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

Abstract

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

CLC Number:

TQ658

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.

Figures/Tables 6

Tab. 1

Tab. 2

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Tab. 4

References 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

提取溶剂	回收率/%
提取溶剂	甲醇	乙腈	丙酮	乙酸乙酯	水+乙酸乙酯	5%氨水+乙酸乙酯	1%醋酸+乙酸乙酯
米诺地尔	103	92	91	31	38	18	18
雌三醇	99	95	87	86	84	90	90
螺内酯	101	103	92	85	72	90	90
坎利酮	100	100	91	87	80	90	90
雌酮	104	101	101	83	82	87	87
雌二醇	105	104	109	86	79	87	87
己烯雌酚	94	100	99	80	79	80	80
黄体酮	100	101	91	84	74	86	86

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

Application of high performance liquid chromatography-tandem mass spectrometry in rapid screening of prohibited drugs in cosmetics

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