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日用化学工业(中英文) ›› 2024, Vol. 54 ›› Issue (1): 102-106.doi: 10.3969/j.issn.2097-2806.2024.01.014

• 分析与检测 • 上一篇    下一篇

高效液相色谱法测定化妆品中3种α-羟基酸及其酯

张丽媛,程巧鸳(),陈岑,李泽桦,黄柳倩,戚绿叶   

  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
  • 收稿日期:2023-01-18 修回日期:2023-12-29 出版日期:2024-01-22 发布日期:2024-01-26
  • 基金资助:
    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)

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

Liyuan Zhang,Qiaoyuan Cheng(),Cen Chen,Zehua Li,Liuqian Huang,Lvye Qi   

  1. NMPA Key Laboratory for Animal Alternative Testing Technology of Cosmetics, Zhejiang Institute for Food and Drug Control, Hangzhou, Zhejiang 310052, China
  • Received:2023-01-18 Revised:2023-12-29 Online:2024-01-22 Published:2024-01-26
  • Contact: *Tel.: +86-13675884436, E-mail: chengqiaoyuan@zjyj.org.cn.

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,3 µm)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,1.8 µm)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100 μg/g,乳糖酸的方法检出限为500 μg/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。

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

Abstract:

A method for the simultaneous determination of 3 kinds of α-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, 3 µm) column by elution with 0.04 mol/L diammonium hydrogen phosphate- acetonitrile 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, 1.8 µm) 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 R2>0.999. The detection limits of gluconic acid and glucolactone are 100 μg/g, and that of lactose acid is 500 μg/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 of α-hydroxy acids and their esters in cosmetics.

Key words: cosmetics, gluconic acid, glucolactone, lactose acid, HPLC, HPLC-MS/MS

中图分类号: 

  • TQ658