高效液相色谱-串联质谱法在化妆品违禁药物快速筛查中的应用

doi:10.3969/j.issn.1001-1803.2021.05.015

摘要/Abstract

摘要：

针对化妆品在使用过程中会使人体皮肤出现过敏、炎症等问题,使用高效液相色谱-串联质谱法（HPLC-MS）快速筛查化妆品中8种违禁药物（米诺地尔,雌三醇,螺内酯,坎利酮,雌酮,雌二醇,己烯雌酚,黄体酮）。将化妆品样品经过一定体积比的甲醇-水混合溶液提取后,利用HLB固相萃取柱进行净化处理,采用色谱柱分离复溶后的样液,以浓度为10 mmol/L的甲醇-水作为流动相进行梯度洗脱,并对8种化妆品违禁药物进行定性和定量分析,检测出8种化妆品的回收率为80%~96%,相对标准偏差为3.7%~8.2%,可满足化妆品违禁药物的筛查要求,提高了化妆品中违禁药物快速筛查准确度。

关键词: 高效液相色谱法, 化妆品, 违禁药物, 快速筛查

Abstract:

In response to people’s skin allergies and inflammation during the process of using cosmetics, high-performance liquid chromatography-tandem mass spectrometry （HPLC-MS） was used to quickly screen 8 prohibited drugs （minoxidil, estriol, spironolactone, canrenone, estrone, estradiol, diethylstilbestrol, progesterone prog） in cosmetics. The cosmetic samples were extracted by methanol water mixed solution with a certain volume ratio. HLB solid phase extraction column is used to purify cosmetic samples. The chromatographic column was used to separate the reconstituted sample solution. Methanol-water with a concentration of 10 mmol/L was used as the mobile phase for gradient elution. 8 kinds of prohibited drugs in cosmetics were analyzed qualitatively and quantitatively. Experiments have detected that the recovery rate of 8 kinds of cosmetics are between 80% and 96%. The relative standard deviations of 8 kinds of cosmetics are between 3.7% and 8.2%, which can meet the screening requirements of prohibited drugs in cosmetics and improve the accuracy of rapid screening of prohibited drugs in cosmetics.

Key words: high performance liquid chromatography-tandem mass spectrometry, cosmetics, prohibited drugs, rapid screening

中图分类号:

TQ658

赵峥嵘. 高效液相色谱-串联质谱法在化妆品违禁药物快速筛查中的应用[J]. 日用化学工业, 2021, 51(5): 463-467.

ZHAO Zheng-rong. Application of high performance liquid chromatography-tandem mass spectrometry in rapid screening of prohibited drugs in cosmetics[J]. China Surfactant Detergent & Cosmetics, 2021, 51(5): 463-467.

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参考文献 15

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分析物	碰撞能量/eV	子离子（m/z）	母离子（m/z）	保留时间/min
米诺地尔	25,10	164.1^*,193.2	210.0	8.1
雌三醇	10, 8	278.9^*,320.9	377.2	13.1
螺内酯	35,65	107.1^*, 90.9	210.0	8.1
坎利酮	35,65	107.1^*, 90.9	341.1	13.9
雌酮	5,22	253.1^*,132.8	271.2	14.1
雌二醇	4,14	354.9^*,278.8	477.3	23.3
己烯雌酚	12,14	279.1^*,343.1	479.3	23.6
黄体酮	23,23	97.0^*,109.0	315.2	21.3

违禁药物	波长/nm	回归方程	线性范围/（mg·L^-1）	相关系数	定量限/（mg·kg^-1）
米诺地尔	230	y=110.1x+43.1	0.5~100	0. 999 3	5.0
雌三醇	204	y=59.7x+61.8	0.5~100	0. 999 4	5.0
螺内酯	240	y=36.4x-4.1	0.5~100	0. 999 9	2.0
坎利酮	280	y=59.6x-0.2	0.5~100	0. 999 8	5.0
雌酮	204	y=46.6x+20.0	0.5~100	0. 999 9	5.0
雌二醇	204	y=73.2x+43.4	0.5~100	0. 999 8	5.0
己烯雌酚	204	y=80.2x-40.2	0.5~100	0. 999 6	5.0
黄体酮	240	y=29.6x+49.8	0.5~100	0. 999 7	2.0

名称	样品含量/（mg·kg^-1）	回收率/%	相对标准偏差/%
米诺地尔	5,10,50	81,85,90	8.2,7.3,6.5
雌三醇	5,10,50	82,86,88	6.0,5.6,4.7
螺内酯	5,10,50	83,86,90	6.1,5.4,5.0
坎利酮	5,10,50	86,90,96	5.3,4.7,4.2
雌酮	5,10,50	84,86,91	5.0,4.7,4.3
雌二醇	5,10,50	82,87,90	5.2,4.1,4.0
己烯雌酚	5,10,50	80,84,87	4.9,4.2,3.7
黄体酮	5,10,50	89,89,90	4.5,4.2,3.8