固相萃取-超高效液相色谱-串联质谱法测定兽药制剂中巴比妥类药物  

Determination of Barbiturates in Veterinary Pharmaceuticals by Solid Phase Extraction-Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：张海超 高美华 刘蓓蕾 王敬 艾连峰 霍惠玲 李研东 ZHANG Haichao;GAO Meihua;LIU Beilei;WANG Jing;AI Lianfeng;HUO Huiling;LI Yandong(Shijiazhuang Customs Technology Center,Shijiazhuang 050051;Hebei Provincial Veterinary Drug Inspection Institute,Shijiazhuang 050035)

机构地区：[1]石家庄海关技术中心,河北石家庄050051 [2]河北省兽药监察所,河北石家庄050035

出　　处：《分析科学学报》2022年第1期83-88,共6页Journal of Analytical Science

基　　金：河北省科技计划(No.19226614D,19225503D);海关总署科技计划(No.2019HK112)。

摘　　要：建立了固相萃取,结合超高效液相色谱-串联质谱(UPLC-MS/MS)测定兽药制剂中巴比妥、苯巴比妥、司可巴比妥和异戊巴比妥4种药物的方法。样品采用乙腈提取,HLB固相萃取柱净化,在ACQUITY BEH C_(18)色谱柱(100 mm×2.1 mm,1.7μm)上,以乙腈和水溶液为流动相梯度洗脱,质谱以多反应监测(MRM)方式进行定量分析。结果表明,4种目标化合物在20~1000 ng/mL范围内线性关系良好,相关系数(R)大于0.9980,方法的检出限为20μg/kg,定量限为50μg/kg。所有目标化合物在3个添加水平(50、100和500μg/kg)下,回收率在70.5%~96.4%之间,相对标准偏差为3.3%~10.4%。该方法净化效果好、普适性强,可实现兽药制剂的针剂、粉剂和合剂中巴比妥类药物的测定。A method was developed for the determination of barbital,phenobarbital,secobarbital and amobarbital in veterinary pharmaceuticals by solid phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Samples were extracted with acetonitrile,and then cleaned up with HLB column,and quantified by UPLC-MS/MS in MRM mode after gradient elution on an ACQUITY BEH C_(18) column(100 mm×2.1 mm,1.7μm)with acetonitrile and water as mobile phase.The results showed that the calibration curves were linear in the range of 20-2000 ng/mL with correlation coefficients higher than 0.9980.The limits of detection were 20μg/kg.The limits of quantification were 50μg/kg.The average recoveries at different levels(50,100 and 500μg/kg)for all the analytes ranged from 70.5%to 96.4%,with the relative standard deviations of 3.3%-10.4%.This method has good purification effect and strong universality,and can be used for the determination of barbiturates illegally added in injection,powder and mixture veterinary drug preparations.

关 键 词：巴比妥类药物 固相萃取 液相色谱-串联质谱 兽药制剂 

分 类 号：O657.63[理学—分析化学]