高效液相色谱-串联质谱法同时测定化妆品中14种禁用着色剂

Simultaneous Determination of 14 Forbidden Colorants in Cosmetics by HPLC-MS/MS

采用液相色谱-质谱联用法建立了同时测定化妆品中14种禁用着色剂（吖啶黄、酸性紫49、溶剂红49、溶剂蓝35、氯化四甲基副玫瑰苯胺、氯化五甲基副玫瑰苯胺、氯化六甲基副玫瑰苯胺、颜料橙5、颜料红53、苏丹红Ⅰ、苏丹红Ⅱ、苏丹红Ⅳ、罗丹明B、分散黄3）的分析方法。待测样品经四氢呋喃分散,并对目标物进行提取后,用含有醋酸铵的甲醇-水混合溶液将基质析出,提取液离心过滤后,以10 mmol/L醋酸铵-乙腈作为流动相在Agilent poroshell 120 EC-C18（2.7μm,3.0 mm×50 mm）色谱柱上梯度洗脱进行分离,以色谱峰的峰面积用标准曲线外标法进行定量。在优化条件下,各目标物的线性范围为0.01～1.0μg/m L,相关系数均大于0.999。14种禁用着色剂的定量下限为0.05～0.5μg/g。在低、中、高3个加标水平下,各目标物的回收率为85.4%～106.3%,相对标准偏差（RSD）均低于10%。方法准确、简便、灵敏、可靠,可用于化妆品中此14种禁用着色剂的定量测定。

An HPLC -MS/MS methord was developed for the simultaneous determination of 14 for- bidden colorants, including metanil yellow, acid violet 49, solvent red 49, solvent blue 35, tetra- methylpararosaniline chloride （ TMPC）, pentamethyhriphenylmethane （ PMTPE ）, hexamethylenepara- rosaniline chloride（HMPC）, pigment orange 5, pigment red 53, sudan I, sudan Ⅱ, Sudan IV, rhodamine B, disperse yellow 3, in cosmetics. Cosmetic samples were extracted and dispersed with tetrahydrofuran, and some matrixes were precipitated out after addition of ammonium acetate solution and methanol. After centrifuged and filtered, the extract was separated on an Agilent poroshell 120 EC - C18 column（2. 7μm, 3.0 mm × 50 mm）by gradient elution with l0 mmol/L ammonium acetate - acetonitrile as mobile phase. The quantitative analysis was performed by the standard curve method of peak area. The linear ranges of 14 analytes were in the range of 0.01 - 1.0μg/mL, with correla- tion coefficients more than 0. 999. The limits of quantitation（LOQs）were in the range of 0.05 -0.5 μg/g. The average recoveries at three spiked levels ranged from 85.4% to 106. 3% with RSDs less than 10% . This method is accurate, simple, sensitive and reliable, and could be used for the anal- ysis of 14 forbidden colorants in cosmetics.