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作 者:郑抒 谢静 秦剑 ZHENG Shu;XIE Jing;QIN Jian(Chongqing Institute for Food and Drug Control,Chongqing 401121,China)
机构地区:[1]重庆市食品药品检验检测研究院,重庆401121
出 处:《中国卫生检验杂志》2022年第24期2979-2982,共4页Chinese Journal of Health Laboratory Technology
摘 要:目的 建立气相色谱-串联质谱(GC-MS/MS)同时检测化妆品中5种氯酚类禁限用物质的方法。方法 目标物采用二氯甲烷作为提取溶剂,超声,经TG-5MS毛细管柱(60 m×0.25 mm×0.25μm)程序升温分离,GC-MS/MS多反应监测(MRM)模式检测,外标法定量。定量限通过分别稀释相应标准溶液至仪器的10倍信噪比(S/N=10)获得,并将该点做为标准曲线最低点,以目标物的质量浓度对相应的峰面积进行线性回归。结果 5种氯酚类物质在对应的线性范围内线性关系良好,相关系数(r)均≥0.998 0。5种氯酚类物质的定量浓度为0.001 6 mg/L~4.8 mg/L。水剂类、乳液膏霜类、粉质类3种基质在低(定量限附近)、中、高3个加标浓度下,方法回收率为80.8%~117.9%,相对标准偏差(RSD)<6%。结论 该方法快速、定性准确、可靠、灵敏度高,能够满足化妆品中5种氯酚类禁限用物质的检测要求。Objective A simultaneous chromatographic separation method for 5 chlorophenols substances in cosmetics was developed using gas chromatography-tandem mass spectrometry(GC-MS/MS). Methods The samples were dissolved in dichloromethane and ultrasonically extracted. 5 chlorophenols were separated under programed temperature elevation, then a TG-5 MS capillary column(60 m×0.25 mm×0.25 μm) was introduced. Their determination was achieved in multiple reaction monitoring(MRM) mode and external standard method were applied for quantitative analysis. The limit of quantitation was obtained by diluting the standard solution to S/N=10, and this point was taken as the lowest point of the standard curve. The corresponding peak area was conducted for linear regression analysis under the mass concentrations of the target objects. Results The 5 chlorophenols compounds presented a good relationship with correlation coefficients(r) higher than or equal to 0.998. Their limit of quantitation concentration is within 0.001 6 mg/L-4.8 mg/L. At three spiked concentration levels, the spiked recoveries were in the range of 80.8%-117.9% for matrix including liquid, emulsion and cream, powdery substrate, and the relative standard deviations(RSD) was less than 6%. Conclusion This method is fast, accurate, reliable and high sensitive, which can be used for the detection of 5 kinds of chlorophenols components in cosmetics.
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