摘要
目的建立高效液相色谱法测定化妆品中7种抗生素和12种防腐剂。方法采用色谱柱为JADE-PAK HCC18柱(4.6 mm×250 mm,5μm),以甲醇-0.01 mol/L草酸(用磷酸调节p H值为2.0)-乙腈为流动相,梯度洗脱;流速为1.0 ml/min;柱温为35℃;检测波长为268 nm。结果盐酸美满霉素、甲硝唑、二水土霉素、盐酸四环素、盐酸金霉素、氯霉素、盐酸多西环素、甲基氯异噻唑啉酮、2-溴-2-硝基丙烷-1,3-二醇、甲基异噻唑啉酮、苯甲醇、苯氧乙醇、4-羟基苯甲酸甲酯、苯甲酸、4-羟基苯甲酸乙酯、4-羟基苯甲酸丙酯、4-羟基苯甲酸异丙酯、4-羟基苯甲酸丁酯、4-羟基苯甲酸异丁酯呈良好的线性关系(r=0.999 9),低、中、高3个水平的平均回收率为86.1%~110.0%,RSD为1.1%~6.9%;目标成分分离度符合要求。结论方法灵敏度高,准确度和精密度良好,操作简单,可用于同时测定化妆品中的非法添加抗生素和防腐剂成分。
Objective To develop a high performance liquid chromatography( HPLC) method for the determination of 7 antibiotics and 12 preservations in cosmetics simultaneously. Methods The analysis was performed on a JADE-PAK HC-C18column( 4. 6 mm × 250 mm,5 μm) at a flow rate of 1. 0 ml/min. The detection wavelength was 268 nm with the column temperature of 35 ℃. The mobile phase was methanol-0. 01 mol/L oxalic acid( p H = 2. 0,adjusted with phosphoric acid)-acetonitrile. Results Good linearities of the method were obtained for minocycline hydrochloride,metronidazole,metronidazole,oxytetracycline dihydrate,tetracycline hydrochloride,chlortetracycline hydrochloride,doxycycline hydrochloride,chtoramphenicol,methylisothiazolinone,2-bromo-2-nitropropane-1,3-diol,methylchloroisothiazolinone,benzyl alcohol,2-phenoxyethanol,methylparaben,benzoic acid,ethylparaben,isopropyl paraben,propylparaben,isoburyl paraben and butyl-p-hydroxybenzoate,with the correlation coefficients( r) of 0. 999 9. The average recovery rate of each material at low,medium and high levels was within 86. 1%-110. 0%,and relative standard deviations( RSDs) were within 1. 1%-6. 9%. And the separation degree of target components met the requirements. Conclusion The method is simple,accurate,sensitive and can be applied to the determination of 7 antibiotics and 12 preservations in cosmetics simultaneously.
作者
丁怡
张静
DING Yi ZHANG Jing(Guangzhou Institute for Drug Control, Guangzhou , Guangdong 510160, China)
出处
《中国卫生检验杂志》
CAS
2017年第1期18-21,26,共5页
Chinese Journal of Health Laboratory Technology
关键词
高效液相色谱法
抗生素
防腐剂
化妆品
High performance liquid chromatography
Antibiotics
Preservatives
Cosmetics