高效液相色谱-串联质谱法同时测定养发类化妆品中15种违禁药物

doi:10.3969/j.issn.1001-1803.2020.05.013

摘要/Abstract

摘要：

建立了高效液相色谱-串联质谱法（HPLC-MS/MS）同时测定养发类化妆品中15种违禁药物的分析方法。样品采用甲醇超声提取,经C₁₈色谱柱分离,采用多反应监测（MRM）扫描方式测定。15种违禁药物的检出限（LODs）为1~20 μg/kg,在10~200 μg/L范围内线性关系良好,相关系数均大于0.998。回收率为84.2%~114.6%,相对标准偏差（RSD,n=6）为1.7%~9.7%。该方法简单、灵敏、准确,可作为养发类化妆品中15种违禁药物的筛查方法。

关键词: 高效液相色谱-串联质谱法, 化妆品, 违禁药物

Abstract:

Liquid chromatography-tandem mass spectrometric （HPLC-MS/MS） method was established for the simultaneous determination of 15 prohibited drugs in hair cosmetics. Samples were extracted by methanol ultrasonic, separated by a C₁₈ column, and determined by multiple reaction monitoring （MRM） scanning mode. The limits of detection （LODs） of the 15 prohibited drugs in various kinds of cosmetics are in the range of 1-20 μg/kg, with a linear relationship in the range of 10-200 μg/L, and the correlation coefficients are all greater than 0.998. The average recoveries are in the range of 84.2%-114.6%, and the relative standard deviation （RSD, n=6） is in the range of 1.7% to 9.7%. The method is simple, sensitive and accurate, and is suitable for the quick screening of 15 prohibited drugs in hair cosmetics.

Key words: HPLC-MS/MS, cosmetics, prohibited drugs

中图分类号:

TQ658

刘红,李晓健,胡贝,李丽霞,丁晓萍. 高效液相色谱-串联质谱法同时测定养发类化妆品中15种违禁药物[J]. 日用化学工业, 2020, 50(5): 354-358.

LIU Hong,LI Xiao-jian,HU Bei,LI Li-xia,DING Xiao-ping. Simultaneous determination of 15 prohibited drugs in hair nourishing cosmetics by HPLC-MS/MS[J]. China Surfactant Detergent & Cosmetics, 2020, 50(5): 354-358.

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参考文献 16

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编号	分析物	保留时间/min	母离子（m/z）	子离子（m/z）	碰撞能量/eV
1	米诺地尔	8.1	210.0	164.1*,193.2	25,10
2	螺内酯	13.9	341.1	107.1*, 90.9	35,65
3	雌酮	14.1	271.2	253.1*,132.8	5,22
4	坎利酮	15.0	341.1	107.1*, 90.9	35,65
5	黄体酮	21.3	315.2	97.0*,109.0	23,23
6	可的松	10.1	361.1	163.1*,121.0	20,30
7	氢化可的松	10.7	363.1	121.0*,327.0	10,25
8	氟米松	11.6	411.1	253.0*,121.1	10,34
9	氟米龙	13.1	377.2	278.9*,320.9	10, 8
10	曲安奈德醋酸酯	17.5	477.3	457.2*,439.1	5,10
11	倍他米松戊酸酯	23.3	477.3	354.9*,278.8	4,14
12	泼尼卡酯	21.9	489.2	114.8*,380.9	12, 6
13	哈西奈德	20.7	455.2	121.0*,104.9	40,48
14	莫米他松糠酸酯	21.3	521.1	503.0*,263.0	4,24
15	氯倍他松丁酸酯	23.6	479.3	279.1*,343.1	12,14

分析物	线性方程	相关系数	回收率/% （RSD/%,n=6）		检出限/ （μg·kg^-1）	定量限/ （μg·kg^-1）
分析物	线性方程	相关系数	水平1	水平2	检出限/ （μg·kg^-1）	定量限/ （μg·kg^-1）
米诺地尔	y=11 558.196 7x-2 442.743 2	0.999 8	91.9（1.7）	100.8（2.3）	1	3
螺内酯	y=312.875 5x+828.202 2	0.999 3	86.4（5.2）	106.3（2.4）	20	60
雌酮	y=1 964.655 8x-2 458.467 0	0.999 9	84.6（3.6）	97.1（1.9）	10	30
坎利酮	y=3 736.962 2x+1 520.313 4	0.999 9	94.8（3.5）	109.1（1.8）	5	15
黄体酮	y=649.832 8x-385.246 5	0.999 9	89.0（4.2）	101.6（2.5）	10	30
可的松	y=500.656 7x+1 595.206 4	0.999 4	94.1（3.5）	110.9（3.2）	10	30
氢化可的松	y=390.418 66x+6 786.174 2	0.999 8	86.2（9.7）	114.6（2.4）	10	30
氟米松	y=398.273 6x+2 465.963 4	0.998 1	92.5（8.2）	114.6（3.8）	10	30
氟米龙	y=1 277.860 9x+5 606.280 1	0.999 0	90.5（5.8）	111.2（1.7）	5	15
曲安奈德醋酸酯	y=2 208.480 8x+2 138.948 1	0.999 7	101.8（7.1）	114.6（4.6）	10	30
倍他米松戊酸酯	y=1 832.935 6x+9 283.597 5	0.998 7	103.8（7.3）	113.1（3.9）	10	30
泼尼卡酯	y=435.779 8x+1 207.266 7	0.999 6	84.2（3.6）	99.4（1.5）	10	30
哈西奈德	y=3 343.852 9x+7 745.213 3	0.999 6	89.6（7.3）	110.9（2.4）	10	30
莫米他松糠酸酯	y=1 432.237 1x-1 308.179 5	0.999 9	95.6（4.9）	111.2（2.1）	10	30