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Simultaneous Determination of Isofetamid and Its Two Metabolites in Fruits and Vegetables Using Ultra-Performance Liquid Chromatography with Tandem Mass Spectrometry

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Abstract

In this paper, an efficient analytical method for the simultaneous determination of a new fungicide (isofetamid) and its two metabolites in fruits and vegetables was developed using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) pretreatment method and ultra-performance liquid chromatography-tandem mass spectrometry. The three compounds were extracted with acetonitrile and cleaned up using primary secondary amine, octadecylsilane, and graphitized carbon black. The three analytes were well separated with good specificity using an electrospray ionization source in positive mode within 5.0 min. The mean recoveries in apple, strawberry, grape, tomato, cucumber, and lettuce for the three target compounds at different levels ranged from 74 to 107%, with relative standard deviations lower than 12.3%. The method showed excellent linearity (R2 ≥ 0.9946) for the three compounds. The limits of quantification of isofetamid and its metabolites were 1 μg kg−1 in apple, tomato, and cucumber and 100 μg kg−1 in strawberry, grape, and lettuce. The proposed method was successfully applied to a residue dynamic experiment, and it can be considered a strong alternative method to monitor the residues of isofetamid and its metabolites simultaneously in fruits and vegetables.

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References

  • 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 86:412–431

    CAS  PubMed  Google Scholar 

  • Avenot HF, Michailides TJ (2010) Progress in understanding molecular mechanisms and evolution of resistance to succinate dehydrogenase inhibiting (SDHI) fungicides in phytopathogenic fungi. Crop Protect 29:643–651

    Article  CAS  Google Scholar 

  • Cabrera LC, Caldas SS, Prestes OD, Primel EG, Zanella R (2016) Evaluation of alternative sorbents for dispersive solid-phase extraction clean-up in the QuEChERS method for the determination of pesticide residues in rice by liquid chromatography with tandem mass spectrometry. J Sep Sci 39:1945–1954

    Article  CAS  Google Scholar 

  • Dong F, Chen X, Liu X, Xu J, Li Y, Shan W, Zheng Y (2012) Simultaneous determination of five pyrazole fungicides in cereals, vegetables and fruits using liquid chromatography/tandem mass spectrometry. J Chromatogr A 1262:98–106

    Article  CAS  PubMed  Google Scholar 

  • EFSA (European Food Safety Authority (2015)Conclusion on the peer review of the pesticide risk assessment of the active substance isofetamid. EFSA J 13(10):130, 4265. https://doi.org/10.2903/j.efsa.2015.4265

  • European Commission (2016) EU Pesticides database. http://ec.europa.eu/food/plant/pesticides/eu-pesticides-database/public/?event=pesticide.residue.CurrentMRL&language= EN&pestResidueId=2463#. Accessed 7 May 2018

  • Fava L, Orrù MA, Crobe A, Barra Caracciolo A, Bottoni P, Funari E (2005) Pesticide metabolites as contaminants of groundwater resources: assessment of the leaching potential of endosulfan sulfate, 2,6-dichlorobenzoic acid, 3,4-dichloroaniline, 2,4-dichlorophenol and 4-chloro-2-methylphenol. Microchem J 79:207–211

    Article  CAS  Google Scholar 

  • Jiang C-H, Liao M-J, Wang H-K, Zheng M-Z, Xu J-J, Guo J-H (2018) Bacillus velezensis, a potential and efficient biocontrol agent in control of pepper gray mold caused by Botrytis cinerea. Biol Control 126:147–157. https://doi.org/10.1016/j.biocontrol.2018.07.017

    Article  Google Scholar 

  • Kaczyński P (2017) Clean-up and matrix effect in LC-MS/MS analysis of food of plant origin for high polar herbicides. Food Chem 230:524–531. https://doi.org/10.1016/j.foodchem.2017.03.091

    Article  CAS  PubMed  Google Scholar 

  • Leroch M, Plesken C, Weber RWS, Kauff F, Scalliet G, Hahn M (2013) Gray Mold populations in German strawberry fields are resistant to multiple fungicides and dominated by a novel clade closely related to Botrytis cinerea. Appl Environ Microbiol 79:159–167. https://doi.org/10.1128/AEM.02655-12

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  • Li Y, Liu X, Wu X, Dong F, Xu J, Zheng Y (2016) Simultaneous determination of flupyradifurone and its two metabolites in fruits, vegetables, and grains by a modified quick, easy, cheap, effective, rugged, and safe method using ultra high performance liquid chromatography with tandem mass spectrometry. J Sep Sci 39:1090–1098

    Article  CAS  PubMed  Google Scholar 

  • Núñez O, Moyano E, Galceran MT (2005) LC–MS/MS analysis of organic toxics in food. Trends Anal Chem 24:683–703

    Article  CAS  Google Scholar 

  • Payá P, Anastassiades M, Mack D, Sigalova I, Tasdelen B, Oliva J, Barba A (2007) Analysis of pesticide residues using the quick easy cheap effective rugged and safe (QuEChERS) pesticide multiresidue method in combination with gas and liquid chromatography and tandem mass spectrometric detection. Anal Bioanal Chem 389:1697–1714

