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作 者:刘湘军[1,2] 赵妍 赵珊 杨奕 张晶 邱细敏[1] 邵兵
机构地区:[1]湖南师范大学医学院,湖南长沙410006 [2]北京市预防医学研究中心,北京100013 [3]南京市产品质量监督检验院,江苏南京210028
出 处:《分析测试学报》2013年第1期64-68,共5页Journal of Instrumental Analysis
基 金:国家自然科学基金项目(21177014);北京市卫生系统高层次卫生技术人才培养计划项目;湖南省教育厅重点项目(10A071)
摘 要:采用超高效液相色谱-串联质谱技术(UPLC-MS/MS)建立了牙膏、洗手液、消毒液、洗发露、香皂等日化产品中三氯生与三氯卡班的同时分析方法。试样中的待测物经过有机溶剂超声提取,上清液稀释后,经ACQUITY UPLC HSS T3色谱柱分离,电喷雾负离子多反应检测模式(MRM)测定,外标法定量。在优化实验条件下,三氯生与三氯卡班分别在1~250、0.2~50μg/L范围内呈良好线性(r2>0.995),方法定量下限(LOQ)分别为0.2~0.7、0.01~0.02 mg/kg。3个加标水平下,三氯生与三氯卡班在5种日化产品中的加标回收率为86%~116%,相对标准偏差(RSD)均不大于15%。该方法适用于日化产品中三氯生与三氯卡班的同时测定。An ultra performance liquid chromatography- tandem mass spectrometric (UPLC -MS/ MS) method was developed for the simultaneous determination of triclosan and triclocarban in daily chemical products, including toothpaste, hand sanitizer, disinfectant, shampoo and soap. The samples were ultrasonically extracted with organic solvents and centrifugated. The analytes were sepa- rated on an ACQUITY UPLC HSS T3 column, and identified under negative electrospray ionization (ESI - ) and multiple reaction monitoring(MRM) mode. The standard calibration curves were used for the quantitative analysis. Good linearities were achieved for triclosan and triclocarban over the ranges of 1 - 250 I^g/L and 0. 2 - 50 Ixg/L, respectively, with correlation coefficients ( r2 ) more than 0. 995. The quantitation limits of the method were in the ranges of 0. 2 - 0. 7 mg/kg for triclosan and 0.01 -0. 02 mg/kg for triclocarban. Mean recoveries of the two target compounds in five kinds of daily chemical products at three spiked concentration levels ranged from 86% to 116% with relative standard deviations(RSDs) no more than 15%. This method could be applied in the simultaneous determination of triclosan and triclocarban in daily chemical products.
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