分析化学2012，Vol.40Issue(1)：101-106,6.DOI:10.3724/SP.J.1096.2012.10419
超高效液相色谱-四极杆飞行时间质谱法测定饲料中9种雄性激素类药物
Simultaneous Determination of Nine Androgen Drugs in Feeds by Ultra-Performance Liquid Chromatography-QuadrupoleTime-of-Flight Mass Spectrometry
摘要
Abstract
An ultra-performance liquid chromatography (UPLC) quadrupole-time-of-flight mass spec-trometric (Q-TOF-MS) method was developed for determination of 9 androgen drugs in feeds. After homogenization, the samples were extracted with ethyl acetate, and then the extracts were directly purified with matrix solid phase extraction. Identification and detection were achieved in the positive electrospray ionization (ESI) mode using Q-TOF-MS. The extracted ion chromatograms of each compound were obtained by entering the accurate molecular mass. The samples were quantified with the chromatographic peak area of each compound. 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 androgen drugs were found to be within 5 X 10-6. For these drugs, the calibration curves were linear between 0 to 1000 μg/L, and the correlation coefficient was more than 0. 99. The recoveries for all compounds in feeds were 70. 0% -99. 7% at the fortified levels of 1LOQ, 2LOQ and 4LOQ with the limit of quantitation (LOQ) of 16, 10, 20, 43, 20, 12, 15, 10 and 16 ng/kg. The relative standard deviations (RSD) for all compounds were less than 10%.关键词
液相色谱/四极杆-飞行时间质谱/饲料/雄性激素Key words
Ultra performance liquid chromatography/Quadrupole-time-of-flight mass spectrometry/Feeds/Androgen drugs引用本文复制引用
张峰,许成保,蓝芳,王秀娟,雍炜,锁然,储晓刚,丁菲,吕泉福..超高效液相色谱-四极杆飞行时间质谱法测定饲料中9种雄性激素类药物[J].分析化学,2012,40(1):101-106,6.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)及北京市科技计划(No.D08050200310803)资助 （No.2009BADB9B02）
