基质分散固相萃取-气相色谱-质谱法测定萝卜中甲拌磷及其代谢物

Determination of phorate and its metabolites in radish by matrix dispersion solid phase extraction-gas chromatography-mass spectrometry

中文关键词:  分散固相萃取法  气相色谱-质谱法  甲拌磷  甲拌磷砜  甲拌磷亚砜  萝卜

英文关键词:dispersive solid-phase extraction  gas chromatography-mass spectrometry  phorate  phorate sulfone  phorate sulfoxide  radish

中文摘要:

      目的 建立基质分散固相萃取-气相色谱-质谱法测定萝卜中甲拌磷及其代谢物的分析方法。方法 萝卜样品用10 mL乙腈和4 g 氯化钠萃取, 用100 mg N-丙基乙二胺(primary secondary amine, PSA)净化, 然后用气相色谱-质谱法测定。气相色谱分离采用DB-1MS非极性石英毛细管柱。质谱离子源温度为230 ℃, 传输线温度为280 ℃。结果 甲拌磷和甲拌磷砜在0.005~0.5 mg/L的浓度范围内、甲拌磷亚砜在0.01~1.0 mg/L的浓度范围内呈现良好的线性, 相关系数r2为0.9990~0.9992。在添加低、中、高3个浓度条件下, 甲拌磷及其代谢物平均回收率为89.2%~116%, 相对标准偏差为1.71%~5.16%, 方法检出限为0.001~0.003 mg/kg, 定量限0.003~0.01 mg/kg, 同常用的气相色谱-火焰光度检测器(gas chromatograph-flame photometric detector, GC-FPD)法比较, 该法可提高抗干扰能力, 使甲拌磷及其代谢物得到较好的分离。结论 该方法所使用的有机溶剂种类和用量少、操作简单、可测定萝卜中甲拌磷及其代谢物含量。

英文摘要:

      Objective To establish a method for the determination of phorate and its metabolites in radish by matrix dispersive solid phase extraction-gas chromatography-mass spectrometry. Methods The radish samples were extracted by 10 mL acetonitrile and 4 g sodium chloride, purified by 100 mg primary secondary amine (PSA), and then detected with gas chromatography-mass spectrometry. DB-1MS nonpolar quartz capillary column was used as separator column. Ion source temperature was 230 ℃, and the transmission temperature line was 280 ℃. Results When phorate and phorate sulfone concentrations were in the range of 0.005?0.5 mg/L, and phorate sulfoxide in the range of 0.1?1.0 mg/L, the linear relation were good obtained with correlation coefficient r2=0.9990-0.9992. Under the conditions of adding low, medium and high concentrations, the average recovery of phorate and its metabolites was 89.2%?116%, and the relative standard deviation was 1.71%?5.16%.The limit of detection was 0.001?0.003 mg/kg, and the limit of quantification was 0.003?0.01 mg/kg. Compared with the commonly used gas chromatograph-fire photometric detector (GC-FPD), this method could improve the anti-interference ability, and get a better separation of phorate and its metabolites. Conclusion This method uses a small amount of organic solvents, simple operation, and can determine the content of phorate and its metabolites in radish.