中国地质学会岩矿测试技术专业委员会、国家地质实验测试中心主办

食品中有机氯农药和多氯联苯气相色谱-质谱分析的离子化方式

曹孝文, 邹宽, 徐丹, 沈伟健, 练鸿振, 葛欣, 沈崇钰. 食品中有机氯农药和多氯联苯气相色谱-质谱分析的离子化方式[J]. 岩矿测试, 2013, 32(1): 22-27.
引用本文: 曹孝文, 邹宽, 徐丹, 沈伟健, 练鸿振, 葛欣, 沈崇钰. 食品中有机氯农药和多氯联苯气相色谱-质谱分析的离子化方式[J]. 岩矿测试, 2013, 32(1): 22-27.
Xiao-wen CAO, Kuan ZOU, Dan XU, Wei-jian SHEN, Hong-zhen LIAN, Xin GE, Chong-yu SHEN. Different Ionization Modes in Gas Chromatography-Mass Spectrometric Determination of Organochlorine Pesticides and Polychlorinated Biphenyls in Food[J]. Rock and Mineral Analysis, 2013, 32(1): 22-27.
Citation: Xiao-wen CAO, Kuan ZOU, Dan XU, Wei-jian SHEN, Hong-zhen LIAN, Xin GE, Chong-yu SHEN. Different Ionization Modes in Gas Chromatography-Mass Spectrometric Determination of Organochlorine Pesticides and Polychlorinated Biphenyls in Food[J]. Rock and Mineral Analysis, 2013, 32(1): 22-27.

食品中有机氯农药和多氯联苯气相色谱-质谱分析的离子化方式

  • 基金项目:
    国家重点基础研究发展计划(973计划)项目(2009CB421601); 国家自然科学基金项目(90913012);公益性行业科研专项基金项目(200810099)
详细信息
    作者简介: 曹孝文,硕士,从事食品安全分析。E-mail:cherrycxw@126.com
    通讯作者: 练鸿振,博士,教授,博士生导师,主要从事色谱/质谱分析研究。E-mail:hzlian@nju.edu.cn 葛欣,博士,教授,主要从事色谱/质谱分析研究。E-mail:gexin@nju.edu.cn
  • 中图分类号: O657.63;S482.32; O625.21

Different Ionization Modes in Gas Chromatography-Mass Spectrometric Determination of Organochlorine Pesticides and Polychlorinated Biphenyls in Food

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  • 对食品中有机氯农药和多氯联苯的气相色谱-质谱联用(GC-MS)分析方法中三种离子化方式,电子轰击电离(EI)、正化学电离(PCI)和负化学电离(NCI)进行了总结和比较。PCI-MS/MS方法和EI-MS/MS方法都有很高的选择性和较高的灵敏度;PCI方法在分析含硝基、羰基等基团的化合物时有明显优势,EI则在分析狄氏剂、异狄氏剂、硫丹及其代谢物时比PCI表现稍好,而NCI-MS的灵敏度最高,但抗干扰能力稍弱,且不适合分析滴滴涕类和多氯联苯类化合物。在食品安全分析中,三种质谱方法的准确性好,精密度高,检测限较低,都能够满足食品中农残检测的要求,在日常检测工作中可互为补充和替代。同时指出,GC在有机氯化合物分析中仍表现出明显的优越性;常规的GC-MS尤其在EI电离模式下,易受到基质干扰而使谱图变得复杂;新型离子化方式包括高选择性化学电离技术的应用,将是食品安全中GC-MS联用分析的发展方向之一。
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  • [1]

    El-Shahawi M S, Hamza A, Bashammakh A S, Al-Saggaf W T. An overview on the accumulation, distribution, transformations, toxicity and analytical methods for the monitoring of persistent organic pollutants[J].Talanta, 2010, 80: 1587-1597. doi: 10.1016/j.talanta.2009.09.055

    [2]

    Qin Y Y, Leung C K M, Lin C K, Leung A O W, Wang H S, Giesy J P, Wong M H. Halogenated POPs and PAHs in blood plasma of Hong Kong residents[J].Environmental Science & Technology, 2011, 45: 1630-1637.

    [3]

    Iozza S, Muller C E, Schmid P, Bogdal C, Oehme M. Historical profiles of chlorinated paraffins and polychlorinated biphenyls in a dated sediment core from Lake Thun (Switzerland)[J].Environmental Science & Technology, 2008, 42: 1045-1050.

