摘要
研究并建立了洗涤用品（液类、粉类和皂类）中4种烷基酚（对叔辛基酚、邻正壬基酚、对正辛基酚、对正壬基酚）的液相色谱-串联质谱的检测分析方法。洗涤用品样品以甲醇为提取溶剂,超声提取,过膜,滤液上机测量。采用Waters XBr idge C18色谱柱,以甲醇-0.1%氨水溶液为流动相,梯度洗脱分离后,在LC/MS/MS多反应监测模式下进行定性与定量分析。对叔辛基酚、邻正壬基酚、对正辛基酚和对正壬基酚定量限分别为1、1、0.5和0.5μg/kg,4种烷基酚线性范围均为0.2~100μg/kg;皂类洗涤用品中4种烷基酚在低、中、高3种加标水平的回收率为83.1%~117.4%,相对标准偏差为2.1%~10.3%;液类洗涤用品中4种烷基酚在低、中、高3种加标水平的回收率为82.2%~116.3%,相对标准偏差为1%~8.1%;粉类洗涤用品4种烷基酚中,对叔辛基酚、邻正壬基酚、对正辛基酚3种在低、中、高3种加标水平的回收率为81.8%~114.6%,而对正壬基酚添加回收率仅为44.9%~55.1%,4种烷基酚相对标准偏差为1.4%~7.1%。应用该方法对市面上销售的洗涤产品进行了检测,并对结果进行了分析。
A comprehensive analytical method based on liquid chromatography tandem mass spectrometry has been developed for the determination of alkylphenolsin detergent products,including 4-N-octylphenol,2-octylphenol,2-nonylphenol and 4-N-nonylphenol. Detergentproduct samples were placed in methanol solution and vortexed,ultrasonic extracted. Qualitative and quantitative analyses were carried out for the analytes under the multiple reaction monitoring（ MRM） mode after the chromatographic separation on Waters XBridge C18 column withmethanol： 0. 1% NH4 OH gradient elution. The limits of detection（ LODs） for 2-octylphenol,2-nonylphenol and 4-N-octylphenol,4-N-nonylphenolwere 1,1,0. 5,0. 5 μg / kg. The linear range was 0. 2 ~ 100 μg / kg. The mean recoveries for alkylphenols in soapdetergent products at three spiked levels were in the range of 83. 1% ~ 117. 4%,with the relative standard deviations from 2. 1% ~ 10. 3%; The mean recoveries for alkylphenols in liquid detergent products at three spiked levels were in the range of 82. 2% ~ 116. 3%,with the relative standard deviations from 1% ~ 8. 1%; The mean recoveries for 2-octylphenol,2-nonylphenol and 4-N-octylphenolin powder detergent products at three spiked levels were in the range of 83. 1% ~117. 4%,while the mean recoveries for 4-N-nonylphenol were 44. 9% ~ 55. 1%,both of their relative standard deviations were from2. 1% ~ 10. 3%. The detergentproducts sold on the market were tested by this method,and the results were analyzed.
出处
《化学试剂》
CAS
北大核心
2015年第3期239-242,共4页
Chemical Reagents
基金
国家质检总局公益性行业科研专项资助项目(2012104013-9)
关键词
洗涤用品
液相色谱-串联质谱法
辛基酚
壬基酚
soap
liquid chromatography tandem massspectrometry
octylphenols
nonylphenols
