Citation: QIN Meiling, CHAI Shuangshuang, MA Youning, GAO Huanhuan, ZHANG Hantong, HE Qiao. Determination of pyriminobac-methyl and bispyribac-sodium residues in rice by liquid chromatography-tandem mass spectrometry based on QuEChERS[J]. Chinese Journal of Chromatography, ;2017, 35(7): 719-723. doi: 10.3724/SP.J.1123.2017.02032 shu

Determination of pyriminobac-methyl and bispyribac-sodium residues in rice by liquid chromatography-tandem mass spectrometry based on QuEChERS

Rice Product Quality Inspection and Supervision Center, Ministry of Agriculture, Laboratory of Quality and Safety Risk Assessment for Rice, Ministry of Agriculture, China National Rice Research Institute, Hangzhou 310006, China

Received Date: 27 February 2017

Fund Project: National Agricultural Product Quality Safety Risk Assessment Project (No.GJFP2016001001)

A method was developed for the determination of pyriminobac-methyl and bispyribac-sodium residues in rice by liquid chromatography-tandem mass spectrometry (LC-MS/MS) coupled with modified QuEChERS. The samples were extracted with acidified acetonitrile, and then purified by octadecylsilane bonded silica (C₁₈) adsorbents. The analytes were separated on a ZORBAX SB C₁₈ column through a gradient elution using 0.1% (v/v) aqueous formic acid aqueous containing 5 mmol/L ammonium acetate and acetonitrile as mobile phases. Positive electrospray ionization (ESI⁺) was used. Qualitative work was performed using selected dynamic multiple reaction monitoring (dynamic MRM) mode. Quantization was performed using external standard method. The results showed good linearities of pyriminobac-methyl and bispyribac-sodium with correlation coefficients (r²) not less than 0.996. The limits of detection (LODs) of the method were 0.8 μ g/kg for pyriminobac-methyl, and 3 μ g/kg for bispyribac-sodium. The mean spiked recoveries of pyriminobac-methyl and bispyribac-sodium at three spiked levels were 76.6%-85.6% and 73.0%-86.7%, respectively, and the relative standard deviations (RSDs) of pyriminobac-methyl and bispyribac-sodium were 0.9%-3.4% and 1.2%-5.5%, respectively. This method is simple, rapid, sensitive, and suitable for the simultaneous determination of pyriminobac-methyl and bispyribac-sodium in rice.
- QuEChERS,
- liquid chromatography-tandem mass spectrometry (LC-MS/MS),
- pyriminobac-methyl,
- bispyribac-sodium,
- rice
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