测定美白类化妆品中氢醌和苯酚的高效液相色谱法改进研究

目的：对高效液相色谱法测定美白类化妆品中氢醌、苯酚的色谱条件进行优化。方法：以系统适用性为指标，比较了色谱柱类型、缓冲盐种类及流动相pH 对氢醌、苯酚和化妆品样品分离效果的影响。对优化后色谱条件进行了方法学考察，并在此条件下对抽检的化妆品样品进行测定。结果：最优色谱条件：采用C₁₈（4.6 mm×250 mm，5 μm）色谱柱，以10 mmol·L^-1 磷酸二氢钾水溶液（磷酸调pH 3.5）-甲醇为流动相进行梯度洗脱，流速1 mL·min^-1，柱温25 ℃，检测波长280 nm，进样量5 μL。在最优色谱条件下，氢醌质量浓度在0.4~40 μg·mL^-1 范围内，苯酚质量浓度在0.7~70 μg·mL^-1 范围内线性关系良好，相关系数分别为0.999 8 和0.999 9，氢醌、苯酚检测限分别为0.000 5 和0.001 μg，定量限分别为0.002 和0.003 5μg，精密度试验的RSD 分别为0.4%~1.0% 和0.3%~1.8%，回收率分别为98.4%~99.5% 和100.4%~102.2%。对市售的美白祛斑类化妆品200 批进行测定，在本文的样品处理方法下氢醌和苯酚的检出限分别为1 和2μg·g^-1，定量限分别为4 和7 μg·g^-1，杂质峰和目标峰能够实现基线分离、峰形对称。结论：本法测定美白祛斑类化妆品中氢醌、苯酚含量的专属性好，可以为化妆品检验标准的改进提供参考。

Objective: To improve the chromatographic conditions for the determination of hydroquinone and phenol in whitening cosmetics by HPLC. Methods: Based on the system suitability, the factors including column type,buffer salt and pH of mobile phase on separation were studied. The method developed has been validated,and the cosmetic samples were determined under the optimized conditions. Results: The optimized chromatographic conditions were:C₁₈(4.6 mm×250 mm,5 μm)column was used with the mobile phase of 10 mmol·L^-1 monopotassium phosphate solution(adjusted to pH 3.5 with phosphoric acid)-methanol in a gradient elution programme at a flow rate of 1 mL·min^-1. The column temperature was set at 25℃,the determine wavelength was 280 nm,and injection volume was 5 μL. Under the optimized condition,hydroquinone and phenol got good liner relationship in the ranges of 0.4-40 μg·mL^-1 and 0.7-70 μg·mL^-1 with correlation coefficient of 0.999 8 and 0.999 9. LODs were 0.000 5 μg and 0.001 μg,and LOQs were 0.002 μg and 0.003 5 μg,respectively. The recoveries were 98.4%-99.5% and 100.4%-102.2% with RSDs of 0.4%-1.0% and 0.3%-1.8%,respectively. 200 batches of commercially available whitening cosmetics were analyzed,including astringent,emulsion, cream,and mask,etc. The limits of detection content of hydroquinone and phenol were 1 μg·g^-1 and 2 μg·g^-1, and the limits of quantitation content were 4 μg·g^-1 and 7 μg·g^-1,respectively. The target peak and the interference peak separated well with symmetrical shape. Conclusion: The improved method has good specificity for the determination of hydroquinone and phenol in whitening cosmetics,which can provide a reference for the improvement of cosmetics test.

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