高效液相色谱法测定化妆品中的溴米索伐、卡溴脲和卡立普多及质谱确证

doi:10.3969/j.issn.1001-1803.2021.06.014

摘要/Abstract

摘要：

建立了化妆品中禁用物质溴米索伐、卡溴脲和卡立普多的高效液相色谱分析方法。该方法通过将二极管阵列检测器和蒸发光散射检测器串联使用,实现了3种待测物的同时检测。其中,溴米索伐和卡溴脲采用二极管阵列检测器进行检测,定量限为5 mg/kg,方法平均回收率为90.7%~100.5%,相对标准偏差小于5.8%;卡立普多采用蒸发光散射检测器进行检测,定量限为20 mg/kg,方法平均回收率为96.8%~103.9%,相对标准偏差小于5.9%。对于疑似阳性的样品,进一步采用高效液相色谱-串联质谱法进行确证分析。该方法操作简便,检测时间短,方法学数据满足分析要求,适用于化妆品中禁用物质溴米索伐、卡溴脲和卡立普多的分析。

关键词: 化妆品, 溴米索伐, 卡溴脲, 卡立普多, 高效液相色谱, 质谱确证

Abstract:

An analytical method for the determination of bromisoval, carbromal and carisoprodol in cosmetics was developed based on high-performance liquid chromatography （HPLC）. This method was capable of simultaneously quantifying the three analytes in a single run by combining a diode array detector （DAD） and an evaporative light scattering detector （ELSD） in series. The limits of quantitation （LOQs） for bromisoval and carbromal were 5 mg/kg, and the average recoveries ranged from 90.7% to 100.5% with the relative standard deviations （RSDs） less than 5.8%. The LOQ for carisoprodol was 20 mg/kg, and the average recoveries ranged from 96.8% to 103.9% with the RSDs less than 5.9%. The suspicious samples were subjected to further verification with high-performance liquid chromatography tandem mass spectrometry （HPLC-MS/MS）. This method is simple, fast and suitable for the routine analysis of bromisoval, carbromal and carisoprodol in cosmetics.

Key words: cosmetics, bromisoval, carbromal, carisoprodol, high-performance liquid chromatography, mass spectrometric verification

中图分类号:

TQ658

尚宇瀚,郭项雨,宗艺晶,李焘,李文涛,马强. 高效液相色谱法测定化妆品中的溴米索伐、卡溴脲和卡立普多及质谱确证[J]. 日用化学工业, 2021, 51(6): 564-568.

SHANG Yu-han,GUO Xiang-yu,ZONG Yi-jing,LI Tao,LI Wen-tao,MA Qiang. Determination of bromisoval, carbromal and carisoprodol in cosmetics using HPLC and their verification by HPLC-MS/MS[J]. China Surfactant Detergent & Cosmetics, 2021, 51(6): 564-568.

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待测物	保留时间/min	定性离子对（m/z）	锥孔电压/V	碰撞能量/eV	相对离子丰度/%	允许相对偏差/%
溴米索伐	1.83	223.6/179.9,223.6/57.1	20	14, 18	100,47	±25
卡溴脲	2.27	237.2/194.1,237.2/114.2	30	8, 14	100,80	±20
卡立普多	2.47	261.1/176.1,261.1/62.0	30	6, 15	100,81	±20

化合物	w/（mg·kg^-1）	水剂类化妆品		乳液类化妆品		膏霜类化妆品
化合物	w/（mg·kg^-1）	回收率/%	RSD/%	回收率/%	RSD/%	回收率/%	RSD/%
溴米索伐	5	99.4	1.6	90.7	2.5	97.4	2.0
	10	99.8	1.0	91.6	2.9	99.7	3.4
	50	100.1	1.3	92.7	3.4	98.9	4.6
卡溴脲	5	94.6	3.3	98.7	3.4	96.4	5.8
	10	94.6	3.2	98.9	3.3	100.5	3.9
	50	94.0	3.8	98.9	2.1	95.2	2.6
卡立普多	20	96.8	5.0	102.7	4.5	103.6	3.1
	40	99.7	4.8	103.6	4.2	102.5	3.0
	200	99.1	5.8	103.3	5.9	103.9	4.6