两亲性聚离子液体膜微萃取-液相色谱-串联质谱法测定水中5种氯酚
LC-MS/MS Determination of 5 Chlorophenols in Water with Microextraction of Amphiphilic Polymeric Ionic Liquid Membrane
摘 要
采用两亲性聚离子液体膜微萃取-液相色谱-串联质谱法测定水中5种氯酚的含量。以Shim-pack XR-ODS Ⅱ色谱柱为分离柱，以不同体积比的0.005 mol·L-1乙酸铵溶液和甲醇-乙腈（1+4）溶液的混合液为流动相进行梯度洗脱，采用电喷雾负离子源多反应监测模式检测。方法的检出限（3S/N）为0.33~5.4 ng·L-1。加标回收率为86.4%~99.1%，测定值的日内相对标准偏差（n=6）为0.80%~8.2%，日间相对标准偏差（n=6）为1.7%~8.7%。
两亲性聚离子液体膜
微萃取
水
氯酚
LC-MS/MS
amphiphilic polymeric ionic liquid membrane
microextraction
water
chlorophenol
Abstract
LC-MS/MS was applied to the determination of 5 chlorophenols in water with microextraction of amphiphilic polymeric ionic liquid membrane. Shim-pack XR-ODS Ⅱ chromatographic column was used as stationary phase, and the mixture of 0.005 mol·L-1 ammonium acetate solution and methanol-acetonitrile (1+4) solution mixed in different ratios was used as mobile phase in gradient elution. ESI- and multi-reactions monitor mode were adopted in MS/MS. Detection limits (3S/N) of the method were in the range of 0.33-5.4 ng·L-1. Values of recovery found by standard addition method were in the range of 86.4%-99.1%, with intra-day RSD's (n=6) in the range of 0.80%-8.2% and inter-day RSD's (n=6) in the range of 1.7%-8.7%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201711007
所属栏目 工作简报
基金项目 浙江省自然科学基金（LY14B070004，LY16B050001）
收稿日期 2017/4/12
修改稿日期
网络出版日期
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联系人作者金米聪(jmcjc@163.com)
备注陈晓红(1967-),女,浙江宁波人,主任技师,研究方向为色质谱联用检测新技术新方法
引用该论文: CHEN Xiaohong,MIN Jianqing,WANG Qian,CAI Meiqiang,JIN Micong. LC-MS/MS Determination of 5 Chlorophenols in Water with Microextraction of Amphiphilic Polymeric Ionic Liquid Membrane[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(11): 1276～1280
陈晓红,闵剑青,王倩,蔡美强,金米聪. 两亲性聚离子液体膜微萃取-液相色谱-串联质谱法测定水中5种氯酚[J]. 理化检验－化学分册, 2017, 53(11): 1276～1280
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参考文献
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【2】WANG K D, CHEN P S, HUANG S D. Simultaneous derivatization and extraction of chlorophenols in water samples with up-and-down shaker-assisted dispersive liquid-liquid microextraction coupled with gas chromatography/mass spectrometric detection[J]. Anal Bioanal Chem, 2014,406(8):2123-2131.
【3】高学杰,张毅,孙仕萍.毛细管气相色谱法测定水中2,4,6-三氯酚和五氯酚[J].中国卫生检验杂志, 2011,21(5):1098-1099.
【4】周瑞娟,段炼,孙晓杰,等.离子液体键合固相微萃取涂层用于水样中五氯酚的测定[J].高等学校化学学报, 2010,31(10):1945-1948.
【5】周颖,吴显芳,屈卫东,等.水中五氯酚测定方法的研究[J].卫生研究, 2007,36(3):287-288.
【6】胡庆兰.离子液体固相微萃取涂层分析人体尿液中的五氯酚[J].应用化学, 2013,30(3):323-328.
【7】沈登辉,章清荷,王冰霜,等.饮用水中五氯酚的固相萃取-气相色谱串联质谱测定法[J].环境与健康杂志, 2014,31(1):51-53.
【8】邱纪时,钟惠英,祝翔宇,等.杭州湾南岸海水中的氯酚类化合物的污染特征及生态风险评价[J].海洋环境科学, 2016,35(2):231-237.
【9】杨秋红,程小艳,杨坪.固相萃取-高效液相色谱串联质谱法同时检测地表水中的2,4-二氯酚、2,4,6-三氯酚和五氯酚[J].分析化学, 2011,39(8):1208-1212.
【10】闵剑青,陈梅兰,陈晓红,等.离子液体超声辅助萃取-LC/MS法测定环境水中痕量五氯酚[J].分析测试学报, 2015,34(4):438-442.
