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A Modified QuEChERS Sample Preparation Method for Simultaneous Determination of 62 Pesticide Residues in Edible Fungi Using Gas Chromatography–Triple Quadrupole Mass Spectrometry

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Abstract

A rapid analytical method for the simultaneous determination of 62 pesticides in edible fungi was established based on modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) sample preparation method with gas chromatography–triple mass spectrometry (GC–MS/MS). Before extracting the target compounds from edible fungi, the dry samples were soaked in distilled water for 30 min to improve the extraction efficiency. The samples were extracted with acetonitrile–water and acetic acid–sodium acetate buffer solution (pH = 5.5) and salted out by anhydrous MgSO4. Then the extracts were cleaned up with n-propyl ethylene diamine (PSA), octadecylsilane (C18), graphitized carbon black (GCB), and anhydrous MgSO4. Additional concentration steps were performed in this to improve the sensitivity of the method. Finally, the cleaned extracts were detected by GC–MS/MS in multi-reaction monitoring (MRM) mode, and the internal standard curve method was applied to quantify the pesticides. In the linear range of each pesticide, good linear calibrations with coefficients (R 2) with additional concentration steps were performed in this to improve the sensitidry Lentinula edodes. Recoveries at three levels (10, 50, and 100 μg/kg) ranged from 75.4 to 117.1 % for all the compounds, with relative standard deviations (RSD) between 3.2 and 15.2 %. The limits of quantification (LOQs) were 0.625–20 μg/kg. The QuEChERS method was more straightforward, less time and labor intensive, as well as more sensitive, selective, and accurate for screening multiple pesticide residues, and it has been applied to edible fungi samples from different provinces in China.

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References

  • Agilent (2014) Agilent bond elut silica-based SPE selection guide. Agilent Technologies. https://www.chromspec.com/pdf/e/ag78.pdf. Accessed Jun 2014

  • Agilent (2014) Agilent sampliQ products for sample preparation. Agilent Technologies. http://www.chem.agilent.com/Library/brochures/5989-9334EN.pdf. Accessed Jun 2014

  • Anastassiades M, Lehotay SJ, Stajnbaher D, Schenck FJ (2003) Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce. J AOAC Int 86(2):412–431

    CAS  Google Scholar 

  • Beltran J, Lopez FJ, Cepria O, Hernandez F (1998) Solid-phase microextraction for quantitative analysis of organophosphorus pesticides in environmental water samples. J Chromatogr A 808:257–263

    Article  CAS  Google Scholar 

  • Bidari A, Ganjali MR, Norouzi P et al (2011) Sample preparation method for the analysis of some organophosphorus pesticides residues in tomato by ultrasound-assisted solvent extraction followed by dispersive liquid-liquid microextraction. Food Chem 126:1840–1844

    Article  CAS  Google Scholar 

  • Blasco C, Masia A, Gabriel-Morillas F, Pico Y (2011) Comparison of the effectiveness of recent extraction procedures for antibiotic residues in bovine muscle tissues. J AOAC Int 94(3):991–1000

    CAS  Google Scholar 

  • Boyd-Boland AA, Pawliszyn JB (1995) Solid-phase microextraction of nitrogen-containing herbicides. J Chromatogr A 704:163–172

    Article  CAS  Google Scholar 

  • Castillo M, González C, Miralles A (2011) An evaluation method for determination of non-polar pesticide residues in animal fat samples by using dispersive solid-phase extraction clean-up and GC-MS. Anal Bioanal Chem 400:1315–1328

    Article  CAS  Google Scholar 

  • Cervera MI, Portolés T, Pitarch E, Beltrán J, Hernández F (2012) Application of gas chromatography time-of-flight mass spectrometry for target and non-target analysis of pesticide residues in fruits and vegetables. J Chromatogr A 1244:168–177

    Article  CAS  Google Scholar 

  • Chen GQ, Cao PY, Liu RJ (2011) A multi-residue method for fast determination of pesticides in tea by ultra performance liquid chromatography-electrospray tandem mass spectrometry combined with modified QuEChERS sample preparation procedure. Food Chem 125:1406–1411

    Article  CAS  Google Scholar 

  • Chen Y, Al-Taher F, Juskelis R, Wong JW, Zhang K, Hayward DG, Zweigenbaum J, Stevens J, Cappozzo J (2012) Multiresidue pesticide analysis of dried botanical dietary supplements using an automated dispersive SPE cleanup for QuEChERS and high performance liquid chromatography-tandem mass spectrometry. J Agric Food Chem 60(40):9991–9999

    Article  CAS  Google Scholar 

  • Cherta L, Beltran J, López FJ, Hernández F (2013) Application of fast gas chromatography–mass spectrometry in combination with the QuEChERS method for the determination of pesticide residues in fruits and vegetables. Food Anal Methods 6(4):1170–1187

