固相萃取-高效液相色谱法测定化妆品中氢醌和苯酚

Determination of hydroquinone and phenol in cosmetics by solid phase extraction-high performance liquid chromatography

目的建立固相萃取-高效液相色谱法测定化妆品中氢醌、苯酚的分析方法。方法化妆品样品经甲醇提取,提取液经水稀释、PEP固相萃取柱净化后,通过CAPCELL PAK C18MGⅡ(250 mm×4. 6 mm,5μm)色谱柱进行分离,以水-甲醇(40∶60,V/V)作为流动相,进行等度洗脱,流速为1 ml/min,柱温为25℃,进样量为5μl,检测波长为280 nm。结果氢醌、苯酚在2μg/ml～50μg/ml内线性关系良好,相关系数均> 0. 999,检出浓度分别为0. 6μg/g和1. 6μg/g,定量浓度分别为2μg/g和6μg/g,回收率分别为92. 7%～96. 3%和100. 0%～100. 3%,相对标准差分别为0. 5%～0. 6%和0. 3%～0. 4%。采用该方法对收集到的液相色谱法或气质色谱干扰严重样品20余批次进行测定,该法能有效除去化妆品中氢醌、苯酚测定的干扰成分。结论该法简便、快速,可用于基质复杂化妆品中氢醌、苯酚的测定。

Objective To establish a method for the determinations of hydroquinone and phenol in cosmetic by solid phase extraction-high performance liquid chromatography (SPE-HPLC).Methods Cosmetic samples were extracted with methanol and diluted with water.The extractant was purified with PEP SPE column,separated with CAPCELL PAK Cis MG II column (250mm × 4.6mm,5μm)and aqueous-methanol(40"60,V/V)was used as mobile phase.Gradient elution was performed under the following circumstances:the flow rate was 1ml/min,column temperature was 25℃,injection volume was 5μl and detection wavelength was 280 nm.Results The method had good liner relationship in the range of 2μg/ml -50μg/ml, with correlation coefficients(r)greater than 0.999.The limits of detection(LODs)of hydroquinone and phenol were 0.6μg/g and 1.6μg/g,and the limits of quantification(LOQs)were 2μg/g and 6μg/g,respectively.The recoveries of hydroquinone and phenol were within 92.7%-96.3% and 100.0%-100.3%,with relative standard deviations(RSD)of 0.5%-0.6% and 0.3%-0.4%,respectively.Using this method,more than 20 batches of samples with severe liquid chromatography or gas chromatography interference were tested,and the developed method can effectively remove the interference components in the detections of hydroquinone and phenol in cosmetics.Conclusion The method is simple and rapid,and can be used to determine hydroquinone and phenol in cosmetics with complex matrixes.