高效液相色谱法测定化妆品中14种α-羟基酸和羟基酸酯  

Determination of 14 kinds ofα-hydroxy acids and hydroxy esters in cosmetics

作　　者：张丽媛 颜琳琦 程巧鸳 戚绿叶 王容 黄柳倩 Liyuan Zhang;Linqi Yan;Qiaoyuan Cheng;Lvye Qi;Rong Wang;Liuqian Huang(NMPA Key Laboratory for Animal Alternative Testing Technology of Cosmetics,Zhejiang Institute for Food and Drug Control,Hangzhou,Zhejiang 310052,China)

机构地区：[1]浙江省食品药品检验研究院、国家药监局化妆品动物替代试验技术重点实验室,浙江杭州310052

出　　处：《日用化学工业（中英文）》2024年第3期353-359,共7页China Surfactant Detergent & Cosmetics

基　　金：2021年《化妆品安全技术规范》制修订项目;2022年度浙江省药品监督管理局科技计划(编号:2021036)。

摘　　要：采用高效液相色谱法(HPLC)建立同时测定化妆品中14种α-羟基酸和羟基酸酯含量的方法,并结合高效液相色谱-串联质谱联用法(HPLC-MS/MS)确证结果。采用高效液相色谱法,以0.05 mol/L的磷酸氢二铵水溶液和甲醇为流动相进行梯度洗脱,采用Waters T3-C_(18)(4.6×250 mm,5μm)色谱柱分离,采用二极管阵列检测器检测,以214 nm为检测波长,外标法定量。采用高效液相色谱-串联质谱联用法,以0.1%甲酸水溶液和含0.1%甲酸乙腈为流动相进行梯度洗脱,采用Waters T3-C_(18)(2.1×100 mm,1.8μm)色谱柱分离,电喷雾电离,正、负离子多反应监测模式定性。14种化合物在各自质量浓度范围内呈良好的线性关系,相关系数R2均大于0.999。4种基质样品,14种化合物平均加标回收率均在85%~115%范围内,相对标准偏差均小于5%,检出限为1~150μg/g,定量限为3~450μg/g。对7批含α-羟基酸和酯的样品进行液质确证,结果均为阳性。该方法操作简便、准确度好、灵敏度高,适用于化妆品中14种α-羟基酸及其酯的测定。The study aimed to establish a method for simultaneous determination of 14 kinds ofα-hydroxy acids and their esters in cosmetics by high performance liquid chromatography(HPLC),and the results were confirmed by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).HPLC was used for gradient elution with 0.05 mol/L diammonium hydrogen phosphate-methanol as the mobile phase.The analytes were separated on a Waters T3-C18(4.6×250 mm,5μm)column and detected at the wavelengths of 214 nm.Quantification analysis was performed by the external standard method.HPLC-MS/MS was used for gradient elution with 0.1%formic acidacetonitrile containing 0.1%formic acid as the mobile phase,and the analytes were separated on a Waters T3-C18(2.1×100 mm,1.8μm)column.Qualitative analysis was performed by electronic spray ionization under a positive ion and negative ion mode with multiple reaction monitoring(MRM).The linearity of the 14 components in the concentration range is good,with the correlation coefficient r≥0.999.The average spiked recoveries of 14 compounds in 4 cosmetic matrices are all in the range of 85%-115%,and the relative standard deviations are all less than 5%.The limits of detections range from 1μg/g to 150μg/g.The limits of quantitation range from 3μg/g to 450μg/g.Seven batches of samples containingα-hydroxy acid and its ester were confirmed by HPLC-MS/MS and the results are positive.The results indicate that the method is simple,sensitive and accurate,and is suitable for the determination of 14 kinds ofα-hydroxy acids and their esters in cosmetics.

关 键 词：化妆品 Α-羟基酸 乳酸甲酯 乳酸乙酯 乳酸丁酯 高效液相色谱法 

分 类 号：TQ658[化学工程—精细化工]