油基顶空-气相色谱-质谱法测定化妆品中甲醛研究  

Determination of formaldehyde in cosmetics by oil based headspace-gas chromatography-mass spectrometry

作　　者：李欣[1] 李帮锐[1] 李谭瑶[1] 范翔[1] 冯家力[1] 曾栋[1] 陈东洋[1] LI Xin;LI Bangrui;LI Tanyao;FAN Xiang;FENG Jiali;ZENG Dong;CHEN Dongyang(Hunan Provincial Center for Disease Control and Prevention,Changsha,Hunan 410005,China)

机构地区：[1]湖南省疾病预防控制中心,湖南长沙410005

出　　处：《实用预防医学》2023年第10期1214-1217,共4页Practical Preventive Medicine

摘　　要：目的开发油基顶空-气相色谱-质谱联用技术,用于测定化妆品中甲醛的含量。方法N,N-二甲基甲酰胺经净化去除甲醛本底后作为样本分散提取剂,顶空-气相色谱-质谱法测定化妆品中的甲醛。结果通过对色谱条件、顶空条件和样本分散溶剂进行优化,甲醛在1~400 mg/L范围内,峰面积与浓度线性关系良好,回归方程相关系数r=0.9993;甲醛在不同剂型化妆品中低、中、高3个浓度水平的加标回收率在90.1%~105.2%之间,相对标准偏差在1.8%~3.7%之间;方法检出限为5 mg/kg,定量限为10 mg/kg。对市售6种不同类型共8批次的化妆品样本进行了测定,其中6份样本检出甲醛,含量在15.1~49.7 mg/kg之间。结论本法采用N,N-二甲基甲酰胺作为分散剂,利用对脂溶、水溶性化合物均有较强的溶解能力,达到对各种基质化妆品样本较好的分散效果;同时利用其沸点高,通过控制顶空温度,采用顶空-气相色谱质谱法测定,有效降低了基质干扰。该方法操作简单,抗干扰能力强,灵敏高,准确可靠。Objective To develop an oil based headspace technique coupled with gas chromatography-mass spectrometry for determination of formaldehyde in cosmetics.Methods N,N-dimethylformamide was used as the sample dispersant after removing formaldehyde and purification,and headspace-gas chromatography-mass spectrometry was employed to detect formaldehyde in cosmetics.Results In this method,the chromatographic conditions,headspace conditions and dispersion solvents of the samples were optimized.The results displayed that the linearity of formaldehyde was good in the range of 1-400 mg/L,and the correlation coefficient(r)was 0.9993.The recoveries of formaldehyde at low-,medium-and high-concentration levels in different dosage forms of cosmetics ranged from 90.1%to 105.2%,with a relative standard deviation of 1.8%-3.7%.The detection limit was 5 mg/kg,and the quantitative limit 10 mg/kg.Totally eight batches of cosmetic samples with 6 different types sold in the markets were determined,and formaldehyde was detected in 6 samples,with the content ranging from 15.1 mg/kg to 49.7 mg/kg.Conclusion In this method,N,N-dimethylformamide was used as extractant and good dispersion effect for various matrix cosmetics samples was achieved,because it had strong dissolving ability for both fat-soluble and water-soluble compounds.Furthermore,it had high boiling point,and the method effectively reduced matrix interference by controlling the headspace temperature.The actual measurement of samples shows that the method has the advantages of simple operation,strong anti-interference ability,high sensitivity,accuracy and good reliability.

关 键 词：甲醛 化妆品 油基顶空 气相色谱-质谱 

分 类 号：R155.6[医药卫生—营养与食品卫生学]