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| Determination of 25 Sulfonylurea Herbicides and Triazolopyrimidine Sulfonamides Herbi?cides in Aquatic Products by Ultra Perfor?mance Liquid Chromatography－Tandem Mass Spectrometry with Rapid Solid Phase Extraction |
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| DOI： |
| KeyWord:sulfonylurea herbicides triazolopyrimidine sulfonamides herbicides aquatic products ultra performance liquid chromatography－tandem mass spectrometry rapid solid phase extraction |
| Author | Institution |
| ZHU Fu-qiang， WU Shu-dong， HAN Yan-jun，GUO Yu-peng |
Binzhou Testing Center， Binzhou ， China |
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| Abstract: |
| A rapid and accurate analysis method based on rapid solid phase extraction and ultra performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS） was developed for the determination of 25 kinds of sulfonylurea herbicides and triazolopyrimidine sulfonamides herbicides in aquatic products. Firstly， the pretreatment conditions for the 25 pesticides in aquatic product samples were systematically optimized， based on recoveries， purification efficiencies and other factors， acetonitrile was used as the extraction solvent， and a SHIMSEN QVet－NM + rapid solid phase extraction cartridge was selected as the pretreatment purification column. Then， the chromatographic conditions and MS parameters were optimized. Finally， the chromatographic separation was performed on a Shim－pack GIST C18（2.1 mm × 50 mm × 2.0 μm） column under linear gradient elution using 0.1% formic acid solution and acetonitrile as the mobile phases. The 25 kinds of sulfonylurea herbicides and triazolopyrimidine sulfonamides herbicides were detected by triple quadrupole MS with electrospray ionization（ESI） in multiple reaction monitoring（MRM） mode under both positive and negative conditions， and quantified by a matrix-matched external standard method. The 25 herbicides showed good linear relationships in the concentration range of 0.20－50 μg/L with correlation coefficients（r2） greater than 0.994. The limits of detection（LOD） and limits of quantitation（LOQ） were in the ranges of 0.30－1.3 μg/kg and 1.2－5.0 μg/kg， respectively. The average recoveries for the analytes at three spiked levels varied from 62.7% to 122%， with the relative standard deviations（RSD） of 0.72%－18%. Results of the matrix effects（ME） for 25 herbicides showed that all of the herbicides exhibited matrix inhibition effects in grass carp， penaeus vannamei and meretrix meretrix. The matrix effects could be reduced by the matrix-matched standard curve method. The method was applied to the detection of 25 herbicides in aquatic product samples. None of them were found in the samples. The experimental results indicated that the proposed method was simple， quick， accurate and sensitive， and was suitable for the determination of 25 kinds of sulfonylurea herbicides and triazolopyrimidine sulfonamides herbicides in aquatic products. |
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