Citation: CHEN Xiaolong, LI Zhengxiang, CAO Zhaoyun, GONG Jiadi, CAO Xiaolin, CHEN Mingxue. Determination of six novel amide fungicides in vegetables and fruits by liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2013, 31(10): 954-960. doi: 10.3724/SP.J.1123.2013.04028 shu

Determination of six novel amide fungicides in vegetables and fruits by liquid chromatography-tandem mass spectrometry

1.
Rice Product Quality Inspection and Supervision Center of Ministry of Agriculture, China National Rice Research Institute, Hangzhou 310006, China

Corresponding author: CHEN Mingxue,
Received Date: 17 April 2013
Available Online: 31 May 2013
Fund Project: 浙江省级重点科技创新团队项目(2012R10028-05). (2012R10028-05)

A method was developed for the simultaneous determination of mepanipyrim, silthiofam, boscalid, fluopicolide, mandipropamid, cyflufenamid in vegetables and fruits by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The analytes were extracted from the samples by acetonitrile and purified by Florisil SPE. The six novel amide fungicides were separated on a Poroshell 120 EC-C₁₈ column with the mobile phases of water and acetonitrile, and finally detected by MS/MS with positive electrospray ionization (ESI⁺) in multiple reaction monitoring (MRM) mode, quantified by external standard method. Under the optimal analytical conditions, the correlation coefficients (r) of the six novel amide fungicides were not lower than 0.9990 in the concentration range from 0.5 to 100 μg/L. The limits of detection (S/N≥3) of the method were 0.15 μg/kg for boscalid, silthiofam, mandipropamid, cyflufenamid, 0.10 μg/kg for mepanipyrim and 0.17 μg/kg for fluopicolide. The recovery tests were performed for the 7 types of vegetables and the 3 types of fruits at the spiked levels of 0.5, 5 and 50 μg/kg, and the recoveries of the six analytes ranged from 65% to 124% with the relative standard deviations (RSDs, n=5) of 1%-18%. The matrix effects in vegetables and fruits of the six amide fungicides were significantly reduced by the purification of Florisil SPE compared with the modified QuEChERS. The method is easy, fast, sensitive and accurate, and can meet the requirements of the determination of the six amide fungicide residues in vegetables and fruits.
- liquid chromatography-tandem mass spectrometry (LC-MS/MS),
- amide fungicides,
- vegetables,
- fruits
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沈阳化工大学材料科学与工程学院沈阳 110142