固相萃取-超高效液相色谱-质谱法测定化妆品中9种α-羟基酸
左家信, 冯家力, 曾栋, 陈东洋, 李帮锐, 张昊, 刘先军, 钟旋, 梁静, 鲁兵
湖南省疾病预防控制中心,湖南 长沙 410005
Determination of nine α-hydroxy acids in cosmetics by solid phase extraction-ultrahigh performance liquid chromatography-mass spectrometry
ZUO Jiaxin, FENG Jiali, ZENG Dong, CHEN Dongyang, LI Bangrui, ZHANG Hao, LIU Xianjun, ZHONG Xuan, LIANG Jing, LU Bing
Hunan Provincial Center for Disease Control and Prevention, Changsha, Hunan 410005, China
摘要 目的 建立了固相萃取-超高效液相色谱-质谱法测定化妆品中9种α-羟基酸的方法。 方法 样品采用0.1%氨水提取,PAX固相萃取柱净化,以0.1%甲酸-水溶液和0.1%甲酸乙腈溶液为流动相梯度洗脱,HSS T3色谱柱分离。质谱采用多反应监测负离子模式,外标法定量。 结果 9种α-羟基酸在相应的浓度范围内(酒石酸0.2~20 mg/L、羟基乙酸10~400 mg/L、苹果酸0.05~10 mg/L、乳酸1.0~50 mg/L、柠檬酸1.0~50 mg/L、2-羟基丁酸1.0~100 mg/L、扁桃酸0.1~10 mg/L、羟基辛酸0.005~1.0 mg/L、二苯乙醇酸0.05~5.0 mg/L)具有较好的线性相关性,相关系数均大于0.99,方法定量限为0.25~50 μg/g。回收率为80.3%~111.9%,相对标准偏差为2.8%~8.2%。 结论 该方法灵敏、准确以及提取率好,适用于化妆品中α-羟基酸的准确定性与定量分析。
关键词 ：
固相萃取 ,
超高效液相色谱 ,
质谱法 ,
α-羟基酸 ,
化妆品
Abstract ：Objective To develop a method of solid phase extraction-ultrahigh performance liquid chromatography-mass spectrometry for detecting nine α-hydroxy acids in cosmetics. Methods Samples were extracted with 0.1% ammonia, cleaned up on a PAX SPE column, and separated on the HSS T3 column with a mixture of 0.1% formic acid in water-0.1% formic acid in acetonitrile as mobile phase by means of gradient elution. The nine α-hydroxy acids were determined by UPLC-MS/MS using multiple reaction monitoring (MRM) and electrospray ionization in negative ion mode and external standard method for quantitative detection. Results The nine α-hydroxy acids had good linear relationships in the corresponding concentration ranges (tartaric acid 0.2-20 mg/L, glycolic acid 10-400 mg/L, malic acid 0.05-10 mg/L, lactic acid 1.0-50 mg/L, citric acid 1.0-50 mg/L, DL-2-hydroxybutyric acid 1.0-100 mg/L, mandelic acid 0.1-10 mg/L, hydroxycaprylic acid 0.005-1.0 mg/L, benzilic acid 0.05-5.0 mg/L), with the correlation coefficients all greater than 0.99. The limits of quantification were 0.25-50 μg/g. The recoveries ranged from 80.3% to 111.9%, and the relative standard deviations (RSDs) ranged from 2.8% to 8.2%. Conclusion The method is sensitive and accurate, with a good extraction rate. It is suitable for the confirmation and quantification of α-hydroxy acids in cosmetics.
Key words ：
solid phase extraction
ultrahigh performance liquid chromatography
mass spectrometry
α-hydroxy acid
cosmetic
收稿日期: 2023-05-02
通讯作者:
鲁兵,E-mail:1325349410@qq.com。
作者简介 : 左家信(1986-),男,硕士,主管技师,研究方向:食品化妆品安全技术研究。
引用本文:
左家信, 冯家力, 曾栋, 陈东洋, 李帮锐, 张昊, 刘先军, 钟旋, 梁静, 鲁兵. 固相萃取-超高效液相色谱-质谱法测定化妆品中9种α-羟基酸[J]. 实用预防医学, 2023, 30(10): 1218-1222.
ZUO Jiaxin, FENG Jiali, ZENG Dong, CHEN Dongyang, LI Bangrui, ZHANG Hao, LIU Xianjun, ZHONG Xuan, LIANG Jing, LU Bing. Determination of nine α-hydroxy acids in cosmetics by solid phase extraction-ultrahigh performance liquid chromatography-mass spectrometry. , 2023, 30(10): 1218-1222.
链接本文:
https://www.syyfyx.com/CN/10.3969/j.issn.1006-3110.2023.10.015 或 https://www.syyfyx.com/CN/Y2023/V30/I10/1218
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2023, Vol. 30 
