高效液相色谱法同时测定化妆品中的8种硝基苯类化合物

Simultaneous determination of 8 nitrobenzenes in cosmetics by high performance liquid chromatography

目的建立了同时测定化妆品中硝基苯、3,4-二硝基甲苯、2,3-二硝基甲苯、2,6-二硝基甲苯、2,5-二硝基甲苯、3,5-二硝基甲苯、2-硝基甲苯、1-氯-4-硝基苯共8种硝基苯类化合物的高效液相色谱-二极管阵列分析方法。方法水剂和粉剂样品用甲醇提取,膏霜类样品用乙酸乙酯提取,高速离心后,目标化合物以水∶甲醇∶乙腈=55∶40∶5(v∶v∶v)为流动相,过XDB-C18色谱柱(5μm,4.6 mm×150 mm)分离,用二极管阵列检测器进行定性定量分析。结果 8种硝基苯类化合物浓度在0.67 mg/L^33.3 mg/L范围内具有良好的线性,相关系数大于0.999,方法检出限为0.83 mg/kg^2.1 mg/kg;在低、中、高的3个添加水平的平均回收率为82%~103%,相对标准偏差为2.0%~6.2%。结论方法简单、准确、回收率良好,能够满足膏霜、水剂、粉状等种类繁多的化妆品样品的测定。

Objective To develop an efficient method for analysis of 8 nitrobenzene compounds in cosmetics,including nitrobenzene,3,4-dinitrotoluene,2,3-dinitrotoluene,2,6-dinitrotoluene,2,5-dinitrotoluene,3,5-dinitrotoluene,2-nitrotoluene and 1-chloro-4-nitrobenzene by reversed-phase high performance liquid chromatography. Methods The lotion and powder samples were extracted with methanol,while the cream samples were extracted with ethyl acetate. Then the extracts were centrifuged at high speed,and the target compounds were separated on an XDB-C18 column（ 5 μm,4. 6 mm × 150 mm） using water/ methanol/ acetonitrile = 55/40/5（ v/ v/ v） as mobile phase at a flow rate of 1. 0 ml/ min,and finally detected with diode array detector for qualitative and quantitative analysis. Results The 8 kinds of nitrobenzenes were linear in the concentrations of 0. 67 mg/ L - 33. 3 mg/ L with correlation coefficients more than 0. 999. The detection limits of the method were from 0. 83 mg/ kg to 2. 1 mg/ kg. The mean recoveries at three spiked levels were from 82% to 103% with relative standard deviations from 2. 0% to 6. 2%. Conclusion The method is simple and accurate with good recovery,and it is applicable to simultaneously analyze the nitrobenzens in different cosmetics samples,including lotion,powder and cream.