静态顶空/气相色谱-质谱法同时测定化妆品中22种有毒挥发性有机溶剂残留

以2015版《化妆品安全技术规范》中规定的常见禁用及限用有毒挥发性有机溶剂为研究对象,建立了静态顶空/气相色谱-质谱法(SHS/GC-MS)同时测定化妆品中22种有毒挥发性有机溶剂(VOC)(二氯甲烷、顺式-1,2-二氯乙烯、反式-1,2-二氯乙烯、2-氯-1,3-丁二烯、三氯甲烷、1,2-二氯乙烷、苯、四氯化碳、三氯乙烯、甲苯、四氯乙烯、氯苯、乙苯、三溴甲烷、间二甲苯、对二甲苯、苯乙烯、邻二甲苯、异丙苯、1,4-二氯苯、1,2-二氯苯、六氯丁二烯)残留的检测方法。试样在80℃下30 min静态顶空,经DB-1柱分离后,采用选择离子监测模式(SIM)进行定性定量分析。优化了顶空、色谱和质谱参数,结果表明:22种VOC在0.5~50 ng/m L浓度范围内均呈良好的线性关系,相关系数均大于0.99,在1.0,2.0,5.0 ng/m L 3个浓度加标水平下的平均回收率为80.3%~102.7%,相对标准偏差(RSD,n=6)为6.4%~9.9%,检出限为0.2~5.0 ng/g。结果表明,该方法简便、灵敏、准确,具有良好的重现性和稳定性,适合于化妆品中22种VOC残留的筛查和确证检测。

Simultaneous Determination of 22 Toxic Volatile Organic Solvent Residues in Cosmetics by Static Headspace/Gas Chromatography-Mass Spectrometry

Based on the Safety and Technical Standards for Cosmetics(2015),a staticheadspace/gas chromatography-mass spectrometric (SHS/GC-MS) method was established to analyze 22 volatile organic compounds (VOCs) residues,including dichloromethane,cis-1,2-dichloroethene,trans-1,2-dichloroethylene,2-chloro-1,3-butadiene,trichloromethane,1,2-dichloroethane,benzene,carbon tetrachloride,trichloroethylene,methylbenzene,tetrachloroethylene,chlorobenzene,ethylbenzene,tribronomethane,m-xylene,p-xylene,phenylethylene,o-xylene,isopropylbenzene,1,4-dichlorobenzene,1,2-dichlorobenzene and hexachlorobutadiene in cosmetics.The experimental conditions for SHS/GC-MS,such as headspace conditions,analytical conditions of GC,quantitative ion's selection and concentration of the samples were optimized.The cosmetic samples were extracted and cleaned-up by headspace at 80 ℃ for 30 min,determined and quantified by MS.22 kinds of VOCs had good linear relations in the range of 0.5-50 ng/mL with correlation coefficients higher than 0.99.The spiked recoveries ranged from 80.3％ to 102.7％,with relative standard deviations (RSD) of 6.4％-9.9％.The limits of detection were in the range of 0.2-5.0 ng/g.This method had the advantages of simplicity,sensitivvity,accurancy,good reproducibility and stability,and was suitable for the screening and analysis of VOCs residues in cosmetics.