加速溶剂萃取/气相色谱-负化学电离质谱法对土壤中毒杀芬的测定研究

建立了加速溶剂萃取/气相色谱-负化学电离质谱法测定土壤中毒杀芬的方法.在加速溶剂萃取实验条件优化的基础上,确定了最佳实验条件:系统压力12.4 MPa,萃取溶剂为正己烷-丙酮(体积比1 : 1),萃取温度100 ℃,静态萃取时间10 min,循环2次.萃取液经活性炭与弗罗里硅土复合小柱净化后,氮吹至1.0 mL,于GC-MS仪上测定.结果表明,毒杀芬的线性范围为0.3 ～3 000 ng/g(毒杀芬总量),相关系数均不小于0.999 0,方法检出限为0.10 ～1.00 ng/g,平均回收率为86% ～104%,相对标准偏差(n=7)为6.8% ～13.5%.

Detection of Toxaphene in Soil by Accelerated Solvent Extraction/GC-NCI MS

A method has been developed for the determination of toxaphene in soil by gas chromatography-negative chemical ionization mass spectrometry(GC-NCI MS) with accelerated solvent extraction(ASE).The experimental conditions were investigated on the basis of the optimization of ASE conditions,and the optimal conditions were obtained as follows: extraction solvent: hexane-actone(1 : 1,by volume),system pressure:12.4 MPa,extraction temperature:100 ℃,extraction time :10 min,cycling twice.The extract was cleaned up by passing through Cleanert PestiCarb and florisil solid phase extraction cartridge.The elute was evaporated to dryness under nitrogen to 1.0 mL and the quantitative analysis of toxaphene was performed by GC-MS.The linear range was 0.3-3 000 ng/g for the total toxaphene),the detection limits of toxaphene ranged from 0.10 to 1.00 ng/g,and the spiked standard recoveries were between 86% and 104% with the relative standard deviations ranging from 6.8% to 13.5%(n=7).The method is accurate,simple,and rapid,and adapts for inspection of toxaphene in soil.