不同前处理对动物组织中氯丙嗪残留检测对比
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摘要
采用超高效液相色谱串联质谱技术,比较QuECHERS法、MCX固相萃取法和叔丁基甲醚直接提取法3种前处理方法对猪肉、猪肝、鸡肉、鱼肉中氯丙嗪残留检测效果的影响。结果表明:3种方法对氯丙嗪的检出限为0.2μg/kg,定量限为0.5μg/kg。在不同加标水平下,QuECHERS法、MCX固相萃取法和叔丁基甲醚直接提取法处理的各类基质中加标回收率(72.5%～108.8%)和相对标准偏差(2.1%～8.6%)均满足方法学要求。MCX固相萃取法净化效果优于QuECHERS法、叔丁基甲醚直接提取法。整体回收率从高到低依次是MCX固相萃取法>QuECHERS法>叔丁基甲醚直接提取法。对于脂肪含量较高的猪肉,3种前处理方法回收率均略低于其他3种基质。
Ultra performance liquid chromatography tandem mass spectrum/mass spectrum(UPLC-MS/MS)was used to detect chlorpromazine residues in porcine muscle, liver, chicken and fish. Three sample preparation methods including QuECHERS, MCX solid-phase extraction and direct extraction by tert-butyl methyl ether were compared. The results showed that the limit of detection(LOD) of chlorpromazine by three methods was 0.2 μg/kg, and the limit of quantitation(LOQ) was 0.5 μg/kg. At different addition levels,the recovery and relative standard deviation(RSD) by three sample preparation methods were 72.5%～108.8% and 2.1%～8.6%, respectively. All met the methodological requirements. The purifying effect of MCX solid-phase extraction was better than the other sample preparation methods. The order of overall recovery was from high to low: MCX solid-phase extraction, QuECHERS, and direct extraction by tertbutyl methyl ether. The recoveries for pork with high fat content by three preparation methods were lower than those of liver, chicken and fish.
Ultra performance liquid chromatography tandem mass spectrum/mass spectrum(UPLC-MS/MS)was used to detect chlorpromazine residues in porcine muscle, liver, chicken and fish. Three sample preparation methods including QuECHERS, MCX solid-phase extraction and direct extraction by tert-butyl methyl ether were compared. The results showed that the limit of detection(LOD) of chlorpromazine by three methods was 0.2 μg/kg, and the limit of quantitation(LOQ) was 0.5 μg/kg. At different addition levels,the recovery and relative standard deviation(RSD) by three sample preparation methods were 72.5%～108.8% and 2.1%～8.6%, respectively. All met the methodological requirements. The purifying effect of MCX solid-phase extraction was better than the other sample preparation methods. The order of overall recovery was from high to low: MCX solid-phase extraction, QuECHERS, and direct extraction by tertbutyl methyl ether. The recoveries for pork with high fat content by three preparation methods were lower than those of liver, chicken and fish.
引文
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[5]Pang N,Wang T L,Hu J.Method validation and dissipation kinetics of four herbicides in maize and soil using QuEChERS sample preparation and liquid chromatography tandem mass spectrometry[J].Food Chemistry,2016,190:793-800.
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[11]Cao Jie(曹洁),Jia Juan(贾娟),Wang Yujin(王玉瑾),et al.Determination of chlorpromazine in blood samples by hollow fiber-liquid phase micro-extraction coupled with gas chromatography[J].Chinese Journal of Health Laboratory Technology(中国卫生检验杂志),2013,23(15):3015-3017.
[12]Hong Yueling(洪月玲),Hao Xuefei(郝学飞),Dong Ke(董柯).HPLC determination of chlorpromazine residue in animal-derived foods[J].Food Science(食品科学),2009,30(14):269-271.
[13]Zhang L,Wu P,Zhang Y,et al.A GC/MS method for the simultaneous determination and quantification of chlorpromazine and diazepam in pork samples[J].Analytical Methods,2014,6(2):503-508.
