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高效液相色谱-四极杆/飞行时间高分辨质谱测定化妆品中的西咪替丁及雷尼替丁
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作者单位
王聪,董喆,李莉,王海燕,孙磊 中国食品药品检定研究院 
基金项目:上海市市级农口系统青年人才成长计划资助项目(沪农青字(2018)第 1-35 号)
中文摘要:建立了化妆品中西咪替丁及雷尼替丁的高效液相色谱-四极杆/飞行时间高分辨质谱检测方法,并对其质谱裂解规律进行研究。待测样品经甲醇超声提取,过滤膜后经Zorbax SB-Aq色谱柱(3.0 mm×100 mm,1.8 μm)分离,用乙腈-含0.1%甲酸的水溶液梯度洗脱后,在双喷雾电喷雾离子源正离子模式下检测,数据采集使用一级母离子全扫描和目标二级离子扫描。在不同的化妆品基质中,西咪替丁和雷尼替丁分别在5.65~113 ng/mL和4.95~990 ng/mL范围内线性关系良好(r>0.999),检出限分别为1.1、0.99 ng/mL,定量下限分别为5.6、5.0 ng/mL;2种待测物在低、中、高3个加标水平下的回收率为86.7%~110%,相对标准偏差(RSD)为0.90%~6.0%,方法重复性良好(RSD<10%)。该方法前处理简单,灵敏度较好,线性、回收率及重复性均满足方法学要求,可用于化妆品中西咪替丁和雷尼替丁的筛查测定。
中文关键词:高效液相色谱-四极杆/飞行时间高分辨质谱  化妆品  西咪替丁  雷尼替丁
 
Determination of Cimetidine and Ranitidine in Cosmetics by High Performance Liquid Chromatography-Quadrupole/Time of Flight High Resolution Mass Spectrometry
Abstract:A method was established for screening and quantitative determination of cimetidine and ranitidine in cosmetics by high performance liquid chromatography-quadrupole/time of flight high resolution mass spectrometry.In addition,the tandem MS fragment pathways of cimetidine and ranitidine were studied.Samples were ultrasonically extracted with methanol and filtered,then separated on a Zorbax SB-Aq column(3.0 mm×100 mm,1.8 μm) with acetonitrile and water containing 0.1% formic acid as mobile phases by gradient elution,finally analyzed with double spray electrospray ion source in positive mode.Data were acquired in full mass scan and target mass/mass scan modes.In different cosmetic matrixes,there were good linear relationships for cimetidine and ranitidine in concentration ranges of 5.65-113 ng/mL and 4.95-99.0 ng/mL,respectively,with their correlation coefficients(r) larger than 0.999.The limits of detection for cimetidine and ranitidine were 1.1 ng/mL and 0.99 ng/mL,and the limits of quantitation were 5.6 ng/mL and 5.0 ng/mL,respectively.The recoveries of two analytes at three spiked levels varied from 86.7% to 110% with relative standard deviations(RSD) of 0.90%-6.0%,and the repeatability was satisfactory(RSD<10%).The proposed method is simple,rapid and sensitive,and could be applied in quick screening and quantitative analysis of cimetidine and ranitidine in cosmetics.
Key Words:high performance liquid chromatography-quadrupole/time of flight mass spectrometry  cosmetics  cimetidine  ranitidine
引用本文:王聪,董喆,李莉,王海燕,孙磊.高效液相色谱-四极杆/飞行时间高分辨质谱测定化妆品中的西咪替丁及雷尼替丁[J].分析测试学报,2020,39(6):756-761.
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