    [4]

    Hopf N B, Ruder A M, Succop P. Background levels of polychlorinated biphenyls in the US population[J].Science of the Total Environment, 2009, 407: 6109-6119. doi: 10.1016/j.scitotenv.2009.08.035

    [5]

    Henriquez-Hernandez L A, Luzardo O P, Almeida-Gonzalez M, Alvarez-Leon E E, Serra-Majem L, Zumbado M, Boada L D. Background levels of polychlorinated biphenyls in the population of the Canary Islands (Spain)[J].Environmental Reviews, 2011, 111: 10-16.

    [6]

    Chia K J, Huang S D. Analysis of organochlorine pesticides in wine by solvent bar microextraction coupled with gas chromatography with tandem mass spectrometric detection[J].Rapid Communications in Mass Spectrometry, 2006, 20: 118-124. doi: 10.1002/(ISSN)1097-0231

    [7]

    Jeon H R, Abd El-Aty M, Cho S K, Chio J H, Kim K Y, Park R D, Shim J H. Multiresidue analysis of four pesticide residues in water dropwort (Oenanthe javanica) via pressurized liquid extraction, supercriticall fluid extraction, and liquid-liquid extraction and gas chromatographic determination[J].Journal of Separation Science, 2007, 30: 1953-1963. doi: 10.1002/(ISSN)1615-9314

    [8]

    Zawiyah S, Man Y B C, Nazimah S A H, Chin C K, Tsukamoto I, Hamanyza A H, Norhaizan I. Determination of organochlorine and pyrethroid pesticides in fruit and vegetables using SAX/PSA clean-up column[J].Food Chemistry, 2007, 102: 98-103. doi: 10.1016/j.foodchem.2006.05.003

    [9]

    Wilkowska A M, Biziuk M. Rapid method for the deter-mination of organochlorine pesticides and PCBs in fish muscle samples by microwave-assisted extraction and analysis of extracts by GC-ECD[J].Journal of AOAC International, 2010, 93: 1987-1994.

    [10]

    Beyer A, Biziuk M. Comparison of efficiency of different sorbents used during clean-up of extracts for determination of polychlorinated biphenyls and pesticide residues in low-fat food[J].Food Research International, 2010, 43: 831-837. doi: 10.1016/j.foodres.2009.11.018

    [11]

    Cieslik E, Sadowska-Rociek A, Ruiz J M M, Surma-Zadora M. Evaluation of QuEChERS method for the determination of organochlorine pesticide residues in selected groups of fruits[J]. Food Chemistry, 2011, 125: 773-778. doi: 10.1016/j.foodchem.2010.09.019

    [12]

    Garcia-Rodriguez D, Carro A M, Cela R, Lorenzo R A. Microwave-assisted extraction and large-volume injection gas chromatography tandem mass spectrometry determination of multiresidue pesticides in edible seaweed[J].Analytical and Bioanalytical Chemistry, 2010, 398: 1005-1016. doi: 10.1007/s00216-010-4006-z

    [13]

    Alder L, Greulich K, Kempe G, Vieth B. Residue analysis of 500 high priority pesticides: Better by GC-MS or LC-MS/MS[J].Mass Spectrometry Reviews, 2006, 25: 838-865. doi: 10.1002/(ISSN)1098-2787

    [14]

    Chusaksri S, Sutthivaiyakit S, Sutthivaiyakit P. Confir-matory determination of organochlorine pesticides in surface waters using LC/APCI/tandem mass spectrometry[J].Analytical and Bioanalytical Chemistry, 2006, 384: 1236-1245. doi: 10.1007/s00216-005-0248-6

    [15]

    Famiglini G, Palma P, Pierini E, Trufelli H, Cappiello A. Organochlorine pesticides by LC-MS[J].Analytical Chemistry, 2008, 80: 3445-3449. doi: 10.1021/ac8000435

    [16]

    Ramesh A, Vijayalakshmi A. Environmental exposure to residues after aerial spraying of endosulfan: Residues in cow milk, fish, water, soil and cashew leaf in Kasargode, Kerala, India[J].Pest Management Science, 2002, 58: 1048-1054. doi: 10.1002/(ISSN)1526-4998

    [17]

    Blasco C, Fernandez M, Pena A, Lino C, Silveira M I, Font G, Pico Y. Assessment of pesticide residues in honey samples from Portugal and Spain[J]. Journal of Agricultural and Food Chemistry, 2003, 51: 8132-8138. doi: 10.1021/jf034870m

    [18]

