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作 者:许勇[1] 潘晨[1] 韩晶[1] 彭兴盛[1] 郑荣[1] XU Yong;PAN Chen;HAN Jing;PENG Xingsheng;ZHENG Rong(NMPA Key Laboratory for Monitoring and Evaluation of Cosmetics,Shanghai Institute for Food and Drug Control,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:《上海预防医学》2022年第2期177-182,共6页Shanghai Journal of Preventive Medicine
摘 要:【目的】建立液相色谱-串联质谱(LC-MS/MS)法测定睫毛增长液中比马前列素、他氟乙酰胺、拉坦前列素、曲伏前列素和他氟前列素的分析方法。【方法】样品经50%乙腈的水溶液超声提取,加入4 g NaCl和1 g MgSO;的混合盐沉淀杂质,离心。上层有机相经微孔滤膜过滤后,用Agilent Poroshell 120 PFP-C18柱(2.7μm,2.1 mm×100 mm)分离,以含5 mmol·L;乙酸铵的0.02%甲酸-乙腈为流动相,梯度洗脱,流速0.5 mL·min;。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】比马前列素、他氟乙酰胺、拉坦前列素、曲伏前列素和他氟前列素在试验范围内线性良好,r>0.999。考察了膏霜、乳液、凝胶、水4种常见睫毛增长液基质的3个水平的加标回收率。结果回收率均在93.2%~103.5%,相对标准偏差(RSD)均在1.2%~3.4%,检出限(LOD)在0.000 2~1.5μg·g;。在测定的63批睫毛增长液中,检出比马前列素15批。【结论】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上述5种前列素类似物的测定。[Objective] To determine bimatoprost,tafluprost ethyl amide,latanoprost,travoprost and tafluprost in eyelash enhancing cosmetics by establishing a LC-MS/MS method.[Methods]The samples were extracted with a 50% acetonitrile water solution. A salt mixture(4 g NaCl,1 g MgSO;) was added to the solution to induce phase separation. After centrifugation and filtration,the analysis of five prostaglandin analogs was performed with an Agilent Poroshell 120 PFP-C18(2.7 μm,2.1 mm×100 mm)column,using 0.02% formic acid containing 5 mmol·L;Acetic acid amine and acetonitrile by gradient elution at a flow rate of 0.5 mL·min;. The analytes were detected with electrospray ionization source in positive ion mode(ESI+)and multiple reaction monitoring(MRM),and quantified by external standard curve.[Results]The results showed that it had a good linearity in the range of locatable ambit of concentration with correlation coefficients(r)larger than 0.999. The detection limit of five prostaglandin analogs(LOD)was 0.000 2-1.5 μg·g;. The spiked recoveries were 93.2% to 103.5% with a relative standard deviation(RSD)of 1.2% to 3.4%.[Conclusion]The method is simple,rapid and highly sensitive. It is suitable for the determination of five prostaglandin analogs in eyelash enhancing cosmetics.
关 键 词:睫毛增长液 比马前列素 他氟乙酰胺 拉坦前列素 曲伏前列素 他氟前列素 液相色谱-串联质谱法
分 类 号:R917[医药卫生—药物分析学]
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