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.
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)
出处
《分析科学学报》
北大核心
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)。
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
Soil
Ultra high performance liquid chromatography-triple quadruple mass spectrometry(UPLC-MS/MS)
Fluroxypyr
Nicosulfuron
Atrazine
