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目的:建立测定化妆品中抗生素含量的高效液相色谱检测方法。方法:样品经甲醇+0.1 mol/L盐酸=1+1的混合溶液提取,用HPLC-DAD进行分析检测,色谱条件为:色谱柱:Waters-AtlantisT3,4.6 mm×150 mm I.D.,粒径5μm;流动相:乙腈+0.02 mol/L磷酸二氢钾(含0.1%甲酸)=15+85;流速:1.0 ml/min;检测波长:218 nm。结果:氨苄西林浓度在25 mg/L～250 mg/L时,美满霉素、土霉素、四环素浓度在50 mg/L～500 mg/L时,工作曲线回归系数为0.999以上,平均回收率为85.6%～109.5%,精密度(RSD)为3.01%～7.74%,氨苄西林检出限为5 mg/L,美满霉素检出限为10 mg/L、土霉素检出限为10 mg/L、四环素检出限为15 mg/L。结论:该方法前处理简单,分离效果好,准确度高,能够满足测定化妆品中氨苄西林、美满霉素、土霉素、四环素的需要。
Objective: To establish a method for the determination of antibiotics in cosmetics by high performance liquid chromatography. Methods: The sample was extracted with methanol +0.1 mol / L hydrochloric acid = 1 + 1 mixed solution and analyzed by HPLC-DAD. The chromatographic conditions were as follows: Column: Waters-AtlantisT3, 4.6 mm × 150 mm ID, 5μm; mobile phase: acetonitrile + 0.02 mol / L potassium dihydrogen phosphate (containing 0.1% formic acid) = 15 + 85; flow rate: 1.0 ml / min; detection wavelength: 218 nm. Results: When ampicillin concentration was between 25 mg / L and 250 mg / L, the regression coefficients of minocycline, oxytetracycline and tetracycline were above 0.999 when the concentration was 50 mg / L to 500 mg / L. The average recoveries (RSD) was 3.01% ~ 7.74%, the limit of detection of ampicillin was 5 mg / L, the limit of detection of minocycline was 10 mg / L. The detection limit of oxytetracycline was 10 mg / L, tetracycline detection limit of 15 mg / L. Conclusion: The method is simple pretreatment, good separation effect and high accuracy, which can meet the need of determination of ampicillin, minocycline, oxytetracycline and tetracycline in cosmetics.