    Zhang Z L, Ohiozebau E, Rhind S M. Simultaneous extraction and clean-up of polybrominated diphenyl ethers and polychlorinated biphenyls from sheep liver tissue by selective pressurized liquid extraction and analysis by gas chromatography-mass spectrometry[J].Journal of Chromatography A,2011,1218:1203-1209. doi: 10.1016/j.chroma.2010.12.098

    [19]

    Frenich A G, Plaza-B R, Vidal J L M. Compari-son of tandem-in-space and tandem-in-time mass spectrometry in gas chromatography determination of pesticides: Application to simple and complex food samples[J].Journal of Chromatography A, 2008, 1203: 229-238. doi: 10.1016/j.chroma.2008.07.041

    [20]

    Kosikowska M, Biziuk M. Review of the determination of pesticide residues in ambient air[J].Trends in Analytical Chemistry, 2010, 29: 1064-1072. doi: 10.1016/j.trac.2010.06.008

    [21]

    Wong J W, Zhang K, Tech K, Hayward D G, Makovi C M, Krynitsky A J, Schenck F J, Banerjee K, Dasgupta S, Brown D. Multiresidue pesticide analysis in fresh produce by capillary gas chromatography-mass spectro-metry/selective ion monitoring (GC-MS/SIM) and -tandem mass spectrometry (GC-MS/MS)[J].Journal of Agricultural and Food Chemistry, 2010, 58: 5868-5883. doi: 10.1021/jf903854n

    [22]

    Vidal J L M, Arrebola F J, Mateu-Sanchez M. Appli-cation of gas chromatography-tandem mass spectrometry to the analysis of pesticides in fruits and vegetables[J].Journal of Chromatography A, 2002, 959: 203-213. doi: 10.1016/S0021-9673(02)00444-2

    [23]

    Frenich A G, Moreno J L F, Vidal J L M, Liebanas F J A. Application of gas chromatography coupled to triple quadrupole mass spectrometry for the multiresidue analysis of pesticides in olive oil[J].Journal of Agricultural and Food Chemistry, 2007, 55: 8346-8352. doi: 10.1021/jf071615j

    [24]

    Bolanos P P, Frenich A G, Vidal J L M. Application of gas chromatography-triple quadrupole mass spectrometry in the quantification-confirmation of pesticides and polychlorinated biphenyls in eggs at trace levels[J].Journal of Chromatography A, 2007, 1167: 9-17. doi: 10.1016/j.chroma.2007.08.019

    [25]

    Gomara B, Garcia-Ruiz C, Gonzalez M J, Marina M J. Fractionation of chlorinated and brominated persistent organic pollutants in several food samples by pyrenyl-silica liquid chromatography prior to GC-MS determination[J].Analytica Chimica Acta, 2006, 565: 208-213. doi: 10.1016/j.aca.2006.02.053

    [26]

    Saito K, Sjodin A, Sandau C D, Davis M D, Nakazawa H, Matsuki Y, Patterson D G. Development of a accelerated solvent extraction and gel permeation chromatography analytical method for measuring persistent organohalogen compounds in adipose and organ tissue analysis[J].Chemosphere, 2004, 57: 373-381. doi: 10.1016/j.chemosphere.2004.04.050

    [27]

    Rivera-Rodriguez L B, Rodriguez-Estrella R, Ellington J J, Evans J J. Quantification of low levels of organochlorine pesticides using small volumes (≤100μl) of plasma of wild birds through gas chromatography negative chemical ionization mass spectrometry[J].Environmental Pollution, 2007, 148: 654-662. doi: 10.1016/j.envpol.2006.11.018

    [28]

    Yoon H R, Cho S Y, Kim J M, Yoon I B, Park M K, Park J H. Analysis of multi-component pesticide residues in herbal medicines by GC-MS with electron impact ionization and with positive- and negative-ion chemical ionization[J].Chromatographia, 1999, 49: 525-534. doi: 10.1007/BF02467753

    [29]

    Chaler R, Vilanova R, Santiago-Silva M, Fernandez P, Grimalt J O. Enhanced sensitivity in the analysis of trace organochlorine compounds by negative-ion mass spectrometry with ammonia as reagent gas[J].Journal of Chromatography A, 1998, 823: 73-79. doi: 10.1016/S0021-9673(98)00516-0

    [30]

    Rothweiler B, Berset J D. High sensitivity of ortho-substituted polychlorobiphenyls in negative ion mass spectrometry (NCI-MS): A comparison with EI-MS and ECD for the determination of regulatory PCBs in soils[J].Chemosphere, 1999, 38: 1517-1532. doi: 10.1016/S0045-6535(98)00372-5

    [31]

