超高效液相色谱-四极杆飞行时间质谱测定动物饲料中3种巴比妥类违禁药物  

Simultaneous Determination of Three Barbitals in Feeds by Ultra-Performance Liquid Chromatography-Quadrupole-Time-of-Flight Mass Spectrometry

作　　者：张峰[1] 丁菲[1,2] 储晓刚[1] 李范珠[2] 雍炜[1] 王秀娟[1] 吕泉福[1,3] 许成保 

机构地区：[1]中国检验检疫科学研究院,北京100123 [2]浙江中医药大学,杭州310053 [3]西南大学,重庆400715 [4]河北农业大学,保定071060

出　　处：《分析化学》2011年第6期788-792,共5页Chinese Journal of Analytical Chemistry

基　　金：国家科技支撑计划(No.2009BADB9B02);质检公益性行业科研项目(No.200910145);国家质检总局科技计划(No.2008IK167);北京市科技计划(No.D08050200310803)资助

摘　　要：建立了超高效液相色谱-四极杆飞行时间质谱(UPLC-Q-TOF-MS)快速检测动物饲料中违禁添加的巴比妥、苯巴比妥和异戊巴比妥3种药物的分析方法。样品经甲醇振荡提取,再用C18固相萃取柱净化处理后,采用UPLC-Q-TOF-MS分析检测。在电喷雾负离子模式和飞行时间模式下,以20 mDa为提取离子窗口,输入各化合物的精确分子离子质量数得到相应的提取离子色谱图,以该色谱峰面积进行定量分析。通过碰撞诱导解离模式(CID)得到各化合物碎片离子的精确质荷比,进一步确证各化合物的结构。各化合物的质量精确度均小于5×10-6,3种化合物在0.05～2.0 mg/L范围内均呈良好的线性关系,线性系数均大于0.99。本方法的巴比妥、苯巴比妥和异戊巴比妥的定量限(LOQ)分别为0.25,0.20和0.23 mg/kg。3个添加水平(LOQ,2LOQ和4LOQ)的回收率为62%～85%;相对标准偏差(RSD)均小于10%。本方法可用于饲料中禁用的巴比妥药物的测定。A method using ultra-performance liquid chromatography（UPLC） quadrupole-time-of-flight mass spectrometry（Q-TOF-MS） was developed for screening and confirmation of 3 barbital drugs,barbital,phenobarbital,amobarbital,in feeds.After homogenization,the samples were extracted with methanol,and then the extracts were directly purified through C18 cartridge.Identification and detection were achieved in the negative electrospray ionization（ESI） mode using Q-TOF-MS.Accurate mass measurements were performed at a mass resolution of 10000 using continuous introduction of a lock mass with 20 mDa mass window.The potential of UPLC-Q-TOF MS for confirmatory analysis was shown by determining the accurate mass of all compounds and fragment ions upon collision-induced-dissociation（CID） at different energies.The extra mass measurements errors for all barbital drugs were found to be within 5×10-6.The calibration graphs were linear in the concentration range of 0.05-2.0 mg/L for three drugs.All calibration curves showed good linearity（r0.99）.The recoveries for all compounds in feeds were 62%-85% at the fortified levels of LOQ,2LOQ and 4LOQ,with the limits of quantification（LOQ） of 0.25,0.20 and 0.23 mg/kg.The relative standard deviations（RSD） for all compounds are less than 10%.

关 键 词：液相色谱 四极杆-飞行时间质谱 饲料 巴比妥 

分 类 号：S816.17[农业科学—饲料科学]