摘要
目的 建立快速、准确、灵敏的猪组织(猪肉、猪肝和猪肾)中氯丙嗪、异丙嗪及其代谢产物氯丙嗪亚砜和异丙嗪亚砜的同位素内标稀释-液相色谱-串联质谱分析方法。方法 样品用乙腈提取,MCX固相萃取小柱净化。以0.1%甲酸乙腈和0.1%甲酸为流动相,采用梯度洗脱方式在ACQUITY UFLC?HSS T3色谱柱(100 mm×2.1 mm, 1.8μm)上进行分离,以电喷雾正离子多反应监测模式进行检测,同位素内标法定量。结果 氯丙嗪和异丙嗪在0.1~20.0μg/L,氯丙嗪亚砜和异丙嗪亚砜在0.5~100.0μg/L范围内具有良好的线性关系,相关系数(r)均大于0.999,方法的检出限为0.04~0.17μg/kg,定量限为0.12~0.51μg/kg,样品的回收率为90.8%~106.0%,精密度为1.9%~6.2%(n=6)。结论 本方法灵敏度高、结果准确,适用于猪肉、猪肝和猪肾中氯丙嗪、异丙嗪及其代谢产物氯丙嗪亚砜和异丙嗪亚砜残留的监测。
OBJECTIVE To establish a rapid,accurate and sensitive method by liquid chromatography-tandem mass spectrometry with isotope internal standard dilution technique for the determination of chlorpromazine and promethazine and their metabolites in swine tissues.METHODS The swine tissues sample was extracted with acetonitrile and purified on MCX cartridge.The liquid chromatography separation was performed on an ACQUITY UFLC®HSS T3(100 mm×2.1 mm,1.8μm)with a linear gradient elution program of 0.1%(V/V)fomic acid-acetonitrile and 0.1%(V/V)formic acid-water solution as the mobile phase.The analytes were analyzed using ESI operating in the positive multiple reaction monitoring(MRM)mode.RESULTS The limits of quantitation(LOQs)and limits of detection(LODs)for the target objects were 0.12-0.51 μg/kg and 0.04-0.17μg/kg,respectively.The calibration curves were linear in range of 0.1-20.0 μg/L for chlorpromazine and promethazine,and 0.5-100.0μg/L for their metabolites(chlorpromazine sulfoxide and isopropyl sulfoxide).The recoveries were between 90.8%-106.0%,and the relative standard deviations(RSDs)were between 1.9%-6.2%(n=6).CONCLUSION The method is highly sensitive and accurate,and is suitable for the analysis of chlorpromazine and promethazine and their metabolites(chlorpromazine sulfoxide and isopropyl sulfoxide)in swine tissues.
作者
陈晓红
周健
金米聪
Chen Xiaohong;Zhou Jian;Jin Micong(Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals of Zhejiang Province,Ningbo Key Laboratory of Poison Research and Control,Ningbo Municipal Center for Disease Control and Prevention,Ningbo 315010,China)
出处
《卫生研究》
CAS
CSCD
北大核心
2022年第3期476-482,共7页
Journal of Hygiene Research
基金
浙江省自然科学基金(No.LY18B050001)
宁波市“科技创新2025”重大专项(No.2018B10075)。
关键词
氯丙嗪
异丙嗪
氯丙嗪亚砜
异丙嗪亚砜
液相色谱-串联质谱法
猪组织
chlorpromazine
promethazine
chlorpromazine sulfoxide
isopropyl sulfoxide
liquid chromatography-tandem mass spectrometry(LC-MS/MS)
swine tissues
