Liu Hualiang, Li Fang, Yang Run, Wang Lianhong, Ma Yongji
Jiangsu Provincial Center for Disease Control and Prevention, Nanjing 210009, China.
Se Pu. 2009 Jan;27(1):50-3.
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 concentration. 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 - 1 000 microg/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.
建立了一种采用超高效液相色谱-串联质谱法(UPLC-MS/MS)分析化妆品中常见抗生素和甲硝唑的方法。称取1克各化妆品样品,用含0.1 mol/L甲酸的甲醇-水(1:1,v/v)进行萃取。萃取后的样品在进行UPLC/MS/MS分析前需过滤。研究了流动相中甲酸浓度对灵敏度和保留时间的影响,结果表明1%为最佳浓度。7种分析物,即米诺环素、土霉素、四环素、金霉素、强力霉素、氯霉素、甲硝唑,可在5分钟内分离并检测出来,比传统液相色谱法快得多。检测限为3 - 20 ng/g,回收率为87% - 101%。校准曲线在2 - 1000 μg/L范围内呈良好线性,相关系数大于0.995。该方法还应用于测定市售的11个实际样品中的常见抗生素和甲硝唑。在2个样品中检测到氯霉素,浓度分别为0.37%和0.19%;在1个样品中检测到甲硝唑,浓度为1.02%;其他未检测到。