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目的对《化妆品卫生规范》(2007年版)的法定HPLC法进行改进,提高定性定量测定化妆品中盐酸美满霉素的准确性。方法采用C8色谱柱,以0.1 mol/L草酸铵溶液-二甲基甲酰胺-0.1 mol/L乙二胺四乙酸二钠溶液(55∶25∶20)(pH 6.5)为流动相,检测波长为280 nm,流速为1.7 ml/min,柱温35℃。结果方法检出限为5 ng,盐酸美满霉素在0.5μg/ml~1000μg/ml浓度范围内线性关系良好,相关系数r=0.9999,回收率为98.7%~104.5%。结论该方法灵敏度高,专属性强,能准确测定化妆品中的盐酸美满霉素,可作为《化妆品卫生规范》(2007年版)抗生素类非法添加物质检测方法的补充。
Objective To improve the statutory HPLC method of Cosmetic Hygienic Practice (2007 Edition) to improve the accuracy of qualitative and quantitative determination of cosmetic minocycline hydrochloride. Methods A C8 column was used. The mobile phase was 0.1 mol / L ammonium oxalate solution - dimethylformamide - 0.1 mol / L disodium ethylenediaminetetraacetate solution (pH = 6.5) 280 nm, flow rate of 1.7 ml / min, column temperature 35 ℃. Results The detection limit was 5 ng. The calibration curve of minocycline hydrochloride was good in the range of 0.5 μg / ml to 1000 μg / ml. The correlation coefficient was 0.9999. The recoveries ranged from 98.7% to 104.5%. Conclusion The method is sensitive, specific and accurate and can accurately determine the content of minocycline hydrochloride in cosmetic products. It can be used as a supplement to the method of testing the illegal addition of antibiotics in Cosmetic Hygienic Practice (2007 Edition).