摘要
A rapid and accurate high performance liquid chromatography tandem mass spectrometry（HPLS-MS） method was established for quantification of chlorpromazine in pork. The porcine samples were pretreated with acetonitrile to precipitate proteins and followed by extraction with tert--butyl methyl ether（TBME）. The separation was performed on a 5 μm Agilent XDB--C18 column with gradient elution. The mobile phase A was 0.01 mol/L ammonium formate in water and mobile phase B was acetonitrile. The flow rate was at 0.8 mL/min. Quantification was performed on a triple-quadrupole tandem mass spectrometer using the multiple selected reaction monitoring（MRM） mode. Transition of m/z ＋319.1 to 58.1 was used for the quantification of chlorpromazine. The method was validated at the concentration range of 0.4040 μg/kg to 8.080 μg/kg for chlorpromazine with correlation coefficient of 0.9999. The spiked recoveries were more than 80.0% and the limit of detection（LOD） was 0.052 μg/kg. The developed method, which offers advantages of convenience, rapid, specificity and higher sensitivity, can be used for determination of chlorpromazine hydrochloride in porcine muscles.
本文建立了高效、准确的测定猪肉样品中氯丙嗪残留量的高效液相色谱-串联质谱法。碱化的样品混悬液由乙腈沉淀蛋白后再由特丁基甲醚萃取,经冷冻离心分离15分钟后注入高效液相色谱--串联四极杆质谱仪进行分析。色谱柱为5μm Agilent XDB--C18柱,流动相由A--0.01 mol/L甲酸铵缓冲液(pH=4)和B--乙腈组成,以0.8 mL/min的流速进行梯度洗脱,以电喷雾离子源正离子(ESI+)多反应监测模式(MRM)进行定量。氯丙嗪在0.4040–8.080μg/kg范围内线性关系良好,线性相关系数为0.999,加标回收率在80.0%以上,定量下限为0.052μg/kg。该方法简便、快速、灵敏、专一,适用于动物组织中的氯丙嗪研究。
基金
Chongqing Natural Science Foundation(Grant No.CSCT2013jcyjA10040)