    Article  Google Scholar 

  • Cheung LM, Cheung PCK, Ooi VEC (2003) Antioxidant activity and total phenolics of edible mushroom extracts. Food Chem 81:249–255

    Article  CAS  Google Scholar 

  • Cortés-Aguado S, Sánchez-Morito N, Arrebola FJ, Frenich AG, Vidal JLM (2008) Fast screening of pesticide residues in fruit juice by solid-phase microextraction and gas chromatography–mass spectrometry. Food Chem 107:1314–1325

    Article  CAS  Google Scholar 

  • European Parliament and Council (2005) Regulation (EC) No 396/2005 of the European Parliament and of the Council of 23 February 2005 onmaximum residue levels of pesticides in or on food and feed of plant and animal origin and amending Council Directive 91/414/EEC

  • European Commission (2013) Guidance document on analytical quality control and validation procedures for pesticide residues analysis in food and feed. SANCO/12571

  • Gómez-Ramos MM, Ferrer C, Malato O, Agüera A, Fernández-Alba AR (2013) Liquid chromatography-high-resolution mass spectrometry for pesticide residue analysis in fruit and vegetables: screening and quantitative studies. J Chromatogr A 1287:24–37

    Article  CAS  Google Scholar 

  • González-Curbelo MÁ, Hernández-Borges J, Borges-Miquel TM, Rodríguez-Delgado MÁ (2011) Determination of pesticides and their metabolites in processed cereal samples. Food Addit Contam Part A 29(1):104–116

    Article  CAS  Google Scholar 

  • Guan YQ, Tang H, Chen DZ, Xu T, Li L (2013) Modified QuEChERS method for the analysis of 11 pesticide residues in tea by liquid chromatography-tandem mass spectrometry. Anal Methods 5(12):3056–3067

    Article  CAS  Google Scholar 

  • Hercegova A, Domotorova M, Matisova E (2007) Sample preparation methods in the analysis of pesticide residues in baby food with subsequent chromatographic determination. J Chromatogr A 1153:54–73

    Article  CAS  Google Scholar 

  • Hu YY, Zheng P, He YZ, Sheng GP (2005) Response surface optimization for determination of pesticide multiresidues by matrix solid phase dispersion and gas chromagatography. J Chromatogr A 1098(1–2):188–193

    Article  CAS  Google Scholar 

  • Kanrar B, Mandal S, Bhattacharyya A (2010) Validation and uncertainty analysis of a multiresidue method for 42 pesticides in made tea, tea infusion and spent leaves using ethyl acetate extraction and liquid chromatography–tandem mass spectrometry. J Chromatogr A 1926–1933

  • Kinsella B, O’Mahony J, Malone E, Moloney M, Cantwell H, Furey A, Danaher M (2009) Current trends in sample preparation for growth promoter and veterinary drug residue analysis. J Chromatogr A 1216:7977–8015

    Article  CAS  Google Scholar 

  • Kolberg DI, Prestes OD, Adaime MB, Zanella R (2011) Development of a fast multiresidue method for the determination of pesticides in dry samples (wheat grains, flour and bran) using QuEChERS based method and GC–MS. Food Chem 125:1436–1442

    Article  CAS  Google Scholar 

  • Kuang H, Miao H, Hou XL, Zhao YF, Shen JZ, Wu YN (2010) Determination of enantiometric fractions of cypermethrin and cis-bifenthrin in Chinese teas by GC/ECD. J Sci Food Agric 90:1374–1379

    Article  CAS  Google Scholar 

  • Lazartigues A, Wiest L, Baudot R, Thomas M, Feidt C, Cren-Olive C (2011) Multiresidue method to quantify pesticides in fish muscle by QuEChERS-based extraction and LC-MS/MS. Anal Bioanal Chem 400:2185–2193

    Article  CAS  Google Scholar 

  • Le Doux M (2011) Analytical methods applied to the determination of pesticide residues in foods of animal origin. A review of the past two decades. J Chromatogr A 1218:1021–1036

    Article  CAS  Google Scholar 

  • Lee JM, Park JW, Jang GC, Hwang KJ (2008) Comparative study of pesticide multi-residue extraction in tobacco for gas chromatography–triple quadrupole mass spectrometry. J Chromatogr A 1187:25–33

    Article  CAS  Google Scholar 

  • Lehotay SJ, Son KA, Kwon H, Koesukwiwat U, Fu WS, Mastovska K, Hoh E, Leepipatpiboon N (2010) Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables. J Chromatogr A 1217(16):2548–2560

    Article  CAS  Google Scholar 

  • Li N, Lei L, Nian L, Zhang R, Wu ST, Ren RB, Wang YQ, Zhang HQ, Yu AM (2013) A modified QuEChERS method for the determination of some herbicides in yogurt and milk by high performance liquid chromatography. Talanta 105:219–228

