分散固相萃取-液相色谱-串联质谱法同时快速测定化妆品中81种糖皮质激素

引用本文: 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. 分散固相萃取-液相色谱-串联质谱法同时快速测定化妆品中81种糖皮质激素[J]. 色谱, 2017, 35(8): 816-825. doi: 10.3724/SP.J.1123.2017.04005 shu

Citation: LUO Huitai, HUANG Xiaolan, WU Huiqin, ZHANG Qiuyan, ZHU Zhixin, HUANG Fang, LIN Xiaoshan, MA Yefen, DENG Xin. Simultaneous rapid determination of 81 glucocorticoids in cosmetics by dispersive solid phase extraction and liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2017, 35(8): 816-825. doi: 10.3724/SP.J.1123.2017.04005 shu

分散固相萃取-液相色谱-串联质谱法同时快速测定化妆品中81种糖皮质激素

中国广州分析测试中心, 广东省化学危害应急检测技术重点实验室, 广东广州 510070
基金项目:
广东省省级科技计划项目（2014A040401038，2014B070705001）.

摘要: 建立了分散固相萃取-液相色谱-串联质谱同时快速测定化妆品中81种非法添加糖皮质激素（GCs）的分析方法。样品用水分散后加乙腈超声提取，经十八烷基键合硅胶（C₁₈）和N-丙基乙二胺（PSA）净化，待测物选用具有多重色谱保留模式的Poroshell 120 PFP色谱柱（100 mm×2.1 mm，2.7 μ m）分离，以0.2%（v/v）乙酸水溶液-乙腈为流动相梯度洗脱，在电喷雾正离子模式下以动态多反应监测方式测定，内标法定量。81种待测物在各自的浓度范围内线性关系良好，相关系数均大于0.99，在3个不同的添加水平下，平均回收率为68.8%~105.3%，RSD为2.9%~13.1%（n=6），方法的检出限（S/N≥3）和定量限（S/N≥10）分别为0.002~0.006 μ g/g和0.005~0.020 μ g/g。筛查了137个化妆品样品，发现16个阳性样品，含量为16.9~158 μ g/g。结果表明，该法简便快速，灵敏可靠，适用于化妆品中81种GCs的同时快速定性定量筛查分析。

关键词:

English

Simultaneous rapid determination of 81 glucocorticoids in cosmetics by dispersive solid phase extraction and liquid chromatography-tandem mass spectrometry

Guangdong Provincial Key Laboratory of Emergency Test for Dangerous Chemicals, China National Analytical Center(Guangzhou), Guangzhou 510070, China
Received Date: 05 April 2017
Fund Project:
Science and Technology Plan Project of Guangdong Province of China (Nos. 2014A040401038, 2014B070705001).

Abstract: A novel method was developed for the simultaneous rapid determination of 81 illegally added glucocorticoids (GCs) in cosmetics using dispersive-solid phase extraction (d-SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). The analytes were extracted by acetonitrile after dispersing with water, and then purified using the C₁₈ and primary secondary amine (PSA). The chromatographic separations were performed on a Poroshell 120 PFP column (100 mm×2.1 mm, 2.7 μ m) under multiple chromatographic retention modes. Acetonitrile and 0.2% (v/v) acetic acid aqueous solution were used as mobile phases with gradient elution, and all the 10 groups of isomers were baseline separated. The qualitative identification and quantitative analysis of the 81 GCs were operated in the electrospray ionization positive mode using dynamic multiple reaction monitoring (DMRM). The 81 GCs finally were quantified by internal standard method. The correlation coefficients of linear calibration curves were greater than 0.99 in the corresponding mass concentration ranges. The average recoveries of the 81 GCs at three spiked levels ranged from 68.8% to 105.3% with relative standard deviations (RSDs) of 2.9%-13.1% (n=6). The LODs (S/N ≥ 3) and LOQs (S/N ≥ 10) were 0.002-0.006 μ g/g and 0.005-0.020 μ g/g, respectively. A number of 137 cosmetic samples submitted by customers were screened. Sixteen positive samples were found, and the contents of GCs were from 16.9 μ g/g to 158 μ g/g. The results showed that the new method is simple, rapid, sensitive and reliable, and it is suitable for qualitative and quantitative screening analysis of the 81 GCs in cosmetics simultaneously.

Key words:

liquid chromatography-tandem mass spectrometry (LC-MS/MS)
/ dispersive-solid phase extraction (d-SPE)
/ isotope dilution
/ illegally added
/ glucocorticoids (GCs)
/ cosmetics

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分散固相萃取-液相色谱-串联质谱法同时快速测定化妆品中81种糖皮质激素

English

Simultaneous rapid determination of 81 glucocorticoids in cosmetics by dispersive solid phase extraction and liquid chromatography-tandem mass spectrometry

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

分散固相萃取-液相色谱-串联质谱法同时快速测定化妆品中81种糖皮质激素

English

Simultaneous rapid determination of 81 glucocorticoids in cosmetics by dispersive solid phase extraction and liquid chromatography-tandem mass spectrometry

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

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