超高效液相色谱-电喷雾串联质谱测定动物源食品中五氯酚的残留量
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摘要
采用固相萃取净化样品,结合液相色谱-三重四极杆串联质谱技术(LC-MS/MS),在负离子扫描模式下,建立了3种动物源食品(鸡肉、鱼肉、虾肉)中五氯酚残留的检测方法。优化的仪器检测条件为:5 mmol/L乙酸铵溶液和甲醇作为流动相,梯度洗脱。选用0. 02 mol/L盐酸-乙腈溶液作为提取溶剂,经WAX固相萃取小柱净化处理后,在0. 001,0. 004和0. 05 mg/kg3个添加水平下,五氯酚在鸡肉、鱼肉和虾肉中的回收率分别为88. 8%～98. 8%,93. 1%～104. 3%和89. 2%～98. 4%,相对标准偏差(RSD)分别为6. 2%～7. 9%,3. 7%～5. 1%和7. 1%～9. 2%。五氯酚在3种样品中的定量限均为0. 001 mg/kg。本方法可用于动物源食品中五氯酚的残留检测。
A rapid and sensitive method based on solid phase extraction using liquid chromatographytandem mass spectrometry( LC-MS/MS) in negative ion scanning was developed for the residue detection of pentachlorophenol in three animal-origin foods( chicken,fish and prawn). When using methanol-5 mmol/L ammonium acetate as the mobile phase,gradient elution resulted in the best chromatographic resolution and sensitivity. When 0. 02 mol/L hydrochloric acid-acetonitrile solution was used as the extraction solvent,the samples were purified by WAX solid phase extraction cartridge,at the spiked levels of 0. 001,0. 004 and 0. 05 mg/kg. The average recoveries of pentachlorophenol were 88. 8%-98. 8%,93. 1%-104. 3% and 89. 2%-98. 4%,with relative standard deviations of6. 2%-7. 9%,3. 7%-5. 1% and 7. 1%-9. 2% in chicken,fish and prawn,respectively. The limit of quantification( LOQ) was 0. 001 mg/kg,which was defined as the lowest spiking level with satisfactory recovery results. This established method was suitable for the residual detecting of pentachlorophenol in animal-origin foods.
A rapid and sensitive method based on solid phase extraction using liquid chromatographytandem mass spectrometry( LC-MS/MS) in negative ion scanning was developed for the residue detection of pentachlorophenol in three animal-origin foods( chicken,fish and prawn). When using methanol-5 mmol/L ammonium acetate as the mobile phase,gradient elution resulted in the best chromatographic resolution and sensitivity. When 0. 02 mol/L hydrochloric acid-acetonitrile solution was used as the extraction solvent,the samples were purified by WAX solid phase extraction cartridge,at the spiked levels of 0. 001,0. 004 and 0. 05 mg/kg. The average recoveries of pentachlorophenol were 88. 8%-98. 8%,93. 1%-104. 3% and 89. 2%-98. 4%,with relative standard deviations of6. 2%-7. 9%,3. 7%-5. 1% and 7. 1%-9. 2% in chicken,fish and prawn,respectively. The limit of quantification( LOQ) was 0. 001 mg/kg,which was defined as the lowest spiking level with satisfactory recovery results. This established method was suitable for the residual detecting of pentachlorophenol in animal-origin foods.
引文
[1] Chen C L,Xiang H R,Dai X Z,et al. Asian J Ecotoxicol.,2015,10(6):71陈春丽,向洪锐,戴星照,等.生态毒理学报,2015,10(6):71
[2] Hang X Y,Feng X Q,Wang Y,et al. Mod Prev Med.,2014,41(5):803杭学宇,冯晓青,汪怡,等.现代预防医学,2014,41(5):803
[3] Mu Y C,Hui Y H,Ma B,et al. Chin Fishery Abstr.,2012,2(2):63穆迎春,惠芸华,马兵,等.中国渔业质量与标准,2012,2(2):63
[4] Zhang Y,Xie P J,Liu F,et al. Shanxi Agric Sci.,2016,44(6):805张渊,谢萍娟,刘芬,等.山西农业科学,2016,44(6):805
[5] Huang J W,Mei Y Q,Liu T J,et al. Chin Health Ind.,2016,13(30):74黄季维,梅玉琴,刘天洁,等.中国卫生产业,2016,13(30):74
[6] Zhao J,Chen L,Tang X Q,et al. Chin J Health Technol.,2016,26(19):2773赵舰,程莉,唐晓琴,等.中国卫生检验杂志,2016,26(19):2773
[7] Claduid M,Dietrich von B,Ariela H,et al. J Sep Sci.,2008,31(6-7):1124
