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目的建立用高效液相色谱-二极管阵列检测法(HPLC-PDA)检测祛痘除螨类化妆品中非法添加的盐酸米诺环素,以打击化妆品中非法添加禁限物质的不法行为。方法采用Waters Symmetry C18(5μm,4.6 mm×250 mm)色谱柱;以醋酸铵缓冲盐溶液(取醋酸铵15 g、氯化钾10 g与乙二胺四乙酸二钠5 g,加水溶解并稀释成1 000 ml)-乙腈(70∶30)为流动相等度洗脱;流速为1.0 ml/min;柱温为25℃;检测波长280 nm;用PDA检测,以保留时间和紫外光谱图定性,峰面积定量。结果盐酸米诺环素在1~100μg/ml范围内与峰面积呈良好的线性关系,相关系数为1.000 0,检出限为0.1μg/ml,方法的回收率为88.5%~98.5%,RSD为1.0%~1.5%(n=6)。结论该方法特异性强,灵敏度高,准确可靠,适用于不同基质样品中盐酸米诺环素的检测。
OBJECTIVE To establish HPLC-PDA for the detection of minocycline hydrochloride illegally added in acne and acne cosmetics to combat the unlawful act of illegally adding banned substances in cosmetics. Methods A Waters Symmetry C18 column (5 μm, 4.6 mm × 250 mm) was used. Ammonium acetate buffer solution (15 g of ammonium acetate, 10 g of potassium chloride and 5 g of disodium ethylenediaminetetraacetate) was dissolved in water and diluted (1 000 ml) -acetonitrile (70:30) was used as the eluent of mobile phase. The flow rate was 1.0 ml / min. The column temperature was 25 ℃. The detection wavelength was 280 nm. Peak area quantitative. Results The minocycline hydrochloride showed a good linear relationship with the peak area in the range of 1 ~ 100μg / ml with a correlation coefficient of 1.000 0 and a detection limit of 0.1μg / ml. The recoveries of the method were 88.5% ~ 98.5% Was 1.0% to 1.5% (n = 6). Conclusion The method is specific, sensitive, accurate and reliable and is suitable for the determination of minocycline hydrochloride in different matrix samples.