摘要
目的建立超快速液相色谱-串联质谱方法(LC-MS/MS)对人体血液中氯苯那敏成分进行定性定量分析。方法血液经过乙腈沉淀蛋白后,振荡、离心,过0.22μm有机微孔滤膜,上清液经LC-MS/MS分析。选取Agilent ZORBAX Eclipse C18作为液相色谱柱,柱温为40℃,以5mmol/L甲酸铵-0.1%甲酸水溶液-乙腈作为流动相,流速1.2mL/min,进行梯度洗脱,采用多反应监测模式,通过氯苯那敏的保留时间和两对离子对进行定性,外标-标准曲线法进行定量分析。结果该方法测定血液中氯苯那敏成分在0.1~100ng/mL浓度范围内具有良好线性,相关系数达到0.998 5。方法最低检出限(LOD S/N=3)达0.03ng/mL,定量限(LOQ S/N=10)为0.1ng/mL,日内精密度在5%以下,日间精密度在8%以下,重现性好,回收率高。结论该方法快速、准确、可靠,能够适用于血液中氯苯那敏的分析。
Objective A method by ultra fast liquid chromatography-tandem mass spectrometry(UFLC-MS/MS) was to develop and validate for detecting and determining chlorpheniramine in human plasma. Methods The plasma samples were precipitated with acetonitrile, afterwards oscillated and centrifugalized. The supernatant was filtered by 0.22μm organic micro-pore membrane, then detected by LC-MS/MS. The anlyte was separated from a reversed-phase C18 column(Agilent ZORBAX Eclipse C18) by a gradient elution, with the column oven being at 40°C. The mobile phase of elution was consisted of 5 mmol/L ammonium formate-0.1% methanoic acid-acetonitrile at a flow rate of 1.2 m L/min. Retention time and two ion pairs of chlorpheniramine were used for qualitative analysis in multiple reaction monitoring mode(MRM). The quantitative detection for chlorpheniramine was based on calibration curve. Results By the optimized LC-MS/MS method, the correlation coefficient of chlorpheniramine was 0.9985 within the linear range of 0.1 ng/m L^100 ng/m L. The limit of detection(LOD S/N=3) was 0.03 ng/m L for the chlorpheniramine in plasma samples, with its limit of quantification(LOQ S/N=10) being 0.1 ng/m L. In addition, the intra-and inter-day relative standard deviations(RSDs) were respectively less than 5% and 8%, showing a good reproducibility and high recovery. Conclusions The method developed with this research is rapid, highly accurate and reliable for analysis of chlorpheniramine in human plasma.
作者
孙会会
袁明俊
杜鸿雁
胡琨
仲建军
SUN Huihui;YUAN Mingjun;DU Hongyan;HU Kun;ZHONG Jianjun(Material Evidence Authentication and Research Center of Dezhou Public Security Bureau,Dezhou 253000,Shandong,China;Institute of Forensic Science,Ministry of Public Security,Beijing 100038,China)
出处
《刑事技术》
2020年第1期55-59,共5页
Forensic Science and Technology
关键词
氯苯那敏
液相色谱-串联质谱
血液
chlorpheniramine
liquid chromatography-tandem mass spectrometry
plasma samples
作者简介
第一作者:孙会会,女,山东临沂人,硕士,助理工程师,研究方向为毒物毒品检验。E-mail:shqcome@163.com。
