Determination of β-Agonist Drugs in Animal Tissue

Method:	SPE
Matrix:	Animal tissue
Application No.:	101732
Columns:	ProElut PXC 60 mg / 3 mL 50/pk
Cat No.:	68203
Sample Pretreatment:	1. Sample preparation Weigh 5 g sample, add 15 mL ethyl acetate and 3 mL 10% sodium carbonate, homogenize at 10,000 rpm for 2 min, centrifuge at 6,000 rpm for 2 min, transfer the supernatant to the centrifuge tube, extract residues using 15 mL ethyl acetate, combine ethyl acetate layers. Add 5 mL 0.1 M hydrochloric acid to the ethyl acetate extract, vortex 1 min, centrifuge 1 min at 6,000 rpm, collect the lower aqueous phase. Repeat the extraction and combine lower aqueous phase, adjust to pH 5.2 with 2.5 mol/L sodium hydroxide. 2. Sample purification ProElut™ PXC 60 mg / 3 mL (Cat#68203) Condition: 3 mL MeOH / 3 mL H₂O / 3 mL 30 mM HCl Load: Add sample Wash 1: 3 mL deionized water Wash 2: 3 mL MeOH Elute: 5 mL MeOH (4% NH₄OH), evaporate to near dry at 50ºC by N₂ 3. Derivatization Add 100 µL toluene and 100 µL bis-trimethylsilyl trifluoroacetamide (BSTFA), vortex 20 sec, seal, heat for 1 h at 80 ºC, add 300 µL of toluene after cooling as the sample solution.
Conditions:	GC-MS method GC conditions Column: DM-5MS 30 m x 0.25 mm x 0.25 µm (Cat#8221) Inlet Temperature: 220 ºC Injection Mode: Splitless Injection Volume: 1 µL Temperature Program: Heating to 70 ºC in 0.6 min, then heating to 200 ºC with 25 ºC/min in 6 min, finally heating to 280 ºC with 25 ºC/min in 5 min Carrier Gas: He > 99.999%, flow rate: 0.9 mL/min MS conditions Interface Temperature: 280 ºC Solvent Delay: 8 min EI Temperature: 230 ºC Quadrupole Temperature: 160 ºC Ion Monitoring: Qualitative ion 86, 243, 262, 277, quantitative ion 86
Author:	Dikma Technologies Inc.
Keyword:	β-Agonist Drugs, Animal Tissue, SPE, PXC