【11】金米聪,陈晓红,李小平,等.高效液相色谱-电喷雾电离质谱联用法测定水中痕量五氯酚研究[J].中国卫生检验杂志, 2005,15(3):280-281.
【12】周丽新,陈晓红,金米聪.氯酚的分析技术研究进展[J].卫生研究, 2014,43(4):685-692.
【13】YANG F, SHEN R, LONG Y M, et al. Magnetic microsphere confined ionic liquid as a novel sorbent for the determination of chlorophenols in environmental water samples by liquid chromatography[J]. J Environ Monit, 2011,13(2):440-445.
【14】PENG J F, LIU J F, HU X L, et al. Direct determination of chlorophenols in environmental water samples by hollow fiber supported ionic liquid membrane extraction coupled with high-performance[J]. J Chromatogr A, 2007,1139(2):165-170.
【15】范洪富,王达,马军,等.用离子液体[bmim]PF6和[emim]Beti萃取水中的氯酚[J].大庆石油学院学报, 2007,31(6):68-73.
【16】CAI M Q, WEI X Q, DU C H, et al. Novel amphiphilic polymeric ionic liquid-solid phase micro-extraction membrane for the preconcentration of aniline as degradation product of azo dye Orange G under sonication by liquid chromatography-tandem mass spectrometry[J]. J Chromatogr A, 2014,1349:24-29.
【2】WANG K D, CHEN P S, HUANG S D. Simultaneous derivatization and extraction of chlorophenols in water samples with up-and-down shaker-assisted dispersive liquid-liquid microextraction coupled with gas chromatography/mass spectrometric detection[J]. Anal Bioanal Chem, 2014,406(8):2123-2131.
【3】高学杰,张毅,孙仕萍.毛细管气相色谱法测定水中2,4,6-三氯酚和五氯酚[J].中国卫生检验杂志, 2011,21(5):1098-1099.
【4】周瑞娟,段炼,孙晓杰,等.离子液体键合固相微萃取涂层用于水样中五氯酚的测定[J].高等学校化学学报, 2010,31(10):1945-1948.
【5】周颖,吴显芳,屈卫东,等.水中五氯酚测定方法的研究[J].卫生研究, 2007,36(3):287-288.
【6】胡庆兰.离子液体固相微萃取涂层分析人体尿液中的五氯酚[J].应用化学, 2013,30(3):323-328.
【7】沈登辉,章清荷,王冰霜,等.饮用水中五氯酚的固相萃取-气相色谱串联质谱测定法[J].环境与健康杂志, 2014,31(1):51-53.
【8】邱纪时,钟惠英,祝翔宇,等.杭州湾南岸海水中的氯酚类化合物的污染特征及生态风险评价[J].海洋环境科学, 2016,35(2):231-237.
【9】杨秋红,程小艳,杨坪.固相萃取-高效液相色谱串联质谱法同时检测地表水中的2,4-二氯酚、2,4,6-三氯酚和五氯酚[J].分析化学, 2011,39(8):1208-1212.
【10】闵剑青,陈梅兰,陈晓红,等.离子液体超声辅助萃取-LC/MS法测定环境水中痕量五氯酚[J].分析测试学报, 2015,34(4):438-442.
【11】金米聪,陈晓红,李小平,等.高效液相色谱-电喷雾电离质谱联用法测定水中痕量五氯酚研究[J].中国卫生检验杂志, 2005,15(3):280-281.
【12】周丽新,陈晓红,金米聪.氯酚的分析技术研究进展[J].卫生研究, 2014,43(4):685-692.
【13】YANG F, SHEN R, LONG Y M, et al. Magnetic microsphere confined ionic liquid as a novel sorbent for the determination of chlorophenols in environmental water samples by liquid chromatography[J]. J Environ Monit, 2011,13(2):440-445.
【14】PENG J F, LIU J F, HU X L, et al. Direct determination of chlorophenols in environmental water samples by hollow fiber supported ionic liquid membrane extraction coupled with high-performance[J]. J Chromatogr A, 2007,1139(2):165-170.
【15】范洪富,王达,马军,等.用离子液体[bmim]PF6和[emim]Beti萃取水中的氯酚[J].大庆石油学院学报, 2007,31(6):68-73.
【16】CAI M Q, WEI X Q, DU C H, et al. Novel amphiphilic polymeric ionic liquid-solid phase micro-extraction membrane for the preconcentration of aniline as degradation product of azo dye Orange G under sonication by liquid chromatography-tandem mass spectrometry[J]. J Chromatogr A, 2014,1349:24-29.
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