加速溶剂萃取/超高压液相色谱-质谱联用对土壤中甲胺磷的测定研究  

Detection of Methamidophos in Soil by Accelerated Solvent Extraction / Ultra Performance Liquid Chromatography-Mass Spectrometry

作　　者：张鸣珊[1] 李腾崖[1] 何书海[1] 梁焱 

机构地区：[1]海南省环境科学研究院海南省环境监测中心站,海南海口571158

出　　处：《分析测试学报》2016年第9期1195-1198,共4页Journal of Instrumental Analysis

摘　　要：建立了加速溶剂萃取/超高压液相色谱-质谱联用测定土壤中甲胺磷的方法。确定最佳萃取条件为：萃取溶剂为乙腈，萃取温度80 ℃，静态萃取时间10 min，循环2次。萃取液经旋转蒸发仪浓缩后，进超高压液相色谱-质谱分析，外标法定量,质谱定性。结果表明，甲胺磷的线性范围为3.15~1 050 μg/L，相关系数为0.999 1。低、中、高3个加标水平下甲胺磷的平均回收率为72%~82%，相对标准偏差为5.8%~8.6%，检出限为0.05 μg/kg。该方法具有良好的分离效果、较宽的线性范围和较高的灵敏度，可用于实际样品检测。A method was developed for the determination of methamidophos in soil by accelerated solvent extraction/ultra performance liquid chromatography -mass spectrometry（ASE/UPLC-MS）.The experimental conditions were investigated on the basis of the optimization of ASE conditions,and the optimal conditions were obtained as follows：extraction solvent：acetonitrile,extraction temperature：80 ℃,static extraction time：10 min,cycling twice.The extraction elute was evaporated to dryness with rotary evaporator,and analyzed by UPLC-MS.The target compound was qualitatively analyzed by the external standard method,and qualitatively analyzed by MS/MS method.The linear range was 3.15-1 050 μg/kg for methamidophos,with correlation coefficient（r） of 0.999 1.The recoveries of methamidophos at three spiked levels were in the range of 72%-82% with relative standard deviations of 5.8%-8.6%.The detection limit was 0.05 μg/kg.The method showed the advantages of accuracy,good separation effect and sensitivity,and was suitable for routine sample detection.

关 键 词：加速溶剂萃取 超高压液相色谱-质谱 甲胺磷 土壤 

分 类 号：O657.63[理学—分析化学] S482.33[理学—化学]