加压流体萃取/气相色谱法测定固体废物中甲胺磷

Determination of Methamidophos in Soild Waste by Accelerated Solvent Extraction/Gas Chromatography

建立了加压流体萃取/气相色谱法测定固体废物中甲胺磷的方法,具体操作为取10 g新鲜固体废物,以丙酮-二氯甲烷(4+1)为萃取溶剂,萃取温度为80℃,进行加压流体萃取,萃取液经无水硫酸钠脱水,旋转蒸发浓缩,进入气相色谱仪检测,结果表明,甲胺磷的线性范围为50~1000μg/L,相关系数为0.9998。以石英砂作为空白试样,添加高、中、低浓度甲胺磷标准物质,测定相对标准偏差(RSD,n=6)在2.7%~4.7%,加标回收率在75.9%~94.3%。以杭州某农药厂产生的固体废物为试样,添加高、中、低浓度甲胺磷标准物质,测定相对标准偏差(RSD,n=6)在2.3%~4.4%,加标回收率在73.1%~90.5%。

A method for the determination of methamidophos in solid waste by pressurized fluid extraction and gas chromatography was established.10 g fresh solid waste was extracted with acetone-dichloromethane(4+1)as the extraction solvent at 80℃by pressurized fluid extraction.The extraction solution was dehydrated by anhydrous sodium sulfate and concentrated by rotary evaporation.In accordance with results,it showed that the linear range of methamidophos was 50-1000μg/L,and the correlation coefficient was 0.9998.Taking quartz sand as blank sample,high,medium and low concentrations of methamidophos were added and found the relative standard deviations(RSD,n=6)of methamidophos were in the range of 2.7%-4.7%,and the recoveries were in the range of 75.9%-94.3%.Taking solid waste from an agricultural pharmaceutical factory in Hangzhou as sample,high,medium and low concentrations of methamidophos were added and found the relative standard deviations(RSD,n=6)of methamidophos were in the range of 2.3%-4.4%,and the recoveries were in the range of 73.1%-90.5%.