【摘要】 建立了化妆品中四环素、土霉素、金霉素、强力霉素、甲烯土霉素、去甲基金霉素、二甲胺四环素、脱水四环素和差相四环素含量的液相色谱串联质谱测定方法。对提取溶剂、流动相、流动相的梯度以及质谱参数进行了研究。采用乙腈-甲醇-草酸水溶液提取,LC-MS/MS分离测定,样品中被测物与干扰物能得到良好的分离。甲烯土霉素、去甲基金霉素在0.05~10.0 mg/L范围内其质量浓度与峰面积均呈良好的线性关系,其余7种化合物在0.01~10.0 mg/L范围内其质量浓度与峰面积呈良好的线性关系。添加1.0~50.0 mg/kg时的加标回收率为73%~99%,相对标准偏差低于13.2%。该法简便、快速、准确,可用于化妆品中上述9种四环素类药物的定性、定量检测。更多还原

【Abstract】 A high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS) method was established for the determination of 9 tetracyclines including tetracycline,oxytetracycline,chlorotetracycline,doxycycline,metacycline,demeclocycline,minocycline,anhydrotetracycline,4-epitetracycline in cosmetics.The effects of different extraction reagent,flow phase,gradient and tandem mass spectrometry parameters were investigated.The sample was extracted with methanol-acetonitrile-oxalic acid solution.The separation of analytes was performed on a C18 column with a gradient elution using water,methanol,acetonitrile and 0.5% formic acid solution as mobile phase.The external standard calibration curve was used for quantification.There were good linear relationship between peak areas and concentrations in the range of 0.05-10.0 mg/L for metacycline and demeclocycline,and 0.01-10.0 mg/L for rest of analytes.The correlation coefficients were more than 0.999.The spiked recoveries were 73%-99% with relative standard deviations(RSDs) less than 13.2%.This method was simple,fast,accurate and convenient and could be used as one of the reliable means for quantitative determination of tetracyclines in cosmetics.更多还原