高效液相色谱法测定化妆品中3种α-羟基酸及其酯  

Determination of 3 kinds ofα-hydroxy acids and their esters in cosmetics by high performance liquid chromatography

作　　者：张丽媛 程巧鸳 陈岑 李泽桦 黄柳倩 戚绿叶 Liyuan Zhang;Qiaoyuan Cheng;Cen Chen;Zehua Li;Liuqian Huang;Lvye Qi(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1期102-106,共5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(2021036)。

摘　　要：建立了高效液相色谱法(HPLC)同时测定化妆品中葡糖酸、葡糖酸内酯和乳糖酸的含量,并结合高效液相色谱-串联质谱联用法(HPLC-MS/MS)对结果进行确证。样品经水超声提取,并在氢氧化钠的作用下将葡糖酸、葡糖酸内酯、乳糖酸转化为葡糖酸盐和乳糖酸盐,采用高效液相色谱法,以0.04 mol/L的磷酸氢二铵水溶液和乙腈为流动相进行洗脱,Comixsil HCS(4.6 mm×150 mm,3μm)色谱柱分离,二极管阵列检测器(214 nm)检测,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,Waters T3-C18(2.1 mm×100 mm,1.8μm)色谱柱分离,电喷雾电离,负离子多反应监测模式定性。结果显示,葡糖酸与乳糖酸在相应线性范围内线性关系良好,相关系数均大于0.999。葡糖酸与葡糖酸内酯的方法检出限为100μg/g,乳糖酸的方法检出限为500μg/g。3种化合物4种基质样品加标平均回收率为90.8%~110.1%,相对标准偏差为0.3%~4.4%。该方法操作简便、准确度好、灵敏度高,适用于化妆品中葡糖酸、葡糖酸内酯和乳糖酸的测定。A method for the simultaneous determination of 3 kinds ofα-hydroxy acids and their esters in cosmetics,including gluconic acid,glucolactone and lactose acid,was developed by high performance liquid chromatography(HPLC),and the results were confirmed by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The above three substances were extracted ultrasonically with water.The analytes were separated on a Comixsil HCS(4.6 mm×150 mm,3μm)column by elution with 0.04 mol/L diammonium hydrogen phosphateacetonitrile as mobile phase,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 acid-acetonitrile containing 0.1%formic acid as mobile phase.The analytes were separated on a Waters T3-C18(2.1 mm×100 mm,1.8μm)column.Qualitative analysis was performed by electronic spray ionization under a negative ion mode with multiple reaction monitoring(MRM).The results indicate that gluconic acid and lactose acid show good linearity in its own concentration range with the correlation coefficient of R^(2)>0.999.The detection limits of gluconic acid and glucolactone are 100μg/g,and that of lactose acid is 500μg/g.The average spiked recoveries of these three compounds in 4 cosmetic matrices are all in the range of 90.8%-110.1%,with the RSDs of 0.3%-4.4%.The results indicate that the method is simple,sensitive and accurate,and is suitable for the determination of 3 kinds ofα-hydroxy acids and their esters in cosmetics.

关 键 词：化妆品 葡糖酸 葡糖酸内酯 乳糖酸 高效液相色谱法 高效液相色谱-质谱联用法 

分 类 号：TQ658[化学工程—精细化工]