液相色谱-质谱法同时测定纺织品中19种含氯苯酚类化合物
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摘要
建立了同时测定纺织品中19种含氯苯酚类化合物的液相色谱-质谱(LC-MS)法。采用甲醇为溶剂,超声辅助萃取纺织品中的含氯苯酚类化合物,经蒸发浓缩和定容后,LC-MS测定,外标法定量。结果表明,19种含氯苯酚类化合物在0. 05～5. 0 mg/L范围内线性关系良好(r> 0. 999 90),平均回收率为80. 3%～104%,相对标准偏差(n=6)为4. 0%～9. 8%。方法的定量下限为0. 05 mg/kg。方法灵敏、简便、高效、准确,可满足纺织品中含氯苯酚类化合物的检测需求。
A method was developed for the simultaneous determination of 19 chlorinated phenols in textiles by liquid chromatography-mass spectrometry( LC-MS). The textile samples were extracted with methanol in ultrasonic bath,then evaporated and set to volume. The target compounds were analyzed by LC-MS and quantified by the external method. The calibration curves for 19 chlorinated phenols were linear( r > 0. 999 90) in the concentration range of 0. 05-5. 0 mg/L. The average recoveries were in the range of 80. 3%-104% with their relative standard deviations( RSD,n = 6) of 4. 0%-9. 8%. The quantitation limits were 0. 05 mg/kg. The method was sensitive,simple,efficient and accurate,and could meet the requirements for detection of chlorinated phenols in textile products.
A method was developed for the simultaneous determination of 19 chlorinated phenols in textiles by liquid chromatography-mass spectrometry( LC-MS). The textile samples were extracted with methanol in ultrasonic bath,then evaporated and set to volume. The target compounds were analyzed by LC-MS and quantified by the external method. The calibration curves for 19 chlorinated phenols were linear( r > 0. 999 90) in the concentration range of 0. 05-5. 0 mg/L. The average recoveries were in the range of 80. 3%-104% with their relative standard deviations( RSD,n = 6) of 4. 0%-9. 8%. The quantitation limits were 0. 05 mg/kg. The method was sensitive,simple,efficient and accurate,and could meet the requirements for detection of chlorinated phenols in textile products.
引文
[1]Fan Y M,He X Y,Yu X J,Gu X J,Chen S B,Zhan J.J.Instrum.Anal.(樊苑牧,贺小雨,俞雪钧,顾晓俊,陈树兵,湛嘉.分析测试学报),2009,28(7):794-798.
[2]The International Association for Research and Testing in the Field of Textile Ecology(OEKO-TEX).OEKO-TEXStandard 100(国际生态纺织品标签).https://www.oeko-tex.com/en/splashpage/index.xhtml.
[3]GB/T 18414.1-2006.Textiles-Determination of the Content of Chlorinated Phenols-Part 1:Gas ChromatographyMass Spectrography.National Standards of the Peoples Republic of China(纺织品含氯苯酚的测定第1部分:气相色谱-质谱法.中华人民共和国国家标准).
[4]GB/T 18414.2-2006.Textiles-Determinaeion of the Content of Chlorinated Chenols-Part 2:Gas Chromatography.National Standards of the Peoples Republic of China(纺织品含氯苯酚的测定第2部分:气相色谱法.中华人民共和国国家标准).
[5]Gao Y G,Niu Z Y,Zhang Y Y,Ye X W,Bao Y,Cai F,Wang X,Su J,Qu J W.Chin.J.Chromatogr.(高永刚,牛增元,张艳艳,叶曦雯,包艳,蔡发,王新,苏杰,曲京武.色谱),2016,34(9):906-911.
[6]Li L,Xue X L,Lian X B.Chin.J.Anal.Chem.(李琳,薛秀玲,连小彬.分析化学),2010,38(10):1469-1473.
[7]Wang C Y,Wu T M,Pan X Y,Lin J F,Jiang F,Xie T T.Melliand China(王成云,吴透明,潘晓远,林君峰,江帆,谢堂堂.国际纺织导报),2017,(6):36-42.
[2]The International Association for Research and Testing in the Field of Textile Ecology(OEKO-TEX).OEKO-TEXStandard 100(国际生态纺织品标签).https://www.oeko-tex.com/en/splashpage/index.xhtml.
[3]GB/T 18414.1-2006.Textiles-Determination of the Content of Chlorinated Phenols-Part 1:Gas ChromatographyMass Spectrography.National Standards of the Peoples Republic of China(纺织品含氯苯酚的测定第1部分:气相色谱-质谱法.中华人民共和国国家标准).
[4]GB/T 18414.2-2006.Textiles-Determinaeion of the Content of Chlorinated Chenols-Part 2:Gas Chromatography.National Standards of the Peoples Republic of China(纺织品含氯苯酚的测定第2部分:气相色谱法.中华人民共和国国家标准).
[5]Gao Y G,Niu Z Y,Zhang Y Y,Ye X W,Bao Y,Cai F,Wang X,Su J,Qu J W.Chin.J.Chromatogr.(高永刚,牛增元,张艳艳,叶曦雯,包艳,蔡发,王新,苏杰,曲京武.色谱),2016,34(9):906-911.
[6]Li L,Xue X L,Lian X B.Chin.J.Anal.Chem.(李琳,薛秀玲,连小彬.分析化学),2010,38(10):1469-1473.
[7]Wang C Y,Wu T M,Pan X Y,Lin J F,Jiang F,Xie T T.Melliand China(王成云,吴透明,潘晓远,林君峰,江帆,谢堂堂.国际纺织导报),2017,(6):36-42.