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作 者:潘晨[1] 许勇[1] 韩晶[1] 彭兴盛[1] 郑荣[1] PAN Chen;XU Yong;HAN Jing;PENG Xing-sheng;ZHENG Rong(Shanghai Institute for Food and Drug Control,National Medical Products Administration Key Laboratory for Monitoring and Evaluation of Cosmetics,Shanghai 201203,China)
机构地区:[1]上海市食品药品检验所,国家药监局化妆品监测评价重点实验室,上海201203
出 处:《分析测试学报》2020年第7期917-921,共5页Journal of Instrumental Analysis
基 金:上海市药品监督管理局重大资助项目(ZD202003)。
摘 要:建立了高效液相色谱-串联质谱法(HPLC-MS/MS)测定睫毛增长液化妆品中比马前列素含量的分析方法。样品经50%(体积分数)甲醇溶液提取,Agilent Poroshell 120 EC-C18柱(4.6 mm×100 mm,2.7μm)分离,以5 mmol·L^-1乙酸铵水溶液(含0.02%甲酸)-乙腈(体积比55∶45)为流动相等度洗脱,流速0.3 mL·min^-1,采用电喷雾正离子源(ESI+),多反应监测(MRM)扫描方式检测,外标法定量。结果表明,比马前列素在0.5~100 ng·mL^-1质量浓度范围内线性良好,相关系数(r2)为0.9982,在低、中、高3个加标水平下的平均回收率分别为98.6%、101%和99.2%,相对标准偏差(RSD)分别为2.4%、2.1%、1.2%,检出限(LOD,S/N=3)为0.015μg·g^-1,定量下限(LOQ,S/N=10)为0.05μg·g^-1。该方法快速简便、灵敏度高,适用于市售睫毛增长液化妆品中比马前列素的快速准确检测。A high performance liquid chromatography-tandem mass spectrometric(HPLC-MS/MS)method was established for the determination of bimatoprost in eyelash enhancing cosmetics serums.The samples were extracted with 50%(by vloume)methanol,then separated on an Agilent Poroshell 120 EC-C18(4.6 mm×100 mm,2.7μm)column by isocratic elution,with 5 mmol·L^-1 ammonium acetate containing 0.02%formic acid-acetonitrile(55∶45)as mobile phases at a flow rate of 0.3 mL·min^-1.The analyte was detected by HPLC-MS/MS with electrospray ionization source in positive ion mode(ESI+)and multiple reaction monitoring(MRM),and quantified by external standard method.Results showed that there existed a good linear relationship for bimatoprost in the range of 0.50-100 ng·mL^-1 with a correlation coefficient(r2)of 0.9982.The limit of detection(LOD,S/N=3)and limit of quantitation(LOQ,S/N=10)were 0.015 and 0.05μg·g^-1,respectively.The recoveries at low,medium and high spiked levels were 98.6%,101%and 99.2%,with relative standard deviations(RSDs)of 2.4%,2.1%and 1.2%,respectively.The method is simple,rapid and high sensitive,and is suitable for the rapid determination of bimatoprost in eyelash enhancing cosmetics serums.
关 键 词:比马前列素 睫毛增长 化妆品 高效液相色谱-串联质谱法(HPLC-MS/MS)
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