    Chernetsova E S, Revelsky A I, Revelsky I A, Mikhasenko I A, Sobolevsky T G. Determination of polychlorinated dibenzo-p-dioxins, dibenzofurans, and biphenyls by gas chromatography/mass spectrometry in the negative chemical ionization mode with different reagent gases[J].Mass Spectrometry Reviews, 2002, 21: 373-387. doi: 10.1002/(ISSN)1098-2787

    [32]

    Niessner G, Buchberger W, Eckerstorfer R. Multi-residue screening methods for the determination of pesticides in plant materials[J].Journal of Chromatography A, 1999, 846: 341-348. doi: 10.1016/S0021-9673(99)00198-3

    [33]

    Zhang X A, Mobley N, Zang J G, Zheng X M, Lu L, Ragin O, Smith C J. Analysis of agricultural residues on tea using d-SPE sample preparation with GC-NCI-MS and UHPLC-MS/MS[J].Journal of Agricultural and Food Chemistry, 2010, 58: 11553. doi: 10.1021/jf102476m

    [34]

    Medina C M, Pitarch E, Portoles T, Lopez F J, Hernandez F. GC-MS/MS multi-residue method for the determination of organochlorine pesticides, polychlori-nated biphenyls and polybrominated diphenyl ethers in human breast tissues[J].Journal of Separation Science, 2009, 32: 2090-2102. doi: 10.1002/jssc.v32:12

    [35]

    Hernando M D, Aguera A, Fernandez-Alba A R, Piedra L, Contreras M. Gas chromatographic determination of pesticides in vegetable samples by sequential positive and negative chemical ionization and tandem mass spectrometric fragmentation using an ion trap analyzer[J].Analyst, 2001, 126: 46-51. doi: 10.1039/b006933g

    [36]

    Haib J, Hofer I, Renaud J M. Analysis of multiple pesticide residues in tobacco using pressurized liquid extraction, automated solid-phase extraction clean-up and gas chromatography-tandem mass spectrometry[J].Journal of Chromatography A, 2003, 1020: 173-187. doi: 10.1016/j.chroma.2003.08.049

    [37]

    Louter A J H, van Doornmalen J, Vreuls J J, Brinkman U A T. On-line solid-phase extraction thermal desorp-tion gas chromatography with ion trap detection tandem mass spectrometry for the analysis of microcontaminants in water[J].Journal of High Resolution Chromatography, 1996, 19: 679-685. doi: 10.1002/(ISSN)1521-4168

    [38]

    Sauret N, Millet M, Herckes P, Mirabel P, Wortham H. Analytical method using gas chromatography and ion trap tandem mass spectrometry for the determination of S-triazines and their metabolites in the atmosphere[J].Environmental Pollution, 2000, 110: 243-252. doi: 10.1016/S0269-7491(99)00299-7

    [39]

    Aguera A, Contreras M, Crespo J, Fernandez-Alba A R. Multiresidue method for the analysis of multiclass pesticides in agricultural products by gas chromatography-tandem mass spectrometry[J].Analyst, 2002, 127: 347-354. doi: 10.1039/b109499h

    [40]

    Hernando M D, Piedra L, Belmonte A, Aguera A, Fernandez-Alba A R. Determination of traces of five antifouling agents in water by gas chromatography with positive/negative chemical ionisation and tandem mass spectrometric detection[J]. Journal of Chromatography A, 2001, 938: 103-111. doi: 10.1016/S0021-9673(01)01201-8

    [41]

    Mastovska K, Lehotay S J. Rapid sample preparation method for LC-MS/MS or GC-MS analysis of acrylamide in various food matrices[J].Journal of Agricultural and Food Chemistry, 2006, 54: 7001-7008. doi: 10.1021/jf061330r

    [42]

    Cao X W, Shen W J, Zhu J, Zhang J, Jiang Y, Zhao Z Y, Wu B, Yu K Y, Liu H, Lian H Z, Shen C Y. A comparative study of the ionization modes in GC-MS multi-residue method for the determination of organo-chlorine pesticides and polychlorinated biphenyls in crayfish[J].Food Analytical Method, DOI: 10.1007/s12161-012-9447-x.

    [43]

    Portoles T, Sancho J V, Hernandez F, Newton A, Hancock P. Potential of atmospheric pressure chemical ionization source in GC-QTOF MS for pesticide residue analysis[J].Journal of Mass Spectrometry, 2010, 45: 926-936. doi: 10.1002/jms.1784

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出版历程
收稿日期:  2012-05-24
录用日期:  2012-06-09

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