HPLC-MS/MS法测定血液中氯美扎酮OACHSSCD
Detection of Chlormezanone in Blood Using HPLC-MS/MS Method
目的 建立血液中氯美扎酮的HPLC-MS/MS检测方法.方法 在待测样品中加入乙腈沉淀蛋白,振荡、超声后离心取上清液,经0.22 μm聚四氟乙烯滤膜过滤后,采用InfinityLab Poroshell 120 EC-C18(100 mm×4.6 mm,2.7 μm)色谱柱分离,流动相A为0.1%甲酸水溶液,流动相B为乙腈,以流速0.4 mL/min梯度洗脱.质谱仪采用电喷雾离子源正离子模式、多反应监测模式.结果 血液样品中氯美扎酮在相应范围内线性关系良好,相关系数(r)均大于 0.999,检出限为 22.83 ng/mL,定量限为 100 ng/mL.基质效应为2.1%~3.9%,提取回收率为 88.8%~92.3%.采用本方法从阳性检材中检出氯美扎酮的质量浓度为1 217.23 ng/mL.结论 本方法前处理简单、样品用量少、线性范围宽,可用于血液中氯美扎酮的检测.
Objective To establish a high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method for detecting chlormezanone in blood samples.Methods Acetonitrile was added to the samples to precipitate proteins.After vortex and ultrasonication,the mixture was centrifuged,and the supernatant was collected.It was then filtered using a 0.22 μm polytetrafluoroethylene mem-brane.Separation was performed using an InfinityLab Poroshell 120 EC-C18 column(100 mm×4.6 mm,2.7 μm).The mobile phase consisted of phase A(0.1%formic acid)and phase B(acetonitrile),with gra-dient elution at a flow rate of 0.4 mL/min.The mass spectrometer was operated with an electrospray ionization in positive ion mode and multiple reaction monitoring mode.Results Chlormezanone in blood samples showed good linearity within the tested range,with the correlation coefficients(r)all greater than 0.999.The limit of detection and the limit of quantitation of chlormezanone were 22.83 ng/mL and 100 ng/mL,respectively.The matrix effects were 2.1%-3.9%and recoveries were 88.8%-92.3%.Using this method,the mass concentration mass of chlormezanone detected in a positive sample was 1 217.23 ng/mL.Conclusion This method requires simple sample preparation and a small sample volume,and offers a wide linear range,making it suitable for the detection of chlormezanone in blood.
刘悦;梁未未;朱焕慧;何天夫;田源源;彭聪;王松才
广州市公安局警务技术支队,广东 广州 510442广州市公安局警务技术支队,广东 广州 510442广州市公安局警务技术支队,广东 广州 510442广州市公安局警务技术支队,广东 广州 510442广州市公安局警务技术支队,广东 广州 510442广州市公安局警务技术支队,广东 广州 510442广州市公安局警务技术支队,广东 广州 510442
医药卫生
法医学毒物分析氯美扎酮血液高效液相色谱-串联质谱法(HPLC-MS/MS)
forensic medicinetoxicological analysischlormezanonebloodhigh performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)
《法医学杂志》 2026 (2)
130-134,5
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