顶空-气相色谱-质谱法测定化妆品中33种有害挥发性有机溶剂OA
Determination of 33 Harmful Volatile Organic Solvents in Cosmetics by Headspace-Gas Chromatography-Mass Spectrometry
该研究建立了同时测定化妆品中33种有害挥发性有机溶剂(VOCs)的顶空-气相色谱-质谱(HS-GC-MS)分析方法.样品经甲醇分散并加水稀释后,于65 ℃下平衡30 min,采用VF-1301毛细管色谱柱(30m× 0.25 mm×1 μm)分离,选择离子监测(SIM)模式检测.定量分析以甲苯-D8和1,2-二氯苯-D4为内标物,并依据不同基质特性,分别采用溶剂或基质标准曲线进行测定.结果表明,33种VOCs在一定质量浓度范围内均呈良好的线性关系,相关系数(r)为0.995 1~0.999 8,方法检出限为0.02~0.40 mg·kg-1,定量下限为0.05~1.0mg·kg-1.在3个加标水平下,水剂、膏霜、凝胶、乳液、粉剂5种基质的平均回收率为85.1%~119%,相对标准偏差(RSD)为0.20%~8.4%.应用所建方法测定169批市售化妆品,共78批样品检出目标物,其中甲苯、邻二甲苯、乙苯、间/对二甲苯、苯的检出率较高,分别为34.9%、20.1%、20.1%、17.8%和10.1%.阳性样品主要集中于防晒类和染发类化妆品,11批染发类化妆品中苯含量超过限值(2.0 mg·kg-1),3批其余类别产品中分别检出禁用原料二氯甲烷、三氯甲烷.该方法简便、快速,灵敏度与准确度良好,适用于化妆品中33种有害挥发性有机溶剂的检测.
In this study,an analytical method based on headspace-gas chromatography-mass spec-trometry(HS-GC-MS)was established for the simultaneous determination of 33 harmful volatile or-ganic solvents(VOCs)in cosmetics.The sample was prepared by dispersion in methanol followed by dilution with water,and equilibrated at 65℃ for 30 min.The separation was performed on a VF-1301 capillary column(30 m×0.25 mm×1 μm),and detection was carried out in selected ion moni-toring(SIM)mode.Quantification was performed using toluene-D8 or 1,2-dichlorobenzene-D4 as in-ternal standards.The selection of solvent calibration curves or matrix-matched calibration curves was based on the properties of each matrix.The results showed good linearity of 33 VOCs in corresponding concentration ranges,with the correlation coefficients(r)ranging from 0.995 1 to 0.999 8.The lim-its of detection(LODs)ranged from 0.02 to 0.40 mg·kg-1,and the limits of quantification(LOQs)ranged from 0.05 to 1.0 mg·kg-1.At three spiked levels,the average recoveries of the five matrices(aqueous,cream,gel,lotion and powder)ranged from 85.1%to 119%,with relative standard de-viations(RSDs)between 0.20%and 8.4%.The method was used to analyze 169 commercially avail-able cosmetic products,and 78 batches were found to contain the target compounds.Among them,toluene,o-xylene,ethylbenzene,m-xylene & p-xylene,and benzene showed relatively high detec-tion rates of 34.9%,20.1%,20.1%,17.8%and 10.1%,respectively.Positive samples were mainly concentrated in sunscreen and hair dye cosmetics.The content of benzene exceeded the limit(2.0 mg·kg-1)in 11 batches of hair dye cosmetics,and prohibited raw materials such as dichloro-methane and trichloromethane were detected in 3 batches of other product types.The method is sim-ple,rapid,sensitive,and accurate,making it suitable for high-throughput detection of various harmful VOCs in cosmetics.
简育莹;卓婧;张丽蓉;陈硕;卢端萍;张伟清
福建省食品药品质量检验研究院,福建 福州 350012福建省食品药品质量检验研究院,福建 福州 350012福建省食品药品质量检验研究院,福建 福州 350012福建省食品药品质量检验研究院,福建 福州 350012福建省食品药品质量检验研究院,福建 福州 350012中国食品药品检定研究院,北京 100050
化学化工
顶空-气相色谱-质谱法化妆品挥发性有机溶剂苯系物禁用原料
headspace-gas chromatography-mass spectrometrycosmeticsvolatile organic sol-ventsbenzene seriesprohibited raw materials
《分析测试学报》 2026 (9)
1933-1942,10
福建省药品监督管理局科技项目(SYJ2025008)
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