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超声提取/超高效液相色谱-串联质谱法测定土壤中乙酰甲胺磷与甲胺磷的研究
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作者单位
魏立菲,李逸,张荧 珠江流域水环境监测中心 
基金项目:国家自然科学基金青年基金项目(41303082)
中文摘要:建立了超声提取/超高效液相色谱-三重四极杆串联质谱(UPLC-MS/MS)快速测定土壤中乙酰甲胺磷和甲胺磷的方法。10.0 g土壤样品采用20.0 mL甲醇超声萃取30 min,取上清液过0.22 μm滤膜后进行UPLC-MS/MS分析,外标法定量。结果表明:乙酰甲胺磷和甲胺磷在0.002~20.0 μg/L质量浓度范围内线性良好(r2>0.999),方法检出限分别为0.004 9 μg/kg和0.003 4 μg/kg。在0.400、4.00、40.00 μg/kg加标水平下,土壤样品中乙酰甲胺磷和甲胺磷的平均回收率分别为83.0%~91.5%和88.0%~94.8%,相对标准偏差(RSD,n=6)分别为2.3%~4.8%和1.8%~4.2%。该方法前处理简单快捷、灵敏度高、定性定量准确,可用于土壤样品中乙酰甲胺磷和甲胺磷含量的快速检测。
中文关键词:乙酰甲胺磷  甲胺磷  超声提取  超高效液相色谱-串联质谱(UPLC-MS/MS)
 
Study on Determination of Acephate and Methamidophos in Soil by UPLC-MS/MS with Ultrasonic Extraction
Abstract:A method was developed for the determination of acephate and methamidophos in soil by ultrahigh performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) with ultrasonic extraction.10.0 g soil sample was extracted with 200 mL methanol under ultrasonic assistance for 30 min.Then the clear supernatant extract was filtered through 0.22 μm membrane,and analyzed by UPLC-MS/MS with external standard method.There were good linear relationships for acephate and methamidophos both in the range of 0.002-20.0 μg/L with their correlation coefficients(r2) larger than 0.999.The detection limits for acephate and methamidophos in soil were 0.004 9 μg/kg and 0.003 4 μg/kg,respectively.The recoveries for acephate and methamidophos at three spiked levels of 0.400,4.00 and 40.00 μg/kg were in the ranges of 83.0%-91.5% and 88.0%-94.8% with their relative standard deviations(RSDs,n=6) of 2.3%-4.8% and 1.8%-4.2%,respectively.The method was simple,rapid,sensitive and accurate in both quantitation and qualitation,and was suitable for the routine determination of acephate and methamidophos in soil samples.
Key Words:acephate  methamidophos  ultrasonic extraction  UPLC-MS/MS
引用本文:魏立菲,李逸,张荧.超声提取/超高效液相色谱-串联质谱法测定土壤中乙酰甲胺磷与甲胺磷的研究[J].分析测试学报,2019,(2):219-223.
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