Chinese Journal of Chromatography

Chinese Journal of Chromatography ›› 2018, Vol. 36 ›› Issue (4): 339-344.DOI: 10.3724/SP.J.1123.2017.10027

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Determination of spirotetramat and its four metabolites in citrus by ultra-high performance liquid chromatography-triple quadrupole-ion trap mass spectrometry

XU Cheng1,2, ZHANG Shenghu2, ZHANG Yi2, PU Yuepu1, YIN Lihong1, ZHANG Juan1, SONG Ninghui2   

  1. 1. Key Laboratory of Environmental Medicine Engineering of Ministry of Education, School of Public Health, Southeast University, Nanjing 210000, China;
    2. Nanjing Institute of Environmental Sciences, Ministry of Environmental Protection, Nanjing 210042, China
  • Received:2017-10-27 Online:2018-04-08 Published:2014-02-26
  • Supported by:

    Ministry of Education Key Laboratory of Environmental Medicine Engineering Open Project Fund (No. 2017EME001).

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Abstract:

A method for the simultaneous determination of spirotetramat and its four metabolites in citrus was developed by ultra-high performance liquid chromatography-triple quadrupole-ion trap mass spectrometry (UPLC-Q TRAP MS).The samples were extracted with acetonitrile and purified by QuEChERS pretreatment.The extracts were detected using an electrospray ionization (ESI) positive ion source under multiple reaction monitoring (MRM) mode, and quantified by matrix matching external standard method.The results showed that spirotetramat and its four metabolites had good linearities in the range of 2-1000 μg/L with correlation coefficients (R2) greater than 0.99.The limits of detection (LODs) of spirotetramat and its four metabolites were in the range of 0.08 to 0.49 μg/kg, while the limits of quantification (LOQ) were in the range of 0.26 to 1.62 μg/kg.The average spiked recoveries were in the range of 94.0% to 98.70%, and the relative standard deviations were 1.1%-5.3%.The results from field trials showed that the contents of the final residues of spirotetramat and its four metabolites in the flesh, peel and whole fruit samples were 5.93-14.20, 11.30-17.86 and 1.30-16.51 μg/kg with the highest recommended dose of 60 mg/kg (active ingredient).The residues in harvested citrus were lower than the national standard maximum residue limit (1.00 mg/kg).The method is simple, rapid and accurate, with a high sensitivity and good separation effect, and the effect of matrix interference can be effectively reduced.The accuracy and precision of this method can meet the requirements of quantitative analysis.The method is suitable for the qualitative and quantitative detection of spirotetramat and its four metabolites in citrus.

Key words: citrus, QuEChERS, spirotetramat and its metabolites, ultra-high performance liquid chromatography-triple quadrupole-ion trap mass spectrometry (UPLC-Q TRAP MS)

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