Determination of 48 Glucocorticoids Beyond Statutory Standard Methods in Cream-based Cosmetics by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

SHEN Dan-dan; GONG Shan-shan; LI Yue-chen; XUE Heng-yue; YU Ben-tao; JIANG Bo-hai; WANG Dong; ZHANG Rong; MAO Xi-qin

doi:10.12452/j.fxcsxb.24040601

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Determination of 48 Glucocorticoids Beyond Statutory Standard Methods in Cream-based Cosmetics by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

Scientific Papers | 更新时间：2024-07-08

- Determination of 48 Glucocorticoids Beyond Statutory Standard Methods in Cream-based Cosmetics by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry
- Journal of Instrumental Analysis Vol. 43, Issue 7, Pages: 978-986(2024)
- 作者机构：
  
  1.大连市药品检验检测院，辽宁大连 116021
  2.大连理工大学化工学院，辽宁大连 116024
- 作者简介：
- 基金信息：
- DOI：10.12452/j.fxcsxb.24040601
  CLC： O657.7;TQ658
- Published：15 July 2024，
  
  Received：06 April 2024，
  
  Revised：20 May 2024，
- 稿件说明：
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沈丹丹,宫珊珊,李悦忱,薛恒跃,于本涛,姜博海,王冬,张蓉,毛希琴.超高效液相色谱-串联质谱法测定膏霜乳类化妆品中法定标准以外的48种糖皮质激素[J].分析测试学报,2024,43(07):978-986.

SHEN Dan-dan,GONG Shan-shan,LI Yue-chen,XUE Heng-yue,YU Ben-tao,JIANG Bo-hai,WANG Dong,ZHANG Rong,MAO Xi-qin.Determination of 48 Glucocorticoids Beyond Statutory Standard Methods in Cream-based Cosmetics by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2024,43(07):978-986.
沈丹丹,宫珊珊,李悦忱,薛恒跃,于本涛,姜博海,王冬,张蓉,毛希琴.超高效液相色谱-串联质谱法测定膏霜乳类化妆品中法定标准以外的48种糖皮质激素[J].分析测试学报,2024,43(07):978-986. DOI： 10.12452/j.fxcsxb.24040601.

SHEN Dan-dan,GONG Shan-shan,LI Yue-chen,XUE Heng-yue,YU Ben-tao,JIANG Bo-hai,WANG Dong,ZHANG Rong,MAO Xi-qin.Determination of 48 Glucocorticoids Beyond Statutory Standard Methods in Cream-based Cosmetics by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2024,43(07):978-986. DOI： 10.12452/j.fxcsxb.24040601.

摘要

我国现行法定标准检验方法包括GB/T 24800.2-2009、GB/T 40145-2021和《化妆品安全技术规范》（2015年版），共涵盖58种糖皮质激素。该文以超高效液相色谱-串联质谱法测定膏霜乳类化妆品中法定标准以外的48种糖皮质激素。样品经提取、净化后，通过Waters ACQUITY UPLC BEH C

（3.0 mm×150 mm，1.7 μm）色谱柱分离，以0.2%乙酸水溶液-0.2%乙酸甲醇溶液为流动相梯度洗脱。在电喷雾正离子模式下，以动态多反应监测（MRM）方式测定，外标法定量。48种糖皮质激素在2.5~60 μg/L范围内具有良好的线性关系，相关系数均大于0.995，方法检出限（

≥3）和定量下限（

≥10）分别为 0.03 μg/g和0.1 μg/g。所有目标物在膏霜乳基质中的基质效应不明显。在1倍、2倍和8倍定量下限加标水平下，平均回收率为80.9%~110%，相对标准偏差（RSD，

=6）为0.70%~9.3%。采用该方法在1份样品中检出6

-羟基曲安奈德，含量为0.3 μg/g，并以多反应监测-信息依赖采集-增强子离子扫描模式（MRM-IDA-EPI）进行确证。该方法前处理操作简便可行、测定结果准确可靠，可填补化妆品中糖皮质激素的监管空白。

Abstract

Current domestic statutory inspection methods for glucocorticoids in cosmetics included GB/T 24800.2-2009，GB/T 40145-2021 and the Safety and Technical Specification for Cosmetics（2015 edition），which covered 58 glucocorticoids in total. A method was developed to determine 48 glucocorticoids beyond statutory inspection methods in cream-based cosmetics by ultra high performance liquid chromatography-tandem mass spectrometry. After extraction and purification，samples were loaded on a Waters ACQUITY UPLC BEH C

column（3.0 mm×150 mm，1.7 μm），where aqueous solution containing 0.2% acetic acid and methanol solution containing 0.2% acetic acid were used as mobile phases for gradient elution. After separation of target compounds，an electrospray ionization source in positive mode was used for mass analysis. All target compounds were analyzed with multiple reaction monitoring mode（MRM） and quantified by external standard method. The limits of detection（LODs，