[8] Farhadi K,Farajzadeh M A,Matin A A,et al. Cent Eur J Chem.,2009,7(3):369
[9] Kormosh Z A,Savchuk T I,Bazel Y R. J Water Chem Technol.,2013,35(4):152
[10] Remes A,Pop A,Manea F,et al. Sensors.,2012,12(12):7033
[11] Zhou M,Wu X L,Li C,et al. Phys Testing Chem Anal Part B(Chem Anal),. 2015,51(4):436周敏,吴小玲,李聪,等.理化检验-化学分册,2015,51(4):436
[12] Luo X Q,Han S,Lu Y Q,et al. Anhui Agric Sci.,2016,44(25):55罗晓琴,韩深,吕艳秋,等.安徽农业科学,2016,44(25):55
[13] Yang Q Y,Cheng X Y,Yang P,et al. Chin J Anal Chem,. 2011,39(8):1208杨秋红,程小艳,杨坪,等.分析化学,2011,39(8):1208
[14] Min J Q,Chen M L,Chen X H,et al. J ental Anal.,2015,34(4):438闵剑青,陈梅兰,陈晓红,等.分析测试学报,2015,34(4):438
[15] Blake T A,Zheng X,Aggerholm T,et al. The Analyst.,2002,127(11):1463
[16] Wang Z W,Lin Y,Jin H F,et al. J Agro-environ Sci.,2005,24(6):1249王兆炜,林琦,金海峰,等.农业环境科学学报,2005,24(6):1249
[17] Zhou W Q,Shan J,Guo H Y,et al. J Nanjing Univ:Nat Sci Ed.,2012,48(6):768周文强,单军,郭红岩,等.南京大学学报:自然科学版,2012,48(6):768
[18] Liao L C,Yan Y Y,Lin L,et al. J Sichuan Univ(Med Sci Editi).,2004,35(3):427廖林川,颜有仪,林岚,等.四川大学学报(医学版),2004,35(3):427
[19] GB 23200. 92-2016,National food safety standards—Determination of pentachlorophenol residue in animal-derived foods Liquid chromatography-mass spectrometry GB 23200. 92-2016,动物源性食品中五氯酚残留量的测定液相色谱-质谱法
[20] Ruan Y,Qian W J. Dyeing&Finishing.,2008,34(23):40阮勇,钱微君.印染,2008,34(23):40
[2] Hang X Y,Feng X Q,Wang Y,et al. Mod Prev Med.,2014,41(5):803杭学宇,冯晓青,汪怡,等.现代预防医学,2014,41(5):803
[3] Mu Y C,Hui Y H,Ma B,et al. Chin Fishery Abstr.,2012,2(2):63穆迎春,惠芸华,马兵,等.中国渔业质量与标准,2012,2(2):63
[4] Zhang Y,Xie P J,Liu F,et al. Shanxi Agric Sci.,2016,44(6):805张渊,谢萍娟,刘芬,等.山西农业科学,2016,44(6):805
[5] Huang J W,Mei Y Q,Liu T J,et al. Chin Health Ind.,2016,13(30):74黄季维,梅玉琴,刘天洁,等.中国卫生产业,2016,13(30):74
[6] Zhao J,Chen L,Tang X Q,et al. Chin J Health Technol.,2016,26(19):2773赵舰,程莉,唐晓琴,等.中国卫生检验杂志,2016,26(19):2773
[7] Claduid M,Dietrich von B,Ariela H,et al. J Sep Sci.,2008,31(6-7):1124
[8] Farhadi K,Farajzadeh M A,Matin A A,et al. Cent Eur J Chem.,2009,7(3):369
[9] Kormosh Z A,Savchuk T I,Bazel Y R. J Water Chem Technol.,2013,35(4):152
[10] Remes A,Pop A,Manea F,et al. Sensors.,2012,12(12):7033
[11] Zhou M,Wu X L,Li C,et al. Phys Testing Chem Anal Part B(Chem Anal),. 2015,51(4):436周敏,吴小玲,李聪,等.理化检验-化学分册,2015,51(4):436
[12] Luo X Q,Han S,Lu Y Q,et al. Anhui Agric Sci.,2016,44(25):55罗晓琴,韩深,吕艳秋,等.安徽农业科学,2016,44(25):55
[13] Yang Q Y,Cheng X Y,Yang P,et al. Chin J Anal Chem,. 2011,39(8):1208杨秋红,程小艳,杨坪,等.分析化学,2011,39(8):1208
[14] Min J Q,Chen M L,Chen X H,et al. J ental Anal.,2015,34(4):438闵剑青,陈梅兰,陈晓红,等.分析测试学报,2015,34(4):438
[15] Blake T A,Zheng X,Aggerholm T,et al. The Analyst.,2002,127(11):1463
[16] Wang Z W,Lin Y,Jin H F,et al. J Agro-environ Sci.,2005,24(6):1249王兆炜,林琦,金海峰,等.农业环境科学学报,2005,24(6):1249
[17] Zhou W Q,Shan J,Guo H Y,et al. J Nanjing Univ:Nat Sci Ed.,2012,48(6):768周文强,单军,郭红岩,等.南京大学学报:自然科学版,2012,48(6):768
[18] Liao L C,Yan Y Y,Lin L,et al. J Sichuan Univ(Med Sci Editi).,2004,35(3):427廖林川,颜有仪,林岚,等.四川大学学报(医学版),2004,35(3):427
[19] GB 23200. 92-2016,National food safety standards—Determination of pentachlorophenol residue in animal-derived foods Liquid chromatography-mass spectrometry GB 23200. 92-2016,动物源性食品中五氯酚残留量的测定液相色谱-质谱法
[20] Ruan Y,Qian W J. Dyeing&Finishing.,2008,34(23):40阮勇,钱微君.印染,2008,34(23):40