Citation: LI Fuqin, SHI Lihong, WANG Fei, SUN Caiyuan, KANG Di, ZHANG Yuping, CHEN Lingzhu, HU Deyu. Simultaneous determination of pyraclostrobin and thiophanate-methyl and its metabolite carbendazim residues in soil and citrus by QuEChERS-liquid chromatography- tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2017, 35(6): 620-626. doi: 10.3724/SP.J.1123.2017.01031 shu

Simultaneous determination of pyraclostrobin and thiophanate-methyl and its metabolite carbendazim residues in soil and citrus by QuEChERS-liquid chromatography- tandem mass spectrometry

Research and Development Center for Fine Chemicals, State Key Laboratory of Green Pesticide and Agricultural Bioengineering, Ministry of Education, Guizhou University, Guiyang 550025, China

Received Date: 22 January 2017

Fund Project: Guizhou University Graduate Student Innovation Fund (No. 2016077).

A QuEChERS-liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the determination of pyraclostrobin, thiophanate-methyl and its metabolite carbendazim in soil and citrus. The samples were extracted with methanol or acetonitrile, purified by primary secondary amine (PSA), then separated by LC, detected in multiple reaction monitoring (MRM) mass spectrometry mode via positive electrospray ionization. The analytes were quantified by matrix-matched standard solutions with external standard method. The limits of quantification (LOQs) of pyraclostrobin, thiophanate-methyl and carbendazim in different matrices were 5.8-7.0 μg/kg, 9.3-14.1 μg/kg and 2.1-2.6 μg/kg, respectively. For all the samples, the spiked recoveries ranged from 75.48% to 109.18%, and the relative standard deviations (RSDs) were 0.60%-5.11% (n=5). The method is quick, easy, effective, sensitive and accurate. The matrix-matched calibration solutions can efficiently compensate matrix effects of the pyraclostrobin, thiophanate-methyl and carbendazim in LC-MS/MS analysis. The established method can be applied to the residue analysis of the real samples of soil, citrus peel, citrus pulp and citrus fruits.
- liquid chromatography-tandem mass spectrometry (LC-MS/MS),
- QuEChERS,
- pyraclostrobin,
- thiophanate-methyl,
- carbendazim,
- soil,
- citrus
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