采用液液萃取和气相色谱 - 质谱联用技术对水果、蔬菜和土壤中的醚菌酯和啶酰菌胺进行残留分析。

Residue analysis of kresoxim-methyl and boscalid in fruits, vegetables and soil using liquid-liquid extraction and gas chromatography-mass spectrometry.

作者信息

Liu Xingang, Dong Fengshou, Qin Dongmei, Zheng Yongquan

机构信息

Key Laboratory of Pesticide Chemistry and Application, Ministry of Agriculture, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing, China.

出版信息

Biomed Chromatogr. 2010 Apr;24(4):367-73. doi: 10.1002/bmc.1301.

DOI:10.1002/bmc.1301

PMID:19650146

Abstract

A GC-MS procedure for simultaneously determining and validating kresoxim-methyl and boscalid has been developed in fruit, vegetable and soil matrices. The method was based on one-step liquid-liquid extraction with acetone and dichloromethane solvents. Estimated limits of detection (LODs) for kresoxim-methyl and boscalid were 0.006 and 0.015 mg/kg, and limits of quantification (LOQs) were 0.02 and 0.05 mg/kg, respectively. The intra- and inter- precision were achieved with RSD better than 13.8 and 14.5%, and recoveries were in the range of 77.1-98.7% for kresoxim-methyl and 72.8-105.1% for boscalid. The expanded uncertainties calculated at 0.1 mg/kg were below 18%. Concentration levels for residues of the two fungicides in melon samples from field trials collected 7 days after the last application were clearly below the established MRL values.

摘要

已开发出一种气相色谱-质谱联用（GC-MS）方法，用于同时测定和验证水果、蔬菜及土壤基质中的醚菌酯和啶酰菌胺。该方法基于用丙酮和二氯甲烷溶剂进行一步液液萃取。醚菌酯和啶酰菌胺的估计检测限（LOD）分别为0.006和0.015 mg/kg，定量限（LOQ）分别为0.02和0.05 mg/kg。日内和日间精密度的相对标准偏差（RSD）均优于13.8%和14.5%，醚菌酯的回收率在77.1 - 98.7%范围内，啶酰菌胺的回收率在72.8 - 105.1%范围内。在0.1 mg/kg计算的扩展不确定度低于18%。在最后一次施药7天后采集的田间试验甜瓜样品中，两种杀菌剂残留的浓度水平明显低于既定的最大残留限量（MRL）值。