基于UPLC-MS/MS的几种农兽药残留检测的研究
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摘要
2008年全球金融危机爆发以来,世界各国针对农兽药残留限量制定了更为严格的要求,对进口食品中有害物质的残留限量设置高门槛,使得农兽药残留检测方法的开发迫在眉睫。本文基于UPLC-MS/MS技术,对那罗星、西玛津、萎锈灵、除虫脲和鱼藤酮几种农兽药残留进行检测,所做工作如下:(1)UPLC-MS/MS检测方法的建立和质量控制研究;(2)基于UPLC-MS/MS技术的13种动物源性食品中那罗星残留提取净化方法及检测技术研究;(3)基于UPLC-MS/MS技术的茶叶中西玛津、萎锈灵、除虫脲和鱼藤酮四种农药残留的同时检测提取净化方法及检测技术研究。取得的主要结论如下:
1.建立了一种从13中不同动物源性基质中提取那罗星残留的前处理方法,该方法用乙酸乙酯、甲醇和乙腈针对不同样品提取,正己烷除酯,Tris碱定容,有效提取那罗星。平均回收率范围为72%-100%,RSD为2.8%-11.83%。
2.建立了快速、简便的UPLC-MS/MS多反应监测模式来测定13种不同动物源性食品基质中那罗星药物残留的检测方法,采用UPLC-MS/MS定量定性,通过C18反相色谱柱并在ESI-模式下检测,检测限为0.005 mg/kg,定量限为0.01 mg/kg。线性范围为0.01-0.1 mg/kg。
3.建立了同时提取茶叶中西玛津、萎锈灵、除虫脲和鱼藤酮4种农药残留的方法,试样经饱和氯化钠溶液浸润后,用乙酸乙酯提取,离心后用PSA吸附剂,C18粉和石墨化碳黑粉分散净化,乙酸乙酯层经氮吹至近干,定容过膜,可以作为UPLC-MS/MS检测样品。用外标法定量,0.01,0.02和0.05 mg/kg三个添加水平下,四种农药的回收率为77.4%-95.3%,RSD为4.2%-11.8%。
4.建立了茶叶中西玛津、萎锈灵、除虫脲和鱼藤酮4种农药残留的检测方法。通过ACQUITY UPLC? HSS T3色谱柱(2.1 mm×100 mm,粒径1.8μm)色谱柱分离,MRM模式采集质谱数据。得到4种药物的检出限均为0.001 mg/kg,定量限为0.005 mg/kg,低于欧盟制定的关于茶叶中西玛津、萎锈灵、除虫脲和鱼藤酮4种农药的最大残留限量。
本文的研究成果为制订国家出入境检验检疫行业标准《进出口动物源性食品中那罗星残留量检测方法液相色谱-质谱/质谱法》奠定了基础,有利于我国动物性食品出口企业有效应对日本肯定列表;为我国茶叶制品出口欧盟,顺利通关提供技术支撑。
Because of slather using pesticides and veterinary drugs, it promoted the rapid development of agriculture; meanwhile, it also endangered the quality and safety of food. In recent years China has broken out many food safety incidents, so, foreign countries have a confidence crisis about the food quality and safety of our country. Especially since the global financial crisis broken out in 2008, lots of countries and regions in the world have make more stringent trade protection measures, and some developed countries have continued to strengthen its technology, and set the high threshold residue limits for harmful substances in import-food, which result in China's food exports trouble. by contrast with the Europe-US and other developed countries.
This paper researched the method for determination of pesticides and veterinary drug residues in food based on UPLC-MS/MS technology. The relevant work I made is as follows: (1) Study on establishing the UPLC-MS/MS methods and its quality control, (2)Research on the purification, extraction and determination of nanafroin residue in 13 different kind of food of animal food origin based on UPLC-MS/MS technology, (3)Study on based he purification, extraction and determination of simazine, carboxin, difluron and rotenone residues in tea based on UPLC-MS/MS method.
