高效液相色谱法测定化妆品中17种紫外线吸收剂

为避免使用四氢呋喃和高氯酸这样高腐蚀性的溶剂作流动相,本文从样品前处理方法、色谱柱的选择和流动相条件的优化等方面对《化妆品卫生规范》规定的15种紫外线吸收剂的高效液相色谱测定方法进行了改进,并将目标物检测范围扩大为17种。样品用四氢呋喃/甲醇/水体系提取,离心过滤后,以Phenomenex PFP柱(250 mm×4.6 mm, 5 μm)为分离色谱柱,以20%异丙醇的甲醇溶液(含0.1%甲酸)和水溶液(含0.1%甲酸)作为流动相,梯度洗脱,以311 nm和280 nm为检测波长,进行定性和定量分析。回收率试验及实际阳性样品测定均表明将本方法用于化妆品中17种紫外线吸收剂的测定,结果准确、可靠。与《化妆品卫生规范》方法相比,普通液相色谱仪无需改进即可实现17种紫外线吸收剂的同时检测,增加了方法的普适性,同时所有目标化合物全部基线分离,分离度的提高增加了定量的准确性。

Determination of 17 ultraviolet-filters in cosmetics by high performance liquid chromatography

An optimum HPLC method was developed for the simultaneous determination of 17 ultraviolet (UV)-filters in cosmetics, in which two UV-filters were included more than the 15 UV-filters specified in the Hygenic Standard for Cosmetics (HSC). Our research focused on the optimization of sample processing, chromatographic column, and mobile phase, in order to avoid the use of highly corrosive solvents as tetrahydrofuran (THF) and perchloric acid, which are used in the HSC method. The cosmetic sample was extracted by the mixed solution of THF/methanol/water. The target chemicals were separated on a Phenomenex PFP column (250 mm×4.6 mm, 5 μm) in gradient elution mode using water solution (containing 0.1% formic acid) and 20% methanol solution of isopropyl alcohol (containing 0.1% formic acid) as mobile phases. The detection wavelengths were set at 311 nm and 280 nm. The results of recovery tests and samples analysis indicated that the developed method can be used to simultaneously determine the 17 UV-filters in cosmetics, accurately and reliably. It is a more universal analytical method than the HSC method because common HPLC pump without improvement to adapt to corrosive THF, can be used. At the same time, the quantitative accuracy can be improved because baseline separation of all target chemicals was achieved.