    Article  CAS  Google Scholar 

  • Surma MK, Sadowska-Rociek AB, Cieślik EJ (2014) Evaluation of the QuEChERS method with GC-MS detection for the determination of organochlorine pesticides in food of animal origin. Food Anal Methods 7(2):366–376

    Article  Google Scholar 

  • Magdic S, Boyd-Boland A, Jinno K, Pawliszyn JB (1996) Analysis of organophosphorus insecticides from environmental samples using solid-phase microextraction. J Chromatogr A 736:219–228

    Article  CAS  Google Scholar 

  • Pizzutti IR, De Kok A, Zanellar et al (2000) Method validation for the analysis of 169 pesticides in soya grain, without clean up, by liquid chromatography-tandem mass spectrometry using positive and negative electrospray ionization. J Chromatogr A 1142:123–136

    Article  CAS  Google Scholar 

  • Ru-zhen Y, Jin-hua W, Ming-lin W, Rong Z, Xiao-yu L, Wie-hua L (2011) Dispersive solid-phase extraction cleanup combined with accelerated solvent extraction for the determination of carbamate pesticide residues in Radix glycyrrhizae samples by UPLC-MS-MS. J Chromatogr Sci 49:702–708

    Article  Google Scholar 

  • Santilio A, Stefanelli P, Girolimetti S, Dommarco R (2011) Determination of acidic herbicides in cereals by QuEChERS extraction and LC/MS/MS. J Environ Sci Health B 46(6):535–543

    CAS  Google Scholar 

  • Shengliang Y, Yang G, Meng F (2007) Determination of 36 pesticide residues in mushroom by gel permeation chromatography and gas chromatography-tandem mass spectrometry. Chin J Chromatogr 25(4):581–585

    Google Scholar 

  • Venkateswarlu P, Mohan KR, Kumar CR et al (2007) Monitoring of multi-class pesticide residues in fresh grape samples using liquid chromatography with electrospray tandem mass spectrometry. Food Chem 105(4):1760–1766

    Article  CAS  Google Scholar 

  • Wilkowska A, Biziuk M (2011) Determination of pesticide residues in food matrices using the QuEChERS methodology. Food Chem 125(3):803–812

    Article  CAS  Google Scholar 

  • Xingqiang W, Xusheng G, Shuxuan L, Hanwen S (2014) A highly sensitive method for the determination of thiophanate methyl, cyromazine, and their metabolites in edible fungi by ultra-performance liquid chromatography using accelerated solvent extraction and cleanup with solid-phase extraction. Food Anal Methods 7:774–782

    Article  Google Scholar 

  • Zhang JM, Wu YL, Lu YB (2013) Simultaneous determination of carbamate insecticides and mycotoxins in cereals by reversed phase liquid chromatography tandem mass spectrometry using a quick, easy, cheap, effective, rugged and safe extraction procedure. J Chromatogr B 915–916:13–20

    Article  CAS  Google Scholar 

  • Zhao PY, Wang L, Jiang YP, Zhang FZ, Pan CP (2012a) Dispersive cleanup of acetonitrile extracts of tea samples by mixed multiwalled carbon nanotubes, primary secondary amine, and graphitized carbon black sorbents. J Agric Food Chem 60:4026–4033

    Article  CAS  Google Scholar 

  • Zhao PY, Wang L, Luo JH, Pan CP (2012b) Determination of pesticide residues in complex matrices using multi-walled carbon nanotubes as reversed-dispersive solid phase extraction sorbent. J Sep Sci 35:153–158

    Article  CAS  Google Scholar 

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Acknowledgments

This work was supported by the Health Science and Technology development plan of Jinan City (2014-50).

Conflict of Interest

Cao Xiaoli has no conflict of interest. Yang Xiaoqian has no conflict of interest. Liu Zhong has no conflict of interest. Liu Suhua has no conflict of interest. Liu Lanzheng has no conflict of interest. This article does not contain any studies with human or animal subjects.

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Authors and Affiliations

  1. Jinan Municipal Center for Disease Control and Prevention, Jinan, 250021, Shandong, China

    Xiaoli Cao, Suhua Liu, Xiaoqian Yang, Zhong Liu & Lanzheng Liu

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  1. Xiaoli Cao
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  2. Suhua Liu
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  3. Xiaoqian Yang
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  4. Zhong Liu
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  5. Lanzheng Liu
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Correspondence to Lanzheng Liu.

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Cao, X., Liu, S., Yang, X. et al. A Modified QuEChERS Sample Preparation Method for Simultaneous Determination of 62 Pesticide Residues in Edible Fungi Using Gas Chromatography–Triple Quadrupole Mass Spectrometry. Food Anal. Methods 9, 263–274 (2016). https://doi.org/10.1007/s12161-015-0200-0

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