The results obtained by experimentwere as follow:
1. Established an extraction method to extract nanafrocin residue in 13 different kind of food of animal food origin. It was extracted with ethyl acetate and acetonitrile, using n-hexane to discard the fat, calibrate the volume to scale by Tris base solution, the method can effective extract the target material. The mean overall recoveries of nanafrocin varied from 71% to 101%, RSD was 2.8 %-11.83 %
2. Established a fast, simple and UPLC-MS/MS to analysis nanafrocin residue in 13 different kind of food of animal food origin. The researchers applied a C18 stationary phase coupled to triple quadrupole tandem mass spectrometry in negative electrospray mode. The limit of detection (LOD) was 0.005 mg/kg and the limit of quantification (LOQ) was 0.01 mg/kg in the matrixes. The detector responses were found to be linear over the range 0.01-0.1 mg/kg in each matrix. In conclusion, identification and quantification of nanafrocin residues in foodstuffs of animal origin were successfully achieved using LC-MS/MS. The method can be used to analyze the nanafrocin efficiently.
3. A method for simultaneous determination of simazine, carboxin, diflubenzuron and rotenone in green tea was developed. Ethyl acetate was used to extract the residues after green tea sample was infiltrated in saturated aqueous sodium chloride solution, and the sample was cleaned up with PSA, C18 and graphitized carbon black powder. After that, the ethyl acetate supernatant was concentrated by the nitrogen evaporator. The residues were dissolved with mobile phase and syringe filtered using a 0.22μm nylon filter, tested by UPLC-MS/MS. The average recoveries of 77.4%-95.3%, and the RSD is 4.2%-11.8%.
4. Chromatographic separation was performed on an ACQUITY UPLC? HSS T3 column (2.1 mm×100 mm, 1.8μm) using gradient elution. The positive ionization mode was used and the ions were monitored in the multiple reaction monitoring (MRM) mode. The limit of detection (LOD) is 0.005 mg/L and the limit of quantitation (LOQ) is 0.001 mg/L all of the three substances.
The study on pesticide and veterinary drug residue limits and testing criteria in China the lagged somewhat. In order to safeguard the international impress of Chinese food, to adapt to fierce competition in international trade, and to meet the needs of food safety, we need to establish simple, practical and method to analysis the pesticides and veterinary drug residues in food.
1.建立了一种从13中不同动物源性基质中提取那罗星残留的前处理方法,该方法用乙酸乙酯、甲醇和乙腈针对不同样品提取,正己烷除酯,Tris碱定容,有效提取那罗星。平均回收率范围为72%-100%,RSD为2.8%-11.83%。
2.建立了快速、简便的UPLC-MS/MS多反应监测模式来测定13种不同动物源性食品基质中那罗星药物残留的检测方法,采用UPLC-MS/MS定量定性,通过C18反相色谱柱并在ESI-模式下检测,检测限为0.005 mg/kg,定量限为0.01 mg/kg。线性范围为0.01-0.1 mg/kg。
3.建立了同时提取茶叶中西玛津、萎锈灵、除虫脲和鱼藤酮4种农药残留的方法,试样经饱和氯化钠溶液浸润后,用乙酸乙酯提取,离心后用PSA吸附剂,C18粉和石墨化碳黑粉分散净化,乙酸乙酯层经氮吹至近干,定容过膜,可以作为UPLC-MS/MS检测样品。用外标法定量,0.01,0.02和0.05 mg/kg三个添加水平下,四种农药的回收率为77.4%-95.3%,RSD为4.2%-11.8%。
4.建立了茶叶中西玛津、萎锈灵、除虫脲和鱼藤酮4种农药残留的检测方法。通过ACQUITY UPLC? HSS T3色谱柱(2.1 mm×100 mm,粒径1.8μm)色谱柱分离,MRM模式采集质谱数据。得到4种药物的检出限均为0.001 mg/kg,定量限为0.005 mg/kg,低于欧盟制定的关于茶叶中西玛津、萎锈灵、除虫脲和鱼藤酮4种农药的最大残留限量。
本文的研究成果为制订国家出入境检验检疫行业标准《进出口动物源性食品中那罗星残留量检测方法液相色谱-质谱/质谱法》奠定了基础,有利于我国动物性食品出口企业有效应对日本肯定列表;为我国茶叶制品出口欧盟,顺利通关提供技术支撑。
Because of slather using pesticides and veterinary drugs, it promoted the rapid development of agriculture; meanwhile, it also endangered the quality and safety of food. In recent years China has broken out many food safety incidents, so, foreign countries have a confidence crisis about the food quality and safety of our country. Especially since the global financial crisis broken out in 2008, lots of countries and regions in the world have make more stringent trade protection measures, and some developed countries have continued to strengthen its technology, and set the high threshold residue limits for harmful substances in import-food, which result in China's food exports trouble. by contrast with the Europe-US and other developed countries.
