 Puri■cation with silica gel mini-columnOther than honeyAcetone/n-Hexane (2/3)under acidic conditions with acetic acidMacroporous diatomaceous earth column chromatographyGPCAgriculturalchemicalsfraction[*1][*2]Test sampleGPC column : Shodex CLNpak EV2000AC-12F + EV-G AC12C*1 Puri■cation with trimethyl aminopropylsilyled silica gel mini-column *2 Puri■cation with ethylenediamine- N-propylsilyled silica gel mini-column 152025Tricyclazole (5 mg/L) (agricultural chemical marker)fraction rangeSample : 10 µL (System suitability solution)0.25 mg/mL USP Lamivudine resolution mixture A RS in water1. Lamivudine2. Lamivudine enantiomer30 min101520fraction range25(when puri■cation is insuf■cient)Column Eluent Flow rate Detector Column temp. : 25 ˚CHoneyAcetonitrileSalting-out[*1]: Shodex CLNpak EV-G AC12C + EV2000AC-12F: Acetone/Cyclohexane = 3/17: 3.0 mL/min: UV (254 nm) (preparative type)10152030 min1010min: Shodex ORpak CDBS-453 : Methanol and *Buffer (5 : 95) *Buffer; 7.7 g/L of Ammonium acetate in water: 1.0 mL/min: UV (270 nm): Shodex CLNpak EV-G AC + EV-2000 AC: Acetone/Cyclohexane = 1/4: 5.0 mL/min: UV (254 nm) (preparative type)Column Eluent Flow rate Detector Column temp. : 40 ˚CInjection vol. : 5 mL: Shodex CLNpak EV-G AC + EV-2000 AC: Acetone/Cyclohexane = 1/4: 5.0 mL/min: UV (254 nm) (preparative type)Column Eluent Flow rate Detector Column temp. : 40 ˚CInjection vol. : 5 mLTricyclazole (5 mg/L) GPC Clean-up of beef tallowGPC Clean-up of fatty tuna10min25agricultural3035minSample : 5 mLBeef tallowFatty tuna1. Acrinathrin 5 mg/L2. Tricyclazole 5 mg/L1520253035minAnalysis of epinephrine injection proposed in USP-NF pharmacopeial forumSample preparation outline for simultaneous GC/MS and LC/MS analysis of agricultural chemicals in livestock and marine products (part 1)[Outline]Sample preparation outline for simultaneous LC/MS analysis of agricultural chemicals in livestock and marine products (part 2)[Outline]Muscle, Fat, FishMilk, EggGPCAgriculturalchemicalsfractionAgriculturalchemicalsfraction[*1]Test sampleHoney[*1][*2]Column Eluent Flow rate Detector Column temp. : 45 ˚CInjection vol. : 2 mLFractionation of agricultural chemicals using EV2000AC-12FAcrinathrin (5 mg/L) (agricultural chemical marker)Fluvalinate(5 mg/L)Impurity analysis of lamivudine according to USP-NF methodFractionation of agricultural chemicals using EV-2000 AC(agricultural chemical marker)Acrinathrin (5 mg/L) (agricultural chemical marker)muscle, fat, ■sh, milk, eggliver, kidneychemicals fractionfraction-2fraction-1GPC clean-up of fatty tuna and beef tallow65
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