化妆品中盐酸美满霉素含量测定方法的改进

Improvement of method for determination of minocycline hydrochloride in cosmetics

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 legal HPLC analytical method of ＂Hygienic Standard for Cosmetics＂（2007） and improve the accuracy of qualitative and quantitative determination of minocycline hydrochloride in cosmetis.Methods RP-High-pressure liquid chromatography was performed on a C8column with mobile phase of 0.1 mol/L ammonium oxalate-N,N-dimethylformamide-0.1 mol/L disodium ethylenediaminetetraacetate（55∶ 25∶ 20）.The detection wavelength was 280 nm.The flow rate was 1.7 ml/min.The column temperature was 35 ℃.Results Good linearity between peak area and concentration was found in the range of 0.5 μg/ml^1000 μg/ml for minocycline hydrochloride.The correlative coefficient was 0.9999（n =8）.The recoveries were between 98.7%~104.5%.The detection limit was 5 ng.Conclusion The method has high sensitivity and strong specialization,and can accurately determine the minocycline hydrochloride in cosmetis,so it can be used as the supplementary detection method for illegal additives of antibiotics in＂Hygienic Standard for Cosmetics＂（2007）.