微波辅助衍生化/气相色谱串联质谱同时测定猪肝与猪肾中4种巴比妥药物残留  

Determination of Four Barbiturates in Pig Liver and Kidney by Gas Chromatography-Tandem Ion Trap Mass Spectrometry with Microwave Assisted Derivatization

作　　者：赵海香[1] 杨素萍[1] 刘海萍[1] 曲平化 

机构地区：[1]河北北方学院理学院化学系,河北张家口075000 [2]河北省邢台市畜牧水产局,河北邢台054001

出　　处：《分析测试学报》2012年第12期1525-1530,共6页Journal of Instrumental Analysis

基　　金：河北北方学院博士基金资助项目;河北北方学院校级课题资助(2010001)

摘　　要：采用气相色谱-离子阱串联质谱(GC-MS/MS)同时测定猪肝和猪肾中4种巴比妥类药物(巴比妥、异戊巴比妥、司可巴比妥钠和苯巴比妥)的残留量。残留药物用乙腈超声提取,浓缩后用5 mL 0.1 mol/LK2HPO4(pH 7.4)溶解,采用C18SPE柱净化,正己烷-乙酸乙酯(7∶3)洗脱,经CH3I微波辅助衍生化,甲基化产物经TR-5MS毛细管柱分离,在MS/MS模式下测定,外标法定量。方法在5～100μg/L范围内线性良好,相关系数r>0.99,4种巴比妥药物的检出限(LOD,S/N≥3)在猪肝中不高于0.65μg/kg,猪肾中不高于1.00μg/kg。定量下限(LOQ,S/N≥10)在猪肝中不高于2.20μg/kg,猪肾中不高于3.35μg/kg。4种药物的加标回收率为68%～90%,相对标准偏差(RSD)均不高于10%。方法可以准确监测动物组织中的巴比妥类药物残留。A gas chromatography–tandem ion trap mass spectrometric（GC-MS/MS） method was developed for the simultaneous determination of four barbiturates residues（e.g.barbital,amobarbital,secobarbital sodium and phenobarbital） in pig liver and kindey.The barbiturates residues were extracted by ultrasonic assistant extraction with acetonitrile.The extracts were concentrated and redissolved by 5 mL 0.1 mol/L K2HPO4 （pH 7.4）,cleaned up by C18 SPE cartridge using hexane–ethyl acetate（7∶3） mixture as eluting solvent,then derivatized with CH3 I by microwave irradiation.The methylated barbiturates were separated on a TR-5MS capillary column and detected with an ion trap mass detector.Electron impact（EI） ion source operated in MS/MS mode was adopted for identification and external standard method was employed for quantification.Good linearities （r＞0.99） were obtained in the range of 5-100 μg/L.The limits of detection（LOD,S/N≥3）for four barbiturates were no more than 0.65 μg/kg in liver and 1.00 μg/kg in kidney.The limits of quantitation（LOQ,S/N≥10） were no more than 2.20 μg/kg in liver and 3.35 μg/kg in kidney.The recoveries of four barbiturates at spiked levels of 5，10，15 μg/kg ranged from 68% to 90% with relative standard deviations（RSDs） no more than 10%.The results indicated that the method was accurate for the determination of barbiturate drug residues in animal tissues.

关 键 词：巴比妥类药物 气相色谱-离子阱串联质谱 微波辅助衍生化 猪肝 猪肾 超声提取 C18 SPE柱 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]