超高效液相色谱—串联质谱法检测六种动物组织中盐酸氯丙嗪残留

建立了检测六种动物组织中盐酸氯丙嗪残留的超高效液相色谱-串联质谱(UPLC/MS/MS)分析方法。样品经碱性乙醚提取,浓缩后用甲醇溶解,经超高液相色谱-串联质谱在多反应检测(MRM)模式下测定。在3 min以内完成盐酸氯丙嗪的定量分析。结果显示盐酸氯丙嗪标准曲线在0.2~100μg/L浓度范围内线性良好,标准溶液中D3-氯丙嗪内标浓度为固定值5μg/L。线性相关系数(r)为0.999 8;在0.5、1、5、10μg/kg添加水平下,盐酸氯丙嗪的加标回收率在83%~104%,相对标准偏差(RSD)均小于10%(n=6);本方法对六种动物组织中盐酸氯丙嗪的定量限为0.5μg/kg(S/N10),检出限为0.2μg/kg(S/N3)。

Determination of Chlorpromazine Hydrochloride Residue in Six Kinds of Animal Tissues by Ultra Performance Liquid Chromatography- Tandem Mass Spectrometry

A simple,sensitive and ultra performance liquid chromatography-tandem mass spectrometric（UPLC/MS/MS） method has been developed for the quantification of chlorpromazine hydrochloride residue in six kinds of animal tissues.Chlorpromazine hydrochloride extracted by alkaline ether from animal tissue,was finally dissolved in the methanol after the procedure of being concentration.The sample was separated on BEH C18（100 mm×2.1 mm i.d.,1.7 μm） column using a mobile phase of acetonitrile/5 mmmol/L ammonium acetate.Chlorpromazine hydrochloride was detected in positive ion mode using multiple reactions monitoring（MRM）.The quantitative analysis was finished in 3.0 min.Results showed that in the range of 0.2 to 100 μg/L the standard curves for chlorpromazine hydrochloride were in good linearity,concentration of internal standard（D3-chlorpromazine）was 5 μg/L and the correlation coefficients（r） were 0.999 8.The recoveries for chlorpromazine at the addition of four levels（0.5,1,5,10 μg/kg）were 83%~104% and the relative standard deviation（RSD）for the determination of chlorpromazine were less than 10%（n= 6）.The limits of quantity（S/N ≥10） and limits of detection（S/N ≥3） by the present method for chlorpromazine hydrochloride were found to be 0.5 μg/kg and 0.2 μg/kg,respectively.