≥3） and the limits of quantification（LOQs，

≥10） of the method for all target compounds were 0.03 μg/g and 0

.1 μg/g.The correlation coefficients（

） of 48 glucocorticoids were greater than 0.995 in the range of 2.5-60 μg/L. The matrix effects（MEs） of 48 kinds of glycocorticoids in cream-based cosmetics were investigated via the addition of standard compounds to the extracted matrix solutions to make matrix standard curves. The MEs of all target compounds were within ±15%，meaning that matrix effects are not significant. The average recoveries were 80.9%-110% with relative standard deviations（RSDs，

=6） of 0.70%-9.3% under spiked levels of 1，2 and 8 times of LOQ. One positive sample was confirmed through multiple reaction monitoring（MRM）-information dependent acquisition automated（IDA）-enhance product ion（EPI） to contain 0.3 μg/g of 6

-hydroxy triamcinolone acetonide. In conclusion，pre-processing method developed in this paper is simple and feasible and measurement results for 48 glucocorticoids are accurate and reliable，which can fill the regulatory gap of illegal addition of glucocorticoids in cosmetics.

关键词

超高效液相色谱-串联质谱糖皮质激素化妆品非法添加

Keywords

ultra high performance liquid chromatography-tandem mass spectrometryglucocorticoidcosmeticillegally added

references

Zhao H. Deterg. Cosmet.（赵华. 日用化学品科学），2016，39（3）：8-10.

Liu H，Zhang J Y，Hu B，Huang W，Liu J，Liu Y Y，Sun C Y，Yi X. Flavour Fragrance Cosmet. （刘红，张静雅，胡贝，黄伟，刘杰，柳艳云，孙春艳，易旋. 香料香精化妆品），2020，（4）：83-86.

Dong Y L，Qiao Y S，Huang C F，Wang H Y，Sun L. Deterg. Cosmet.（董亚蕾，乔亚森，黄传峰，王海燕，孙磊.日用化学品科学），2020，43（5）：28-31.

National Medical Products Administration. No.54 Bulletin of National Medical Products Administration（国家药品监督管理局.国家药品监督管理局2021年第54号通告）. ［2021-07-30］. https：//www.nmpa.gov.cn/xxgk/ggtg/hzhpggtg/hzhpchjgg/hzhpcjgjj/20210730164533187.htmlhttps://www.nmpa.gov.cn/xxgk/ggtg/hzhpggtg/hzhpchjgg/hzhpcjgjj/20210730164533187.html.

National Medical Products Administration. No.9 Bulletin of National Medical Products Administration（国家药品监督管理局.国家药品监督管理局2024年第9号通告）. ［2024-02-04］. https：//www.nmpa.gov.cn/xxgk/ggtg/hzhpggtg/hzhpchjgg/hzhpcjgjj/20240204152921101.htmlhttps://www.nmpa.gov.cn/xxgk/ggtg/hzhpggtg/hzhpchjgg/hzhpcjgjj/20240204152921101.html.

GB/T 24800.2-2009. ofDetermination 41 Glucocorticoids in Cosmetics by LC-MS-MS and TLC Method. National Standards of the People's Republic of China

化妆品中四十一种糖皮质激素的测定液相色谱/串联质谱法和薄层层析法.中华人民共和国国家标准.

National Medical Products Administration. No.66 Bulletin of National Medical Products Administration（国家药品监督管理局. 国家药品监督管理局2019年第66号通告）. ［2019-09-27］. https：//www.nmpa.gov.cn/hzhp/hzhpfgwj/hzhpgzwj/20190927152001264.htmlhttps://www.nmpa.gov.cn/hzhp/hzhpfgwj/hzhpgzwj/20190927152001264.html.

State Food and Drug Administration. Safety and Technical Standard for Cosmetics（2015 Ed）. （国家食品药品监督管理总局. 化妆品安全技术规范），2015.

GB/T 40145-2021.Determination of 11 Glucocorticoids Including Desonide in Cosmetics-Liquid Chromatography-Tandem Mass Spectrometry. National Standards of the People's Republic of China（化妆品中地索奈德等十一种糖皮质激素的测定液相色谱-串联质谱法.中华人民共和国国家标准）.