[14]Gu Huabing(顾华兵),Xie Jie(谢洁),Peng Tao(彭涛),et al.Determination of chlorpromazine residues in chicken muscle tissues by high performance liquid chromatography-tandem mass spectrometry[J].China Poultry(中国家禽),2014,36(15):33-36.
[15]Liu Yan(刘燕),Su Ying(苏英),Lan Ruirong(兰瑞容),et al.Determination of antipsychotic drugs chlorpromazine and haloperidol in pork by HPLC-MS/MS[J].Chinese Journal of Pharmaceutical Analysis(药物分析杂志),2015,35(4):685-688.
[16]Dasenaki M E,Thomaidis N S.Multi-residue determination of 115veterinary drugs and pharmaceutical residues in milk powder,butter,fish tissue and eggs using liquid chromatography-tandem mass spectrometry[J].Analytica Chimica Acta,2015,880:103-121.
[17]Wang Jie(王杰),Pei Fei(裴斐),Li Peng(李彭),et al.Comparison of different sample pretreatments for the analysis of quinolone residues in porcine tissues[J].Food Science(食品科学),2018,39(18):309-314.
[18]Qin ling(覃玲),Dong Yalei(董亚蕾),Wang Gangli(王钢力),et al.Determination of 42 veterinary drug residues in common animal derived food by dispersive solid phase extraction coupled with liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Chromatography(色谱),2018,36(9):880-888.
[19]Pi?tkowska M,Gbylik-Sikorska M,Gajda A,et al.Multiresidue determination of veterinary medicines in lyophilized egg albumen with subsequent consumer exposure evaluation[J].Food Chemistry,2017,229:646-652.
[20]Shao Linzhi(邵琳智),Xie Minling(谢敏玲),Lin Feng(林峰).Determination of chloramphenicol in propolis by high performance liquid chromatography-tandem mass spectrometry[J].Journal of Instrumental Analysis(分析测试学报),2017,36(8):1029-1032.
[21]Li Rong(李蓉),Yang Luqi(杨璐齐),Zhang Pengyun(张鹏云),et al.Rapid screening of 24 tranquillizer drugs in fish and fishery products by ultra-high performance liquid chromatographyquadrupole/electrostatic field orbitrap high resolution mass spectroscopy[J].Chinese Journal of Chromatography(色谱),2018,36(2):125-135.
[22]Zhang Y,Zhang J,Liu X,et al.Rapid screening and quantification of multi-class multi-residue veterinary drugs in royal jelly by ultra performance liquid chromatography coupled to quadrupole time-offlight mass spectrometry[J].Food Control,2016,60:667-676.
[23]Costa F P,Caldas S S,Primel E G.Comparison of QuEChERSsample preparation methods for the analysis of pesticide residues in canned and fresh peach[J].Food Chemistry,2014,165:587-593.
[24]Zhang Keming(张科明),Liang Feiyan(梁飞燕),Deng Ming(邓鸣),et al.Multi-residue determination of veterinary drugs in porcine muscle by QuEChERS and liquid chromatographytandem mass spectrometry[J].Chinese Journal of Chromatography(色谱),2016,34(9):860-867.
[25]Zhang Shuo(张烁),Zhou Shuang(周爽),Chen Dawei(陈达炜),et al.Determination of ten sedative residues in livestock products by ultra high performance liquid chromatography-tandem mass spectrometry[J].Journal of Instrumental Analysis(分析测试学报),2014,33(11):1213-1218.
[26]Xue Liangchen(薛良辰),Cai Qinren(蔡勤仁),Zheng Xuan(郑璇),et al.Determination of 9 hydroxy veterinary drug residues in fish by QuEChERS-GPC-GC/MS[J].Journal of Chinese Mass Spectrometry Society(质谱学报),2017,38(6):655-663.
[27]Cao Yafei(曹亚飞),Kang Jian(康健),Chang Qiaoying(常巧英),et al.Multi-residue determination of veterinary drugs in cheese by Qu ECh ERS and liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Chromatography(色谱),2015,33(2):132-139.
