高效液相色谱-串联质谱法测定香水中24种香料类过敏原物质残留量

doi:10.13218/j.cnki.csdc.2018.08.010

摘要/Abstract

摘要： 建立了高效液相色谱-串联质谱法同时测定香水中24种香料类过敏原物质残留量的方法。样品经乙腈提取,以电喷雾离子源(ESI)、多反应监测模式扫描,外标法定量。结果显示,24种香料类过敏原物质在1.0~5.0 mg/L范围内线性关系良好,仪器检出限为1.0 mg/L,方法的检测限为5.0 mg/kg,定量限为15.0 mg/kg,添加水平为5,10和20 mg/kg时,24种香料类过敏原物质的平均回收率为85.9%~110.0%,精密度为5.5%~12.0% (n=10)。

关键词: 香水, 过敏原, 香料, 高效液相色谱-串联质谱

Abstract: A method of simultaneous determination of 24 allergens in perfume was established with high performance liquid chromatography tandem mass spectrometry.The target compounds were extracted with acetonitrile and determined with HPLC-MS/MS (MRM mode,ESI) with external standard method.The results show that,good linear relationship between concentration and peak area ratio is obtained in the range of 1.0~5.0 mg/L for the 24 allergens.The instrument detection limit is 1.0 mg/L and the method detection limit is 5.0 mg/kg.The limit of quantitation (LOQ) is 15.0 mg/kg.The average recoveries of 24 allergens are 85.9%~110.0% at spiked levels of 5,10 and 20 mg/kg with relative standard derivations (RSDs) of 5.5%~12.0% (n=10).

Key words: perfume, allergen, flavor, high performance liquid chromatography tandem mass spectrometry

中图分类号:

TQ658

王玉健,梁振纲,符灵梅,董存柱. 高效液相色谱-串联质谱法测定香水中24种香料类过敏原物质残留量[J]. 日用化学工业, 2018, 48(8): 472-477.

WANG Yu-jian,LIANG Zhen-gang,FU Ling-mei,DONG Cun-zhu. Determination of 24 allergens in perfume with high performance liquid chromatography tandem mass spectrometry[J]. China Surfactant Detergent & Cosmetics, 2018, 48(8): 472-477.

参考文献

[1] Frequeently Perfume Formula Collection.Domestic-overseas flavor fragrance cosmetic information [J].2003(7):11-12.
[2] Wang Wenhui,Li Linfeng,Lu Xueyan.Common allergens and diagnosis of cosmetic allergic contact dermatitis [J].Chinese Journal of Industrial Medicine,2006(19):223-227.
[3] Directive E U.Direction 2003/15/EC of the European Parliament and the Council of 27 February 2003 amending Council Directive 76/768/EEC on the approximation of the laws of the Member States relating to cosmetic products [J].Official Journal of the European Union,2003,66:26-35.
[4] Goossens A.Contact-allergic reactions to cosmetics [J].Journal of Allergy,2011:1-6.
[5] GB/T 24800.9-2009 Determination of citral,cinnamyl alcohol,anise alcohol,cinammal and coumarin in cosmetics by gas chromatography method [S].Beijing:China Standard Press,2009.
[6] GB/T 24800.10-2009 Determination of 19 flavors in cosmetics by gas chromatography-mass spectrometry method [S].Beijing:China Standard Press,2009.
[7] Wang Chao,Wang Xing,Ji Meiqin.Determination of sixteen flavors in cosmetics by gas chromatography -mass spectrometry [J].Chinese Journal of Analysis Laboratory,2006,25(11):118-122.
[8] Lamas J P,Sanchez-Prado L,Garcia-Jares C,et al.Development of a solid phase dispersion-pressurized liquid extraction method for the analysis of suspected fragrance allergens in leave-on cosmetics [J].Journal of Chromatography A,2010,1217(52):8087-8094.
[9] Celeiro M,Guerra E,Lamas J P,et al.Development of a multianalyte method based on micro-matrix-solid-phase dispersion for the analysis of fragrance allergens and preservatives in personal care products [J].Journal of Chromatography A,2014,1344:1-14.
[10] Villa C,Gambaro R,Mariani E,et al.High-performance liquid chromatographic method for the simultaneous determination of 24 fragrance allergens to study scented products [J].Journal of Pharmaceutical and Biomedical Analysis,2007,44(3):755-762.
[11] Xi Haiwei,Ma Qiang,Li Qiang,et al.Simultaneous determination of 17 allergens in cosetics by high performance liquid chromatography [J].Journal of Instrumental Analysis,2010,29(1):46-50.
[12] Sgorbini B,Ruosi M R,Cordero C,et al.Quantitative determination of some volatile suspected allergens in cosmetic creams spread on skin by direct contact sorptive tape extraction-gas chromatography-mass spectrometry [J].Journal of Chromatography A,2010,1217(16):2599-2605.
[13] Niederer M,Bollhalder R,Hohl C.Determination of fragrance allergens in cosmetics by size-exclusion chromatography followed by gas chromatography-mass spectrometry [J].Journal of Chromatography A,2006,1132(1-2):109-116.
[14] Jiang Jinhua,Chen Sheng,Xie Junxian.Analysis of ten harmful fragrances in cosmetics by GC/FTIR [J].Chinese Journal of Health Laboratory Technology,2005,15(12):1415-1418.
[15] Rey A,Corbi E,Pérès C,et al.Determination of suspected fragrance allergens extended list by two-dimensional gas chromatography-mass spectrometry in ready-to-inject samples [J].Journal of Chroma-tography A,2015,1404:95-103.
[16] Devos C,Ochiai N,Sasamoto K,et al.Full evaporation dynamic headspace in combination with selectable one-dimensional/two-dimensional gas chromatography-mass spectrometry for the determination of suspected fragrance allergens in cosmetic products [J].Journal of Chromatography A,2012,1255:207-215.
[17] Li Shan,Guo Yaqin,Xue Weihong,et al.Application of two-dimensional gas chromatography-mass spectrometry infragrance and flavor analysis [J].Flavour Fragrance Cosmetics,2016(4):22-27,66.

[18] Adahchour M,Brandt M,Baier H U,et al.Comprehensive two-dimensional gas chromatography coupled to a rapid-scanning quadrupole mass spectrometer:principles and applications [J].Journal of Chromatography A,2005,1067(1-2):245-254.
[19] Chaintreau A,Cicchetti E,David N,et al.Collaborative validation of the quantification method for suspected allergens and test of an automated data treatment [J].Journal of Chromatography A,2011,1218(43):7869-7877.
[20] Xu Yuanjin,Li Yongku.Analysis of seven organophosphorous pesticides in vegetables by liquid chromatography-electrospray ion mass spectrometry[J].Journal of Instrumental Analysis,2006,25(4):36-40.