HPLC-MS/MS正负离子切换测定农田土壤中的2,4-二氯苯氧乙酸、敌稗和二嗪磷  

Determination of 2,4-dichlorophenoxyacetic acid,propanil and diazinon in farmland soils by positive and negative ion switch of HPLC-MS/MS

作　　者：王晓春[1,2] 张红庆[2] 陶静[1] 李铁纯[1] 

机构地区：[1]鞍山师范学院化学与生命科学学院,鞍山114016 [2]国家地质实验测试中心,北京100037

出　　处：《分析试验室》2016年第12期1375-1378,共4页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金(41430641;41140032);中国地质调查工作项目(1212011220058)资助

摘　　要：利用串联质谱正负离子切换模式功能,建立了一种能快速同时检测农田土壤中2,4-二氯苯氧乙酸,敌稗和二嗪磷残留的液相色谱-串联质谱（HPLCM S/M S）分析方法。样品以加速溶剂萃取,Supelclean ENVI-18固相萃取柱净化,多反应监测（MRM）正负离子切换电喷雾模式进行分析。色谱柱为Luna C18柱（150 mm×2.0 mm,3μm）,流动相为梯度变化的5 mmol/L甲酸铵甲醇溶液和5 mmol/L甲酸铵水溶液。方法检出限（S/N≥3）介于0.94-8.35 ng/L,相关系数≥0.999;在1.0-10.0μg/kg添加水平内,平均加标回收率介于73.8%-106.9%之间,RSD介于5.8%-11%。利用该方法对某地区农田表土的筛查发现该地区存在二嗪磷使用历史,但污染程度较轻。A high performance liquid chromatography -tandem mass spectrometry method （HPLC -MS/MS） was developed for the simultaneous determination of 2,4 - dichlorophenoxyacetic acid, propanil and diazinon in farmland soils. Samples were extracted by accelerated solvent extraction （ASE） and purified by Supelclean ENVITM- 18 solid phase extraction （SPE） cartridges, and then analyzed by HPLC -MS/MS in multiple reaction monitoring （MRM） mode with positive and negative ion switch electrospray ionization. The analytical column was Luna C18 （ 150 mm x 2.0 mm x 3 tzm ） and the mobile phases were methanol and water, containing 5 mM ammonium formate, respectively. The limits of detection （S/N〉..-3） were 0.94 - 8.35 ng/L. All of the target compounds had good linear responses with r ≥ 0. 999 and the average recoveries in the spiked levels of 1.0 to 10.0 μg/kg ranged from 73.8% -106.9% with the RSDs of 5.8% - 11%. The application of the HPLC - MS/MS method has been first demonstrated for the detection of the target compound residues in farmland soils from Jiangsu Province and the results affirmed the use of diazinon in the region.

关 键 词：高效液相色谱-串联质谱 正负离子切换 农田土壤 2 4-二氯苯氧乙酸 敌稗 二嗪磷 

分 类 号：O656.21[理学—分析化学]