摘要
目的:建立超高效液相色谱-电喷雾离子化-三重四极杆串联质谱法(UPLC-ESI-MS/MS)同时测定化妆品中的甲基异噻唑啉酮(MIT)和甲基氯异噻唑啉酮(CIT)。方法:样品以甲醇为溶剂,涡旋混匀后超声提取,12000 rpm、4℃离心10 min,上清液再经0.22μm微孔滤膜滤过,滤液经ACQUITY UPLC BEH C18色谱柱(10 cm×2.1 mm,1.7μm)分离后,以正离子、多反应监测(MRM)模式进行定性定量分析。结果:MIT和CIT的线性范围分别为32.0 ng/ml～800 ng/ml和47.6 ng/ml～952 ng/ml,相关系数均大于0.995,回收率均在85%～115%之间,精密度均小于12%。结论:该方法灵敏、专属、准确,可用于化妆品中MIT和CIT的检测。
Objective：To establish a ultra performance liquid chromatography-electrospray ionization tandem mass spectrometric method（UPLC-ESI-MS/MS） for the determination of methylisothiazolinone and chloromethylisothiazolinone in cosmetics.Methods： Cosmetic samples were extracted ultrasonically with methanol and the extracted solution was centrifugated（12000 rpm and 4℃,10 min）.The supernatant was filtered with 0.22 μm filter membrane and the filtrate was separated by ACQUITY UPLC BEH C18 column（10 cm×2.1 mm,1.7 μm）.The analytes were detected by ESI-MS/MS in positive mode.Results： Calibration curves were linear in the range of 32.0 ng/ml^800 ng/ml for methylisothiazolinone and 47.6 ng/ml^952 ng/ml for chloromethylisothiazolinone,both with the correlation coefficient bigger than 0.995.The recoveries were both in the range of 85%~115% with the precision（RSD） both less than 12%.Conclusion： The method is sensitive,specific and accuracy for the quantitative determination of methylisothiazolinone and chloromethylisothiazolinone in cosmetics.
出处
《中国卫生检验杂志》
CAS
2011年第11期2652-2653,2667,共3页
Chinese Journal of Health Laboratory Technology
