超高效液相色谱-三重四极杆质谱法测定土壤中氯氟吡氧乙酸、烟嘧磺隆及阿特拉津残留  

Determination of Fluroxypyr,Nicosulfuron and Atrazine Residues in Soil by Ultra High Performance Liquid Chromatography-Triple Quadruple Mass Spectrometry

作　　者：毕建玲 辜洋建 于小翠 刘丙顺 陈萍 田兴磊 BI Jianling;GU Yangjian;YU Xiaocui;LIU Bingshun;CHEN Ping;TIAN Xinglei(Shandong Institute Of Geophysical&Geochemical Exploration,Jinan 250013;Shandong Geological Exploration Engineering Technology Research Center,Jinan 250013;Shandong Engineering Research Center for High Precision Detection of Underground Resources and Environment,Jinan 250013;Shandong Institute of Geological Sciences,Jinan 250013)

机构地区：[1]山东省物化探勘查院,山东济南250013 [2]山东省地质勘查工程技术研究中心,山东济南250013 [3]地下资源环境高精度探测山东省工程研究中心,山东济南250013 [4]山东省地质科学研究院,山东济南250013

出　　处：《分析科学学报》2025年第1期106-110,共5页Journal of Analytical Science

基　　金：山东省自然科学基金面上项目(ZR2022MD001);2023年度院科技攻关项目(KY202307)。

摘　　要：采用石墨化碳黑(Graphitized Carbon Blacks,GCB)净化柱对样品进行前处理,建立了超高效液相色谱-三重四极杆质谱法检测土壤中氯氟吡氧乙酸、烟嘧磺隆及阿特拉津残留的方法。以2%甲酸-乙腈溶液对样品中目标物进行涡旋振荡提取,经加入1 g无水硫酸镁GCB净化柱净化,采用Acquity UPLC BEH C18色谱柱(50 mm×2.1 mm,1.7μm)进行洗脱分离,质谱分析采用电喷雾离子源正离子模式,多反应离子监测,外标法定量。结果表明,氯氟吡氧乙酸、烟嘧磺隆、阿特拉津3种目标物在0.50~500μg/L浓度范围内线性关系良好(R^(2)≥0.9973),检出限分别为0.6、0.4、0.2μg/kg,加标回收率为83.7%~90.9%,相对标准偏差为1.42%~5.67%。实际土壤样品测试中,基体加标回收率为82.1%~92.2%,平行样品测定满足要求。本方法操作简单、准确性和灵敏度高,适用于土壤样品中氯氟吡氧乙酸、烟嘧磺隆及阿特拉津残留的测定。A method for detecting residues of fluroxypyr,nicosulfuron,and atrazine in soil using ultra-high performance liquid chromatography-triple quadrupole mass spectrometry was established by using a graphitized carbon black(GCB)purification column for sample pretreatment.The samples were extracted by vortex oscillation with 2%formic acid-acetonitrile solution,purified by a graphitized carbon black(GCB)purification column(1g anhydrous magnesium sulfate was added to the GCB purification column),and separated by an Acquity UPLC BEH C18 column(50 mm×2.1 mm,1.7μm).The pretreated samples were analyzed under multi-reactive ion monitoring positive ion mode and quantitated by an external standard method.The results showed that the linear relationship of three target substances in the concentration range of 0.50-500μg/L was good(R^(2) was 0.9973-0.9990),and the detection limits were 0.6μg/kg,0.4μg/kg and 0.2μg/kg,respectively.The recoveries were 83.7%-90.9%,and the relative standard deviations(RSD)were 1.42%-5.67%.In the actual soil sample test,the recovery rate of matrix labeling was 82.1%-92.2%,and the parallel sample determination met the requirements.The method was simple,accurate and sensitive,and was suitable for the determination of fluroxypyr,nicosulfuron and atrazine residues in soil samples.

关 键 词：土壤 超高效液相色谱-三重四极杆质谱法 氯氟吡氧乙酸 烟嘧磺隆 阿特拉津 

分 类 号：O657.63[理学—分析化学]