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 m L甲醇超声萃取30 min,取上清液过0. 22μm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. 0μg/L质量浓度范围内线性良好(r~2> 0. 999),方法检出限分别为0. 004 9μg/kg和0. 003 4μg/kg。在0. 400、4. 00、40. 00μg/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。
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 m L 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( r~2) larger than 0. 999. The detection limits for acephate and methamidophos in soil were0. 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% and88. 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.
引文
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