首页> 中文期刊> 《分析测试学报》 >化妆品中5种禁用着色剂的高效液相色谱检测及质谱确证

化妆品中5种禁用着色剂的高效液相色谱检测及质谱确证

         

摘要

An HPLC method was developed for the determination of acid yellow 36, pigment red 53 : 1, pigment orange 5, sudan Ⅱ and sudan Ⅳ in cosmetics. The extraction conditions of five prohibited coloring agents in cosmetic samples, including wax, powder and liquid, were investigated. Using tetrabutylammonium hydroxide as an ion-pair reagent, the optimum chromatographic conditions of the prohibited coloring agents were investigated. The optimal conditions were as the follows: stationary phase; Hypersil C18(4. 6 mm ×250 mm, 5 μm) , mobile phase: acetonitrile(A) -0.01 mol/L tetrabutylammonium hydroxide and 0.01 mol/L citric acid(pH 8.2, B) , flow rate; 1.0 mL/ min, column temperature; 30 ℃ and detection wavelengths; 416, 484, 514 nm. The calibration curves of five prohibited coloring agents showed good linearities in the range of 0. 2 - 50 mg/L with correlation coefficients more than 0. 999 and LODs(S/Af =3) of 0. 2 -0. 5 mg/L. The five prohibited coloring agents were verified by HPLC — MS/MS. At three spiked levels, the average recoveries were between 85% and 102% , with relative standard deviations of 0. 5% - 3. 6% . The method was accurate, simple and rapid, and could be used to determine acid yellow 36, pigment red 53 : 1, pigment orange 5, sudan Ⅱ and sudan Ⅳ in cosmetics.%建立了高效液相色谱测定化妆品中酸性黄36、颜料红53∶1、颜料橙5、苏丹红Ⅱ和苏丹红Ⅳ5种禁用着色剂的分析方法.考察了着色剂使用率较高的蜡质类、固体粉类和液体类基质化妆品中着色剂的最佳提取条件.在流动相中添加离子对试剂四丁基氢氧化铵调节着色剂的色谱保留,使之达到完全分离,最佳色谱条件为:以依利特Hypersil C18(4.6 mm×250 mm,5μm)色谱柱分离,流动相为乙腈-0.01 mol/L四丁基氢氧化铵/0.01 mol/L柠檬酸缓冲溶液(pH 8.2),梯度洗脱,流速1.0 mL/min,柱温30℃,检测波长416、484、514 nm.考察了蜡质类、固体粉类和液体类等不同基质化妆品中着色剂的回收率和精密度.在0.2 ~50mg/L范围内,5种禁用着色剂的线性关系良好,相关系数(r)均大于0.999,仪器检出限(S/N=3)为0.2~0.5 mg/L.采用高效液相色谱-串联质谱法对5种禁用着色剂进行确证,在低、中、高3个添加水平下,5种禁用着色剂的平均回收率为85%~ 102%,相对标准偏差为0.5% ~ 3.6%.该方法准确、简便、快速,可用于化妆品中上述5种禁用着色剂的测定.

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