Determination of Phenylurea Herbicide Residues in Environmental Water by High Performance Liquid Chromatography-Tandem Mass Spectrometry Coupled with Magnetic Solid Phase Extraction
摘 要
通过水热合成法制备磁性类沸石咪唑酯材料(Fe3O4@ZIF-8),采用扫描电子显微镜、透射电子显微镜和傅里叶变换红外光谱仪对该材料进行表征。将50 mg Fe3O4@ZIF-8加入100 mL水样中,于40℃振荡吸附10 min后,将Fe3O4@ZIF-8进行磁分离,弃去水样,加入0.5 mL乙腈,涡旋解吸1 min,将洗脱液转移,重复解吸3次,合并洗脱液,用氮气吹至近干后用甲醇-0.1%(体积分数)甲酸溶液(6+4)混合溶液溶解并定容至500 μL,经0.22 μm有机滤膜过滤,滤液在Agilent Zorbax Eclipse XDB-C18反相色谱柱(50 mm×3 mm,1.8 μm)上分离,以甲醇-0.1%(体积分数)甲酸溶液为流动相进行梯度洗脱,质谱分析中采用电喷雾离子源和多反应监测模式。4种苯脲类除草剂质量浓度均在0.01~20.0 μg·L-1内与峰面积呈线性关系,检出限(3S/N)为1.03~3.00 ng·L-1。对空白水样进行加标回收试验,回收率在78.8%~106%之间,相对标准偏差(n=6)小于7.0%。
Abstract
The magnetic zeolitic imidazole ester material (Fe3O4@ZIF-8) was prepared by hydrothermal synthesis method, and was characterized by scanning electron microscope, transmission electron microscope and Fourier transform infrared spectrometer. 50 mg of Fe3O4@ZIF-8 was added to 100 mL of water sample, and the mixture was shaken at 40℃ for 10 min of adsorption. After Fe3O4@ZIF-8 was magnetically separated and the water sample was discarded, 0.5 mL of acetonitrile was added and the mixture was vortexed for 1 min for desportion, the eluate was transferred, and desorption was repeated three times. The combined eluate was dried by nitrogen blowing, the residue was dissolved with a mixed solution of methanol and 0.1% (φ) formic acid solution (6+4), and the volume of the solution was made up to 500 μL. After the solution was filtered through a 0.22 μm organic filter, the filtrate was seperated on an Agilent Zorbax Eclipse XDB-C18 chromatographic column (50 mm×3 mm, 1.8 μm), with a mixture of methanol and 0.1% (φ) formic acid solution as the mobile phase for gradient elution. Electrospray ion source and multi-reaction monitoring mode were selected in mass spectrometry analysis. Linear relationships were found between peak areas of 4 phenylurea herbicides and the corresponding mass concentrations in the same range of 0.01-20.0 μg·L-1, and the detection limits (3S/N) were in the range of 1.03-3.00 ng·L-1. Test for recovery was made by standard addition method to blank sample, giving results in the range of 78.8%-106%, with RSDs (n=6) less than 7.0%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201809003
所属栏目 试验与研究
基金项目 江苏省高校自然科学研究重大项目(15KJA610003);苏州科技大学青年基金项目(341511201);苏州科技大学人才引进科研项目(331511207)
收稿日期 2017/9/20
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备注董南巡,硕士研究生,研究方向为环境监测分析
引用该论文: DONG Nanxun,ZHANG Lijun,GAO Shiqian,LIU Tingting,GU Haidong,YANG Chen. Determination of Phenylurea Herbicide Residues in Environmental Water by High Performance Liquid Chromatography-Tandem Mass Spectrometry Coupled with Magnetic Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(9): 1004~1010
董南巡,张丽君,高仕谦,刘婷婷,顾海东,杨晨. 磁固相萃取-高效液相色谱-串联质谱法测定环境水样中的苯脲类除草剂残留[J]. 理化检验-化学分册, 2018, 54(9): 1004~1010
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【2】陈园.高效液相色谱串联质谱法测定水中苯脲类除草剂的前处理技术方法研究[D].苏州:苏州科技学院, 2015.
【3】吴秋霞.苯基脲类除草剂激发态动力学及光化学行为研究[D].杭州:浙江理工大学, 2015.
【4】张娟.环境中苯脲类除草剂的分析和处理[D].南京:南京工业大学, 2005.
【5】刘恩梅,生威,韩静,等.苯脲类除草剂残留检测方法研究进展[J].食品与机械, 2011,27(3):160-164.
【6】王龙,宋昕,任其翾,等.尿中苯基脲类除草剂代谢物气相色谱分析[J].刑事技术, 2010(2):40-43.
【7】黄智鸿,孙茂红,王素利,等.离子液体涡旋辅助/表面活性剂乳化-液相微萃取测定牛奶中的三嗪类和苯基脲类除草剂[J].现代食品科技, 2016(1):266-271.
【8】滕曼,黄雄风.在线固相萃取-高效液相色谱法测定水中的苯脲化合物[J].环境化学, 2014,33(9):1581-1586.
【9】吴飞,张占恩,张磊.基质固相分散萃取-高效液相色谱串联质谱法测定土壤中残留的苯脲类除草剂[J].现代化工, 2016,36(5):189-192.
【10】熊力,王金成.饮用水中苯基脲除草剂的分子印迹固相萃取方法研究[J].环境监测管理与技术, 2012,24(5):44-48.
【11】王露,汪怡,杭学宇,等.磁性固相萃取-高效液相色谱法测定牛奶中4种磺胺类药物[J].理化检验-化学分册, 2017,53(5):562-565.
【12】胡文凌,张杰,余卫娟,等.磁固相萃取-高效液相色谱法测定环境水样中双酚A[J].理化检验-化学分册, 2015,51(2):153-156.
【13】刘漫,鲁晓明,冯俊鹤,等.美国沸石咪唑酯骨架结构材料的研究进展[J].现代化工, 2008,28(6):81-84.
【14】LI S L, YIN F Y, KOK K L, et al. Zeolite imidazole frameworks membranes for CO2/CH4 separation from natural gas:A review[J]. Journal of Applied Sciences, 2014,14(11):1161-1167.
【15】HU H P, LIU S Q, CHEN C Y, et al. Two novel zeolitic imidazolate frameworks (ZIFs) as sorbents for solid-phase extraction (SPE) of polycyclic aromatic hydrocarbons (PAHs) in environmental water samples[J]. Analyst, 2014,139(22):5818-5826.
【16】WANG Y, JIN S, WANG Q, et al. Zeolitic imidazolate framework-8 as sorbent of micro-solid-phase extraction to determine estrogens in environmental water samples[J]. Journal of Chromatography A, 2013,1291:27-32.
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【18】GE D, LEE H K. Zeolite imidazolate frameworks 8 as sorbent and its application to sonication-assisted emulsification microextraction combined with vortex-assisted porous membrane-protected micro-solid-phase extraction for fast analysis of acidic drugs in environmental water samples[J]. Journal of Chromatography A, 2012,1257:19-24.
【19】陈园,张丽君,顾海东,等.分散固相萃取-UHPLC-MS/MS法测定水中5种苯脲类除草剂[J].化学试剂, 2016,38(3):245-248.
【20】CULLUM N, STEPPHENS P.液相色谱/质谱用于饮用水和地下水中的苯脲及三嗪草类除草剂的确认分析[J].环境化学, 2003,22(5):516-519.
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