目的: 建立二维柱切换高效液相色谱法测定化妆品中氢醌、苯酚的分析方法。方法: 二维色谱柱均为C18色谱柱(250 mm×4.6 mm,5 μm),捕获柱为2条串联的C16色谱柱(20 mm×4.0 mm,5 μm),10 mmol·L-1磷酸二氢钾溶液(用磷酸调节pH3.5)-甲醇为流动相,梯度洗脱,流速1.0 mL·min-1,柱温35 ℃,检测波长280 nm,进样量2 μL。结果: 氢醌和苯酚线性范围分别为5.570~111.5 μg·mL-1 (r=0.999 7)和5.410~108.1 μg·mL-1(r =0.999 6),方法提取回收率分别为91.9%~92.6%和94.4%~94.7%,精密度试验的RSD分别为3.9%~4.1%和0.9%~2.1%,检测下限分别为0.70 μg·g-1和0.69 μg·g-1。市场随机抽取40批美白类化妆品样品(包含乳剂、霜剂、水剂等)均单次进样即可快速完成样品分析,无基质干扰。结论: 本法测定美白类化妆品中氢醌、苯酚含量的专属性好,方法快速、准确,可用于复杂基质的美白类化妆品中氢醌、苯酚的测定。
Objective: To establish a method to determine hydroquinone and phenol in whitening cosmetics by switching column two-dimensional HPLC. Methods: Two C18 columns(250 mm×4.6 mm, 5 μm)and two C16 trapping columns (20 mm×4.0 mm, 5 μm)were 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 program at a flow rate of 1 mL·min-1. The column temperature was set at 35 ℃, the determine wavelength was 280 nm, and injection volume was 2 μL. Results: Hydroquinone and phenol showed good linear relationship in the ranges of 5.570-111.5 μg·mL-1 (r=0.999 7)and 5.410-108.1 μg·mL-1(r=0.999 6). The recoveries were 91.9%-92.6% and 94.4%-94.7% with RSDs of 3.9%-4.1% and 0.9%-2.1%, respectively. Forty batches of commercially available whitening cosmetics(including emulsion, cream, astringent, etc) were analyzed by single measurement without matrix interference. Conclusion: The method has good specificity for the determination of hydroquinone and phenol in whitening cosmetics, which can determine hydroquinone and phenol in whitening cosmetics with complex matrix rapidly and accurately.
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