唑草酮在水稻和稻田中的气相色谱检测

Determination of herbicide carfentrazone-ethyl residues in rice and paddy with a gas chromatograph-election capture detector

为建立水稻和稻田中除草剂唑草酮的气相色谱检测方法,开展试验。糙米、稻壳、水稻茎秆和土壤中的唑草酮残留物采用丙酮/水提取,石油醚萃取,弗罗里硅土柱净化后,乙酸乙酯洗脱,正己烷定容后采用气相色谱检测;稻田水样品经过滤后石油醚萃取,弗罗里硅土柱净化后,乙酸乙酯洗脱,正己烷定容后采用气相色谱检测。所有样品均采用外标法定量。结果表明:唑草酮在糙米中的添加回收率为88.7%～102.8%,变异系数3.0%～5.4%;在稻壳中的添加回收率为84.7%～93.5%,变异系数2.0%～5.3%;在水稻茎秆中的添加回收率为81.1%～91.6%,变异系数1.9%～7.0%;在稻田土壤中的添加回收率为83.0%～92.4%,变异系数4.0%～7.6%;在稻田水中的添加回收率为90.9%～100.5%,变异系数3.3%～4.3%。该检测方法具有操作简单、灵敏度高、净化效果好等特点,能够满足水稻、稻田土壤和水样品中唑草酮的残留检测。

In this study,carfentrazone-ethyl was extracted from the samples of brown rice,rice hull,stem and paddy soil by acetone/water,extracted by petroleum ether,cleaned up with florisil column,eluted by ethyl acetate,and then detected by a gas chromatograph-election capture detector（GC-ECD）.Carfentrazone-ethyl was extracted from paddy water by petroleum ether,cleaned up with florisil column,eluted by ethyl acetate,and then detected by GC-ECD.The results showed that the recovery rate of carfentrazone-ethyl in brown rice was 88.7%-102.8%（RSD 3.0%-5.4%）,in rice hull was 84.7%-93.5%（RSD 2.0%-5.3%）,in stem was 81.1%-91.6%（RSD 1.9%-7.0%）,in paddy soil was 83.0%-92.4%（RSD 4.0%-7.6%）,in paddy water was 90.9%-100.5%（RSD 3.3%-4.3%）.This method was proved to be easy in operation,high in sensitivity and effective in purification,and was reliable to determine carfentrazone-ethyl herbicides residues in rice and paddy field.