This paper researched the method for determination of pesticides and veterinary drug residues in food based on UPLC-MS/MS technology. The relevant work I made is as follows: (1) Study on establishing the UPLC-MS/MS methods and its quality control, (2)Research on the purification, extraction and determination of nanafroin residue in 13 different kind of food of animal food origin based on UPLC-MS/MS technology, (3)Study on based he purification, extraction and determination of simazine, carboxin, difluron and rotenone residues in tea based on UPLC-MS/MS method.
The results obtained by experimentwere as follow:
1. Established an extraction method to extract nanafrocin residue in 13 different kind of food of animal food origin. It was extracted with ethyl acetate and acetonitrile, using n-hexane to discard the fat, calibrate the volume to scale by Tris base solution, the method can effective extract the target material. The mean overall recoveries of nanafrocin varied from 71% to 101%, RSD was 2.8 %-11.83 %
2. Established a fast, simple and UPLC-MS/MS to analysis nanafrocin residue in 13 different kind of food of animal food origin. The researchers applied a C18 stationary phase coupled to triple quadrupole tandem mass spectrometry in negative electrospray mode. The limit of detection (LOD) was 0.005 mg/kg and the limit of quantification (LOQ) was 0.01 mg/kg in the matrixes. The detector responses were found to be linear over the range 0.01-0.1 mg/kg in each matrix. In conclusion, identification and quantification of nanafrocin residues in foodstuffs of animal origin were successfully achieved using LC-MS/MS. The method can be used to analyze the nanafrocin efficiently.
3. A method for simultaneous determination of simazine, carboxin, diflubenzuron and rotenone in green tea was developed. Ethyl acetate was used to extract the residues after green tea sample was infiltrated in saturated aqueous sodium chloride solution, and the sample was cleaned up with PSA, C18 and graphitized carbon black powder. After that, the ethyl acetate supernatant was concentrated by the nitrogen evaporator. The residues were dissolved with mobile phase and syringe filtered using a 0.22μm nylon filter, tested by UPLC-MS/MS. The average recoveries of 77.4%-95.3%, and the RSD is 4.2%-11.8%.
4. Chromatographic separation was performed on an ACQUITY UPLC? HSS T3 column (2.1 mm×100 mm, 1.8μm) using gradient elution. The positive ionization mode was used and the ions were monitored in the multiple reaction monitoring (MRM) mode. The limit of detection (LOD) is 0.005 mg/L and the limit of quantitation (LOQ) is 0.001 mg/L all of the three substances.
The study on pesticide and veterinary drug residue limits and testing criteria in China the lagged somewhat. In order to safeguard the international impress of Chinese food, to adapt to fierce competition in international trade, and to meet the needs of food safety, we need to establish simple, practical and method to analysis the pesticides and veterinary drug residues in food.
