化妆品中的鞣花酸检测方法研究

Research on Determination of Ellagic Acid in Cosmetics

建立了固相萃取-高效液相色谱法检测化妆品中鞣花酸的方法。正交试验结果表明p H对鞣花酸提取效果的影响最大,用体积比1：1的甲醇-水配制0.1 mol/L p H 9甘氨酸-氢氧化钠缓冲溶液10 m L,以此缓冲溶液对样品超声提取20 min最为合适,提取液在10 000 r/min的转速下离心5 min,取5 m L上清液经MAX固相萃取柱处理,以5%（体积分数）甲酸-甲醇溶液洗脱。以MG C18柱（250 mm×4.6 mm×5μm）为固定相,以0.2%磷酸-乙腈（体积比18︰82）为流动相进行洗脱,检测波长为254 nm。该方法线性范围0.5~100 mg/L,检出限、定量下限分别为5.0 mg/kg和20.0 mg/kg,加标回收率83.5%~103.6%。方法简便、准确、能有效去除干扰,适用于化妆品中鞣花酸检测。

A SPE- HPLC method to determine ellagic acid in cosmetics was developed. Orthogonal test showed that p H value affected the result of pre- treatment step mostly. The sample was ultrasonically extracted for 20 min by 0.1 mol/L p H 9 glycine- sodium hydroxide buffer solution prepared with 1/1 methanol- water, then it was centrifugated at 10 000 r/min for 5 min, 5 m L of supernatant was treated by MAX solid phase extraction, eluted by 5% formic acid- methanol solution, finally it was analyzed by MG C18 column（250 mm × 4.6 mm × 5μm）. The mobile phase was 0.2% phosphate acid- acetonitrile（18/82）, detection wavelength was 254 nm. A good linear relationship was obtained between 0.5 mg/L and 100 mg/L. The limit of detection and the limit of quantitation was 5.0 mg/kg（S/N=3） and 20.0 mg/kg（S/N=10）, respectively. The recovery of the method was in the range of 83.5% to 103.6%. The established method was simple, accurate and anti- interference effectly, and it was suitable for analysis of ellagic acid in cosmetics.