分析化学2011，Vol.39Issue(6)：788-792,5.DOI:10.3724/SP.J.1096.2011.00788
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
摘要
Abstract
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 (r＞0.99). 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Key words
Ultra-performance liquid chromatography/ Quadrupole-time-of-flight mass spectrometry/Feeds/ Barbital drugs引用本文复制引用
张峰,丁菲,储晓刚,李范珠,雍炜,王秀娟,吕泉福,许成保..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[J].分析化学,2011,39(6):788-792,5.基金项目
本文系国家科技支撑计划(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.20081K167),北京市科技计划(No.D08050200310803)资助 （No.2009BADB9B02）