[28]Gomez P M,Romero-Gonzalez R,Martinez V J,et al.Analysis of veterinary drug residues in cheese by ultra-high-performance LCcoupled to triple quadrupole MS/MS[J].Journal of Separation Science,2013,36(7):1223-1230.
[29]Matuszewski B K,Constanzer M L,Chavez-Eng C M.Strategies for the assessment of matrix effect in quantitative bioanalytical methods based on HPLC-MS/MS[J].Analytical Chemistry,2003,75(13):3019-3030.
[2]Mainero R L,Gentili A,Perez-Fernandez V,et al.Veterinary drugs residues:a review of the latest analytical research on sample preparation and LC-MS based methods[J].Food Additives&Contaminants:Part A,2017,34(5):766-784.
[3]Li Xiangli(李向丽),Zhang Na(张娜),Wang Wenlin(王文林).Research progress on detecting residues of chlorpromazine and diazepam in foods[J].Journal of Anhui Agricultural Sciences(安徽农业科学),2014,42(2):565-567.
[4]Gao Qian(高倩).Determination of phenothiazine sedatives,neonicotinoid pesticides and acetanilide herbicides in food by liquid chromatography tandem mass spectrometry[D].Shijiazhuang:Hebei Normal University(河北师范大学),2016.
[5]Pang N,Wang T L,Hu J.Method validation and dissipation kinetics of four herbicides in maize and soil using QuEChERS sample preparation and liquid chromatography tandem mass spectrometry[J].Food Chemistry,2016,190:793-800.
[6]Cervera M I,Portolés T,Pitarch E,et al.Application of gas chromatography time-of-flight mass spectrometry for target and non-target analysis of pesticide residues in fruits and vegetables[J].Journal of Chromatography A,2012,1244:168-177.
[7]Eec C R.On pharmacologically active substances and their classification regarding maximum residue limits in foodstuffs of animal origin[J].Official Journal of the European Communities,2010,50:1-72.
[8]Sun Wenjia(孙文佳),Shen Yudong(沈玉栋),Sun Yuanming(孙远明),et al.Determination of esidues of chlorpromazine in pork by chemiluminescent enzyme immunoassay[J].Analytical Chemistry(分析化学),2012,40(9):1397-1402.
[9]Liu W,Li W,Yin W,et al.Preparation of a monoclonal antibody and development of an indirect competitive ELISA for the detection of chlorpromazine residue in chicken and swine liver[J].Journal of the Science of Food and Agriculture,2010,90(11):1789-1795.
[10]Liu Jianjing(刘建静).Development of enzyme-linked immunosorbent assay(ELISA)for chlorpromazine[D].Beijing:Chinese Academy of Agricultural Sciences(中国农业科学院),2009.
[11]Cao Jie(曹洁),Jia Juan(贾娟),Wang Yujin(王玉瑾),et al.Determination of chlorpromazine in blood samples by hollow fiber-liquid phase micro-extraction coupled with gas chromatography[J].Chinese Journal of Health Laboratory Technology(中国卫生检验杂志),2013,23(15):3015-3017.
[12]Hong Yueling(洪月玲),Hao Xuefei(郝学飞),Dong Ke(董柯).HPLC determination of chlorpromazine residue in animal-derived foods[J].Food Science(食品科学),2009,30(14):269-271.
[13]Zhang L,Wu P,Zhang Y,et al.A GC/MS method for the simultaneous determination and quantification of chlorpromazine and diazepam in pork samples[J].Analytical Methods,2014,6(2):503-508.
[14]Gu Huabing(顾华兵),Xie Jie(谢洁),Peng Tao(彭涛),et al.Determination of chlorpromazine residues in chicken muscle tissues by high performance liquid chromatography-tandem mass spectrometry[J].China Poultry(中国家禽),2014,36(15):33-36.
[15]Liu Yan(刘燕),Su Ying(苏英),Lan Ruirong(兰瑞容),et al.Determination of antipsychotic drugs chlorpromazine and haloperidol in pork by HPLC-MS/MS[J].Chinese Journal of Pharmaceutical Analysis(药物分析杂志),2015,35(4):685-688.
