固相微萃取-气相色谱-串联质谱法检测水中克菌丹残留量

Determination of Captan Residues in Water Samples by Solid Phase Micro-Extraction Coupled with Gas Chromatography-Mass Spectrometry

建立了环境水样中克菌丹残留量的固相微萃取-气相色谱-串联质谱联用(SPME-GC-MS/MS)检测方法.通过优化固相微萃取的条件对水样中的克菌丹进行富集,分析结果表明克菌丹在0.10~5.00 mg/L的质量浓度范围内线性关系良好,相关系数r2大于0.99,对农田灌溉水进行加标回收率试验,测定的低、中、高3种不同添加浓度的平均回收率分别为75.7%、79.1%和83.1%,相对标准偏差(RSD)在2.0%~3.4%范围内,检出限(LOD)为7.98μg/L.与传统溶剂萃取农药残留的方法相比,具有前处理简便、无溶剂污染等优点,同时方法准确度和精密度较好,可作为环境水样中克菌丹残留量的监测.

A novel method has been developed for the determination of captan in water samples by solid phase micro-extraction（SPME） coupled with gas chromatography-mass spectrometry （GC-MS/MS）. Some important parameters affecting the extraction efficiency of SPME were studied and optimized. Under optimum conditions, the results showed that the linear range for the determination was 0.10~5.00 mg/L, and the correlation coefficient r2 was greater than 0.99. The spiked recovery test was performed on farm irrigation water samples, and the low, medium and high spiked concentrations were determined. The average recoveries were 75.7%, 79.1%, and 83.1%, respectively, with the relative standard deviation（RSD） between 2.0% and 3.4%. The limit of detection（LOD） was 7.98 μg/L. The captan residues in water samples were successfully analyzed by the proposed method with satisfactory results.