Weng D H，Liu J，Jiang Q Q，Yang L P，Zheng L，Xiao D Q. Flavour Fragrance Cosmet. （翁东海，刘江，蒋清清，杨乐萍，郑琳，肖道清. 香料香精化妆品），2019，（3）：45-49.

Yang P P，Huang W，Li L X，Liu H. Chin. J. Chromatogr.（杨飘飘，黄伟，李丽霞，刘红. 色谱），2023，41（3）：250-256.

Jian L H，Wang H Y，Yu J，Zheng R，Peng X S. Flavour Fragrance Cosmet. （简龙海，王昊阳，于建，郑荣，彭兴盛. 香料香精化妆品），2023，（2）：46-49.

National Medical Products Administration. No. 141 Bulletin of National Medical Products Administration（国家药品监督管理局. 国家药品监督管理局2032年第141号通告）. ［2023-11-02］. https：//www.nmpa.gov.cn/xxgk/ggtg/hzhpggtg/jmhzhptg/20231102111156175.htmlhttps://www.nmpa.gov.cn/xxgk/ggtg/hzhpggtg/jmhzhptg/20231102111156175.html.

Luo H T，Huang X L，Wu H Q，Zhang Q Y，Zhu Z X，Huang F，Lin X S，Ma Y F，Deng X. Chin. J. Chromatogr. 罗辉泰，黄晓兰，吴惠勤，张秋炎，朱志鑫，黄芳，林晓珊，马叶芬，邓欣．色谱），2017 ，35（8）：816-825.

Zhao Y，Wang T，Hua L，Wang Q F，Bao Y，Liu B，Zhou X R. J. Food Saf. Qual.（赵洋，王婷，华蕾，王庆峰，包懿，刘斌，周欣蕊. 食品安全质量检测学报），2019，10（6）：1559-1564.

Liu H，Yang P P，Li L X. J. Instrum. Anal.（刘红，杨飘飘，李丽霞. 分析测试学报），2020，39（9）：1112-1119.

Ma L B，Sun Y，Zhu G F，Lu J Y，Xu Y，Liu T. China Surfactant Deterg. Cosmet.（马亮波，孙宇，朱桂芳，卢嘉仪，徐燕，刘涛. 日用化学工业），2023，53（7）：849-856.

Zhao Q R，Liu H，Meng Y P，Li X，Gao R F，Li X S. Chin. J. Chromatogr.（赵倩茹，刘骅，孟雅萍，李翔，高瑞芳，李祥胜. 色谱），2023，41（12）：1084-1094.

Luo H T，Huang X L，Wu H Q，Zhang Q Y，Zhu Z X，Huang F，Lin X S. Chin. J. Anal. Chem.（罗辉泰，黄晓兰，吴惠勤，张秋炎，朱志鑫，黄芳，林晓珊. 分析化学），2017，45（9）：1381-1388.

Li Y J，Zhao X L，Cen L Y，Wu Y Y，Luo Z Y. Flavour Fragrance Cosmet. （李杨杰，赵祥龙，岑立怡，伍英英，罗卓雅. 香料香精化妆品），2018，（1）：58-62.

Xu Z D，Chen S B，Gao L，Gu J H，Zhu Z H. Flavour Fragrance Cosmet. 徐振东，陈少波，高玲，顾娟红，朱振华. 香料香精化妆品），2019，（5）：38-42.

Li H Y，Liu Y，Wang W，Lü W，Li L X，Wang H X，Ding X P. Chin. J. Anal. Lab.（李红英，刘芸，汪薇，吕稳，李丽霞，王会霞，丁晓萍. 分析试验室），2020，39（12）：1443-1449.

Zhang Q Y，Yang H S，Shen M F，Zhu X H，Yang Z，Yu J. J. Food Saf. Qual.（张秋云，杨洪生，沈美芳，朱晓华，杨总，于洁. 食品安全质量检测学报），2020，11（15）：5007-5012.

He J W，Wen J X，Liu Y X，Hu J Z，Cao Y J，Lai Y H. Chin. J. Chromatogr.（何嘉雯，温家欣，刘亚雄，胡佳哲，曹雅静，赖宇红. 色谱），2022，40（3）：253-265.

Fan X L，Wu W Q，Huang K，Zhu X L，Wang H X. J. Food Saf. Qual.（范小龙，吴婉琴，黄坤，朱晓玲，王会霞.食品安全质量检测学报），2021，12（1）：86-93.

Qiao Y S，Dong Y L，Huang C F，Wang H Y，Sun L. China Surfactant Deterg. Cosmet.（乔亚森，董亚蕾，黄传峰，王海燕，孙磊. 日用化学工业），2021，51（12）：1259-1268.

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