气相色谱-三重四极杆质谱法测定化妆品中α-氯甲苯

Determination ofα-chlorotoluene in cosmetics by gas chromatography-triple quadrupole mass spectrometry

针对《化妆品安全技术规范》(2015年版)中气相色谱法(GC)检测α-氯甲苯的不足,通过对仪器工作条件的优化和样品前处理步骤的改进,采用气相色谱-三重四极杆质谱法(GC-MS/MS)检测技术,建立了化妆品中α-氯甲苯的GC-MS/MS检测方法。本方法专属性良好;在10~200μg/L范围内线性关系良好,线性相关系数(r)为0.9999;定量限、检出限分别为50、15μg/kg;进样精密度的RSD值为1.25%;加标回收率和重复性良好,加标浓度为10、100、200μg/L的低、中、高水平的平均回收率为97.54%~102.78%,对应的RSD值为1.92%~2.26%;中间精密度良好,不同时间、不同人员在同一台仪器上测定结果的RSD值为2.01%;耐用性良好,在原条件、初始柱温±5℃、升温速率±2℃/min、柱流量±0.1 mL/min的条件下检测结果的RSD值为2.10%。选取爽肤水、维生素E乳分别代表液态水基类、膏霜乳液类化妆品,考察本方法的应用效果,结果表明本方法能满足这两类化妆品的检测要求,在液态水基类化妆品中适用性更好。本方法操作简便,专属性强、基质效应低、灵敏度高、结果准确可靠,检测效率高,能同时实现化妆品中α-氯甲苯的含量测定和阳性确证,可为化妆品中α-氯甲苯的检测和监控提供技术支持。

By optimizing the working conditions of the instrument and improving the sample pretreatment steps,the GC-MS/MS method for determination ofα-chlorotoluene in cosmetics was established.The specificity of the method was good.The standard curve was obtained with a good correlation(r=0.9999)in the range 10—200μg/L.The quantitation limits and detection limit were 50μg/kg and 15μg/kg,respectively.The relative standard deviation(RSD)of injection precision was 1.25%.The recoveries and repeatability were good,the average recoveries of low,medium,and high concentration spiked samples were 97.54%—102.78%at spiked concentrations of 10,100 and 200μg/L,respectively.The corresponding RSD was 1.92%—2.26%.The intermediate precision was good,and the RSD of the determination results obtained on the same instrument by different laboratory technicians at different times was 2.01%.The durability was good,under the original condition or conditions with initial column temperature of±5℃,heating rate of±2℃/min,and column flow rate of±0.1 mL/min,the RSD of the detection result was 2.10%.Skin toner and vitamin E emulsion were selected to represent liquid water-based cosmetics and cream emulsion cosmetics respectively,and the application effect of the method was investigated.The results showed that the method could meet the detection requirements of these two kinds of cosmetics,and had better applicability in liquid water-based cosmetics.The method has advantages of simple operation,strong specificity,low matrix effect,high sensitivity,accurate and reliable results,and high detection efficiency.