气相色谱-质谱联用法测定膏霜类化妆品中10种合成麝香

doi:10.13218/j.cnki.csdc.2017.05.011

摘要/Abstract

摘要： 建立了膏霜类化妆品中10种合成麝香的气相色谱-质谱联用(GC-MS)分析方法。样品加入氘代同位素内标后,用正己烷提取,提取液经基体分散固相萃取(MSPD)净化处理,以VF-WAXms毛细管色谱柱分离,选择特征离子监测(SIM)扫描模式测定,采用标准曲线法定量。结果表明,10种合成麝香的线性范围为0.01～0.2 mg/L,相关系数均大于0.99,定量限为0.05～0.10 mg/kg,加标回收率为80.1%～102.2%,相对标准偏差(RSD)均小于5%。

关键词: 化妆品, 合成麝香, 气相色谱-质谱联用法

Abstract: An analytical method was established for simultaneous determination of ten kinds of synthetic musk in cream cosmetics using gas chromatography-mass spectrometry (GC-MS).Samples were spiked with deuterium-labeled isotope internal standards and extracted by n-hexane.Then the extract was purified with matrix solid-phase dispersion (MSPD) and separated by a VF-WAXms capillary column.All the compounds were detected with selected ion monitoring (SIM) scanning mode.Quantification was carried out using standard plot calibration.Results show that the ten kinds of synthetic musk display a good linear relationship within the mass concentration range of 0.01-0.2 mg/L and the correlation coefficients are all higher than 0.99.The quantification limits (LOQs) of the synthetic musk are in the range of 0.05-0.10 mg/kg.Values of spiked recoveries are found to be from 80.1% to 102.2% with all relative standard deviations (RSD) lower than 5%.

Key words: cosmetics, synthetic musk, gas chromatography-mass spectrometry

中图分类号:

TQ658

宁啸骏, 周静, 符昌雨. 气相色谱-质谱联用法测定膏霜类化妆品中10种合成麝香[J]. 日用化学工业, 2017, 47(5): 292-296.

NING Xiao-jun, ZHOU Jing, FU Chang-yu. Determination of ten kinds of synthetic musk in cream cosmetics by GC-MS[J]. China Surfactant Detergent & Cosmetics, 2017, 47(5): 292-296.

参考文献

[1] Sommer C.The role of musk and musk compounds in the fragrance industry [M]//The Handbook of Environmental Chemistry.Berlin:Springer,2004:1-16.
[2] 吴春英,白鹭,陆文龙,等.气相色谱－串联质谱法同时快速检测环境水样中11种合成麝香[J].分析科学学报,2016,32(2):188-192.
[3] 顾越,李晓静,梁高峰,等.淀山湖水、沉积物和鱼体中的合成麝香及人体暴露评估[J].环境科学学报,2017,37(1):388-394.
[4] 周静.上海地区合成麝香和有机氯农药的母婴暴露及人体传递特征研究[D].上海:上海大学,2012.
[5] 王冠.麝香类香料的合成研究进展[J].香料香精化妆品,2016(1):61-72.
[6] 刘志红.合成麝香与生态风险[J].化学教育,2010(12):1-6.
[7] Slanina P.Risk evaluation of dietary and dermal exposure to musk fragrances [M]//The Handbook of Environmental Chemistry.Berlin:Springer,2004:281-310.
[8] The Commission of the European Communities.Commission Directive 2008/42/EC [S/OL].The Commission of the European Communities,2008:13-23.http://eur-lex.europa.eu/eli/dir/2008/42/oj.
[9] The Commission of the European Communities.Commission Directive 2004/88/EC [S/OL].The Commission of the European Communities,2004:72-73.http://eur-lex.europa.eu/eli/dec/2004/88(1)/oj.
[10] 马强,白桦,王超,等.固相萃取-同位素稀释-气相色谱-串联质谱法测定化妆品中的二甲苯麝香[J].分析化学研究报告,2009,37(12):1776-1780.
[11] 郑小严.固相萃取-气相色谱-串接质谱法测定化妆品中的人工合成硝基麝香类化合物[J].分析科学学报,2012,28(5):634-638.
[12] 陈志蓉,高晓譞,穆旻,等.反相高效液相色谱法测定化妆品中的酮麝香[J].科技导报,2011,29(21):41-44.
[13] 闫俊秀.化妆品中2种限用硝基麝香和4种禁用亚硝基类物质的检测研究[D].上海:上海应用技术学院,2011.
[14] 赵田甜,李慧勇,李焯原,等.气相色谱串联质谱法测定洗涤剂中的7种人工合成麝香[J].分析仪器,2015(3):1-4.
[15] 李懿睿,武晓剑,王东辉,等.气相色谱/质谱法测定化妆品中5种麝香类禁限用物质[J].香料香精化妆品,2013,8(4):24-25.
[16] 张玮,张岩,李高杰,等.气相色谱-质谱法测定化妆品中5种合成麝香[J].河北省科学院学报,2012,29(4):59-66.
[17] Llompart M,Celeiro M,Lamas J P,et al.Analysis of plasticizers and synthetic musks in cosmetic and personal care products by matrix solid-phase dispersion gas chromatography-mass spectrometry [J].Journal of Chromatography A,2013,1293:10-19.
[18] Dong H F,Tang H,Chen D Z,et al.Analysis of 7 synthetic musks in cream by supported liquid extraction and solid phase extraction followed by GC-MS/MS [J].Talanta,2014,120:248-254.