[16]Dasenaki M E,Thomaidis N S.Multi-residue determination of 115veterinary drugs and pharmaceutical residues in milk powder,butter,fish tissue and eggs using liquid chromatography-tandem mass spectrometry[J].Analytica Chimica Acta,2015,880:103-121.
[17]Wang Jie(王杰),Pei Fei(裴斐),Li Peng(李彭),et al.Comparison of different sample pretreatments for the analysis of quinolone residues in porcine tissues[J].Food Science(食品科学),2018,39(18):309-314.
[18]Qin ling(覃玲),Dong Yalei(董亚蕾),Wang Gangli(王钢力),et al.Determination of 42 veterinary drug residues in common animal derived food by dispersive solid phase extraction coupled with liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Chromatography(色谱),2018,36(9):880-888.
[19]Pi?tkowska M,Gbylik-Sikorska M,Gajda A,et al.Multiresidue determination of veterinary medicines in lyophilized egg albumen with subsequent consumer exposure evaluation[J].Food Chemistry,2017,229:646-652.
[20]Shao Linzhi(邵琳智),Xie Minling(谢敏玲),Lin Feng(林峰).Determination of chloramphenicol in propolis by high performance liquid chromatography-tandem mass spectrometry[J].Journal of Instrumental Analysis(分析测试学报),2017,36(8):1029-1032.
[21]Li Rong(李蓉),Yang Luqi(杨璐齐),Zhang Pengyun(张鹏云),et al.Rapid screening of 24 tranquillizer drugs in fish and fishery products by ultra-high performance liquid chromatographyquadrupole/electrostatic field orbitrap high resolution mass spectroscopy[J].Chinese Journal of Chromatography(色谱),2018,36(2):125-135.
[22]Zhang Y,Zhang J,Liu X,et al.Rapid screening and quantification of multi-class multi-residue veterinary drugs in royal jelly by ultra performance liquid chromatography coupled to quadrupole time-offlight mass spectrometry[J].Food Control,2016,60:667-676.
[23]Costa F P,Caldas S S,Primel E G.Comparison of QuEChERSsample preparation methods for the analysis of pesticide residues in canned and fresh peach[J].Food Chemistry,2014,165:587-593.
[24]Zhang Keming(张科明),Liang Feiyan(梁飞燕),Deng Ming(邓鸣),et al.Multi-residue determination of veterinary drugs in porcine muscle by QuEChERS and liquid chromatographytandem mass spectrometry[J].Chinese Journal of Chromatography(色谱),2016,34(9):860-867.
[25]Zhang Shuo(张烁),Zhou Shuang(周爽),Chen Dawei(陈达炜),et al.Determination of ten sedative residues in livestock products by ultra high performance liquid chromatography-tandem mass spectrometry[J].Journal of Instrumental Analysis(分析测试学报),2014,33(11):1213-1218.
[26]Xue Liangchen(薛良辰),Cai Qinren(蔡勤仁),Zheng Xuan(郑璇),et al.Determination of 9 hydroxy veterinary drug residues in fish by QuEChERS-GPC-GC/MS[J].Journal of Chinese Mass Spectrometry Society(质谱学报),2017,38(6):655-663.
[27]Cao Yafei(曹亚飞),Kang Jian(康健),Chang Qiaoying(常巧英),et al.Multi-residue determination of veterinary drugs in cheese by Qu ECh ERS and liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Chromatography(色谱),2015,33(2):132-139.
[28]Gomez P M,Romero-Gonzalez R,Martinez V J,et al.Analysis of veterinary drug residues in cheese by ultra-high-performance LCcoupled to triple quadrupole MS/MS[J].Journal of Separation Science,2013,36(7):1223-1230.
[29]Matuszewski B K,Constanzer M L,Chavez-Eng C M.Strategies for the assessment of matrix effect in quantitative bioanalytical methods based on HPLC-MS/MS[J].Analytical Chemistry,2003,75(13):3019-3030.