    Article  CAS  PubMed  Google Scholar 

  • Piqueras CM, Latorre BA, Torres R (2014) Effectiveness of isofetamid, a new succinate dehydrogenase inhibitor fungicide, in the control of grapevine gray mold. Cienc Investig Agrar 41:17–18

  • Qiu SS, Bai YL (2015) Progress on Research and Development of succinate dehydrogenase inhibitor fungicides(II). Mod Agrochem. https://doi.org/10.3969/j.issn.1671-5284.2014.06.001

  • Rainville PD, Plumb RS (2010). Increasing bioanalytical assay sensitivity for low exposure compounds with Xevo TQ-S. http://www.waters.com/webassets/cms/library/docs/720003419en.pdf. Accessed 21 Aug 2018

  • Ribeiro Begnini Konatu F, Sales Fontes Jardim IC (2018) Development and validation of an analytical method for multiresidue determination of pesticides in lettuce using QuEChERS–UHPLC–MS/MS. J Sep Sci 41:1726–1733

    Article  CAS  PubMed  Google Scholar 

  • Rubert J, Soler C, Mañes J (2010) Optimization of matrix solid-phase dispersion method for simultaneous extraction of aflatoxins and OTA in cereals and its application to commercial samples. Talanta 82:567–574

    Article  CAS  PubMed  Google Scholar 

  • Shim CK, Kim MJ, Kim YK, Jee HJ (2014) Evaluation of lettuce germplasm resistance to gray Mold disease for organic cultivations. Plant Pathol J 30:90–95

    Article  PubMed  PubMed Central  Google Scholar 

  • Szpyrka E, Kurdziel A, Matyaszek A, Podbielska M, Rupar J, Słowik-Borowiec M (2015) Evaluation of pesticide residues in fruits and vegetables from the region of South-Eastern Poland. Food Control 48:137–142. https://doi.org/10.1016/j.foodcont.2014.05.039

    Article  CAS  Google Scholar 

  • Tsukuda S (2014) Developing trend of SDHI fungicide and studies on a novel fungicide, isofetamid. Jpn J Pestic Sci 39:89–95

    Article  CAS  Google Scholar 

  • Walorczyk S (2014) Validation and use of a QuEChERS-based gas chromatographic–tandem mass spectrometric method for multiresidue pesticide analysis in blackcurrants including studies of matrix effects and estimation of measurement uncertainty. Talanta 120:106–113

    Article  CAS  PubMed  Google Scholar 

  • Wu X, Yu Y, Xu J, Dong F, Liu X, du P, Wei D, Zheng Y (2017) Residue analysis and persistence evaluation of fipronil and its metabolites in cotton using high-performance liquid chromatography-tandem mass spectrometry. PLoS One 12:e0173690

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  • Yan Y, Zhang S, G-j T, You F-h, Chen J, M-m Z (2017) Acetonitrile extraction coupled with UHPLC–MS/MS for the accurate quantification of 17 heterocyclic aromatic amines in meat products. J Chromatogr B 1068-1069:173–179. https://doi.org/10.1016/j.jchromb.2017.10.015

    Article  CAS  Google Scholar 

  • You X, Sui C, Li Y, Wang X (2017) Simultaneous determination of pyrifluquinazon and its main metabolite in fruits and vegetables by using QuEChERS–HPLC–MS/MS. J Sep Sci 40:702–708

    Article  CAS  PubMed  Google Scholar 

  • Zhang Y, Wu X, Duan T, Xu J, Dong F, Liu X, Li X, du P, Zheng Y (2018) Ultra high performance liquid chromatography with tandem mass spectrometry method for determining dinotefuran and its main metabolites in samples of plants, animal-derived foods, soil, and water. J Sep Sci 41:2913–2923

    Article  CAS  Google Scholar 

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Funding

This work was supported by The National Natural Science Foundation of China (31672062) and Technology Innovation Project from the Chinese Academy of Agricultural Sciences (CAAS-XTCX2016015).

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Authors and Affiliations

  1. State Key Laboratory for Biology of Plant Diseases and Insect Pests, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Yuanmingyuan West Road No. 2, Haidian District, Beijing, 100193, China

    Yanli Man, Xingang Liu, Fengshou Dong, Jun Xu, Xiaohu Wu & Yongquan Zheng

  2. Beijing Bayi School, No. 29 Suzhou Street Haidian District, Beijing, 100080, People’s Republic of China

    Yunxi Zheng

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  1. Yanli Man
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  2. Yunxi Zheng
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  3. Xingang Liu
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  4. Fengshou Dong
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  5. Jun Xu
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  6. Xiaohu Wu
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  7. Yongquan Zheng
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Correspondence to Xingang Liu.

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Yanli Man, Yunxi Zheng, Xingang Liu, Fengshou Dong, Jun Xu, Xiaohu Wu, and Yongquan Zheng declare that they have no conflict of interest.

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Man, Y., Zheng, Y., Liu, X. et al. Simultaneous Determination of Isofetamid and Its Two Metabolites in Fruits and Vegetables Using Ultra-Performance Liquid Chromatography with Tandem Mass Spectrometry. Food Anal. Methods 12, 1487–1496 (2019). https://doi.org/10.1007/s12161-019-01466-y

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