引文
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Marta Llorca, Marinella Farré, Yolanda Picó, DamiàBarceló.2009.Development and validation of a pressurized liquid extraction liquid chromatography–tandem mass spectrometry method for perfluorinated compounds determination in fish. Journal of Chromatography A, 1216(43): 7195-7204
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Rokuro Masuma, De-Zhong Zhen, Yoshitake Tanaka, Satoshi Omura.1990.Site of regulation of nanaomycin biosynthesis by inorganic phosphate. The Journal of Antibiotics, 43(1): 83-87
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Yoshitake Tanaka, Rokuro Masuma, Satoshi Omura.1984.Control of ammonium ion level for efficient nanaomycin production.The Journal of Antibiotics, 37(1-2):1370-1375
Zhiqiang Huang, Yongjun Li, Bo Chen, Shouzhuo Yao. 2007.Simultaneous determination of 102 pesticide residues in Chinese teas by gas chromatography–mass spectrometry. Journal of Chromatography B,853(1-2): 154-162
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SN 0594-1996出口肉及肉制品中西玛津残留检验方法
GB/T 21925-2008水中除草剂残留测定液相色谱/质谱法
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Haruo Tanaka, Yasuaki Koyama, Juichi Awaya, Hirofuto Marumo, Ruiko Oiwa, Michiko Katagiri, Toshiaki Nagai, Satoshi Omura.1975.Nanaomycins, new antibiotics produced by a strain of streptomyces.The Journal of Antibiotics, 28 (11):860-867
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M. Castellari, M. Gratacós-Cubarsí, J.A. García-Regueiroa.2009.Detection of tetracycline and oxytetracycline residues in pig and calf hair by ultra-high-performance liquid chromatography tandem mass spectrometry. Journal of Chromatography A, 1216(46): 8096-8100
M. Clemente, M.P. Hermo, D. Barrón, J. Barbosa.2006. Confirmatory and quantitative analysis using experimental design for the extraction and liquid chromatography–UV, liquid chromatography–mass spectrometry and liquid chromatography–mass spectrometry/mass spectrometry determination of quinolones in turkey muscle. Journal of Chromatography A, 1135(2): 170-178
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Marilyn J. Schneider, Ahmed M. Darwish, Donald W. Freeman.2007.Simultaneous multiresidue determination of tetracyclines and fluoroquinolones in catfish muscle using high performance liquidchromatography with fluorescence detection. Analytica Chimica Acta, 586(1-2):269-274
Marta Llorca, Marinella Farré, Yolanda Picó, DamiàBarceló.2009.Development and validation of a pressurized liquid extraction liquid chromatography–tandem mass spectrometry method for perfluorinated compounds determination in fish. Journal of Chromatography A, 1216(43): 7195-7204
Mira Petrovi?, Maria Dolores Hernando, M. Silvia Díaz-Cruz, DamiàBarceló. 2005. Liquid chromatography–tandem mass spectrometry for the analysis of pharmaceutical residues in environmental samples: a review. Journal of Chromatography A, 1067(1-2): 1-14
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Yang Xiao, Hong Chang, Ai Jia, Jianying Hu.2008.Trace analysis of quinolone and fluoroquinolone antibiotics from wastewaters by liquid chromatography–electrospray tandem mass spectrometry. Journal of Chromatography A, 1214(1-2): 100-108
Yoshitake Tanaka, Kiseko Kamei, Kazuhiko Otoguro, Satoshi Omura.1999. Heme-dependent Radical Generation: Possible Involvement in Antimalarial Action of Non-peroxide Microbial Metabolites, Nanaomycin A and Radicicol. The Journal of Antibiotics, 52(10): 880-888
Yoshitake Tanaka, Rokuro Masuma, Satoshi Omura.1984.Control of ammonium ion level for efficient nanaomycin production.The Journal of Antibiotics, 37(1-2):1370-1375
Zhiqiang Huang, Yongjun Li, Bo Chen, Shouzhuo Yao. 2007.Simultaneous determination of 102 pesticide residues in Chinese teas by gas chromatography–mass spectrometry. Journal of Chromatography B,853(1-2): 154-162