Determination of 27 new fungicides in cereals, vegetables and fruits by dispersive solid phase extraction and liquid chromatography-tandem mass spectrometry

doi:10.3724/SP.J.1123.2016.12040

Abstract

Abstract:

A method for simultaneous determination of 27 new fungicides in cereals, vegetables and fruits using dispersive solid phase extraction and liquid chromatography-tandem mass spectrometry (DSPE-LC-MS/MS) was developed. Samples were extracted with acetone containing 1% (v/v) acetic acid, purified by a mixed sorbent of ethylenediamine-N-propylsilane (PSA), C18, anhydrous magnesium sulfate (MgSO₄) and multi-walled carbon nanotubes (MWCNT), separated by a reversed phase C18 column, and gradiently eluted with acetonitrile and 0.1% (v/v) formic acid solution (containing 5 mmol/L ammonium acetate). Anhydrous magnesium sulfate was used as a dewatering agent. The positive ion mode and multiple reaction monitoring (MRM) mode were used in the analysis, and the analytes were quantified by external standard method. Thifluzamide and triclopyricarbe showed good linearities in the range of 20.47-200 μg/kg, and the limits of detection (LODs) and the limits of quantification (LOQs) were 6.15-16.67 and 20.47-55.5 μg/kg, respectively. The other 25 new fungicides showed good linearities in the range of 0.02-100 μg/kg, and the LODs and LOQs were 0.006-4.44 and 0.02-14.79 μg/kg, respectively. The linear relative coefficients were not less than 0.9950. The recoveries were in the range of 70.02%-117.6% and the relative standard deviations (RSDs) ranged from 0.01% to 19.62% (n=3). The method has the advantages of simplicity, rapidity, high sensitivity and better purification effect. It is suitable for the rapid determination of the 27 new fungicides in cereals, vegetables and fruits.

Key words: cereals, dispersive solid phase extraction (DSPE), fruits, liquid chromatography-tandem mass spectrometry (LC-MS/MS), new fungicide, vegetables

CLC Number:

O658

CUI Chunyan, ZHANG Hongyi, WU Xingqiang, FAN Chunlin, LI Shuai, CHEN Hui, CHANG Qiaoying, PANG Guofang. Determination of 27 new fungicides in cereals, vegetables and fruits by dispersive solid phase extraction and liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2017, 35(5): 487-494.

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