Sun Lei, Zhang Li, Xu Qian, Wang Shuhuai, Wang Xia
China Institute of Veterinary Drug Control, Beijing 100081, China.
Se Pu. 2010 Jan;28(1):38-42. doi: 10.3724/sp.j.1123.2010.00038.
An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/ MS) method was established for the determination of methaqualone, chloropromazine, promethazine, diazepam, nitrazepam, oxazepam, temazepam, midazolam, triazolam and zolpidem residues in pork and kidney. After enzymolysis, the samples were extracted by ethyl acetate and tert-butyl methyl ether, separately. The separation of the ten sedatives was performed on a Waters Acquity UPLC system with a BEH C18 column. The mobile phases were acetonitrile (containing 0.1% formic acid) and water (containing 0.1% formic acid) at a flow rate of 0.3 mL/min. The electrospray was operated in the positive ionization mode and the ten sedatives were identified by multiple reaction monitoring (MRM) mode. The method of matrix-matched standard solution was adopted as the quantitative method. The calibration curves showed good linearity within the concentrations of 2 - 100 microg/L with the correlation coefficients r > 0. 998. The limits of detection of the ten sedatives were 0.5 microg/kg, and the limit of quantification was 1 microg/kg. The recoveries of the ten sedatives were 64.5% - 111.4% at the spiked levels of 2, 5 and 10 microg/kg. The relative standard deviations of intra- and inter-day coefficients of variation were both less than 15%. This method is simple, sensitive and accurate in the determination of sedative residues.
建立了超高效液相色谱 - 串联质谱法(UPLC-MS/MS)测定猪肉和猪肾中安眠酮、氯丙嗪、异丙嗪、地西泮、硝西泮、奥沙西泮、替马西泮、咪达唑仑、三唑仑和唑吡坦残留量的方法。酶解后,样品分别用乙酸乙酯和叔丁基甲醚萃取。十种镇静剂在配备BEH C18柱的Waters Acquity UPLC系统上进行分离。流动相为乙腈(含0.1%甲酸)和水(含0.1%甲酸),流速为0.3 mL/min。采用电喷雾正离子模式,十种镇静剂通过多反应监测(MRM)模式进行鉴定。采用基质匹配标准溶液法作为定量方法。校准曲线在2 - 100 μg/L浓度范围内线性良好,相关系数r > 0.998。十种镇静剂的检测限为0.5 μg/kg,定量限为1 μg/kg。在2、5和10 μg/kg加标水平下,十种镇静剂的回收率为64.5% - 111.4%。日内和日间变异系数的相对标准偏差均小于15%。该方法在测定镇静剂残留量方面简便、灵敏、准确。