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

作　　者：耿慧春[1,2] 方海仙 梅文泉[1,2] 陈兴连 王丽[1,2] 汪禄祥 GENG Hui-Chun;FANG Hai-Xian;MEI Wen-Quan;CHEN Xing-Lian;WANG Li;WANG Lu-Xiang(Quality Standardizing and Testing Technology Institute,Yunnan Academy of Agricultural Science,Kunming 650205,China;Supervision&Testing Center for Farm Products Quality,Ministry of Agriculture Kunming Section,Kunming 650205,China)

机构地区：[1]云南省农业科学院质量标准与检测技术研究所,昆明650205 [2]农业农村部农产品质量监督检验测试中心(昆明),昆明650205

出　　处：《食品安全质量检测学报》2020年第23期8762-8768,共7页Journal of Food Safety and Quality

基　　金：农业联合青年计划项目(2018FG001-081)。

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。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-1 MS 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 r^2=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.

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 

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]