摘要
建立了超高效液相色谱-串联质谱（UPLC—MS／MS）测定化妆品中常见的6种抗生素（美满霉素、土霉素、四环素、金霉素、多西环素、氯霉素）及甲硝唑的方法，并用于实际样品的分析。样品经甲醇-0．1mol／L甲酸溶液（体积比为1：1）超声提取后，以甲醇（含1％甲酸）-水（含1％甲酸）为流动相，经UPLC梯度洗脱分离后以多反应监测（MRM）模式质谱测定。方法的检出限为3～20ng／g，回收率为87％～101％，工作曲线的线性相关系数大于0．995，线性范围为2～1000μg／L（达3个数量级）。对11份市售化妆品进行分析检测，其中2份检出氯霉素，质量分数分别为0．37％和0．19％；1份检出甲硝唑，质量分数为1．02％；美满霉素、土霉素、四环素、金霉素、多西环素未检出。
A method for the analysis of common antibiotics and metronidazole in cosmetics was developed by ultra performance liquid chromatography-tandem mass spectrometry （ UPLC-MS/ MS）. One gram of each cosmetic sample was extracted by methanol-water containing 0. 1 mol/L formic acid （ 1 ： 1, v/v）. The extracted sample was filtered before being analyzed with UPLC/MS/MS. The effects of formic acid concentration in the mobile phase on the sensitivity and retention time were studied, and the results showed that 1% was the optimum concentra- tion. Seven analytes, minocycline, oxytetracycline, tetracycline, chlortetracycline, doxycycline, chloramphenicol, metronidazole, can be separated and detected in 5 min, which is much faster than that by the conventional liquid chromatography. The detection limits were 3 -20 ng/g, and the recoveries were 87% - 101%. The calibration curves showed good linearity in the range of 2 - 1 000μg/L with correlation coefficients larger than 0. 995. The method was also applied to determine common antibiotics and metronidazole in 11 real samples from the market. Chloramphenicol was detected in 2 samples and the concentrations were 0.37% and 0. 19%; metronidazole was detected in 1 sample and the concentration was 1.02%; others were not detected.
出处
《色谱》
CAS
CSCD
北大核心
2009年第1期50-53,共4页
Chinese Journal of Chromatography
基金
国家科技支撑计划项目(No.2006BAK02A01)
关键词
超高效液相色谱-串联质谱法
抗生素
甲硝唑
化妆品
ultra performance liquid chromatography-tandem mass spectrometry （ UPLC-MS/ MS）
antibiotics
metronidazole
cosmetics
