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首页> 外文期刊>Analytica chimica acta >Simultaneous determination of phenyl- and sulfonylurea herbicides in water by solid-phase extraction and liquid chromatography with UV diode array or mass spectrometric detection
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Simultaneous determination of phenyl- and sulfonylurea herbicides in water by solid-phase extraction and liquid chromatography with UV diode array or mass spectrometric detection

机译：固相萃取和液相色谱-紫外二极管阵列或质谱检测法同时测定水中的苯基和磺酰脲类除草剂

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摘要

A method for the simultaneous determination of 10 sulfonyl- and phenylurea herbicides (chlorsulfuron,triasulfuron,fenuron,monuron,flu-ometuron,chlorotoluron,isoproturon,diuron,metobromuron,linuron) and one of their most common degradation products (3-chloro-4-methyl-phenyl urea) has been developed.Liquid chromatography with diode array UV detection (LC-DAD UV) and positive ion electrospray mass spectrometry (LC-ESI-MS) were used for the separation,identification and quantification of these analytes.In the LC-DAD UV method,chromatographic separation was achieved in about 27 min;however,analysis time can be reduced to less than 13 min when LC-MS is applied,since no complete separation of the chromatographic peaks was required.A preconcentration step based on solid-phase extraction was applied for the simultaneous extraction of sulfonylureas (acidic in nature) and phenylureas (neutral compounds) from water samples.Different types of sorbents were evaluated:silica-based C_(18) and two polymeric sorbents,Oasis HLB and LiChrolut EN.The best results were obtained with Oasis HLB,a co-polymer of poly(divinylbenzene-co-N-vinylpyrrolidone).Other parameters,such as the elution solvent and sample volume,were optimised in order to maximise extraction efficiency;the recoveries obtained varied between 70 and 95% for the acidic and neutral herbicides extracted jointly without acidification of the sample.Both procedures,SPE LC-DAD UV and SPE-LC-MS,were applied to spiked river waters and were compared in terms of selectivity and sensitivity.The detection limits obtained in river water samples were below 50ng L~(-1) for both procedures.
机译：同时测定10种磺酰基和苯脲类除草剂（氯磺隆，三氟磺隆，苯磺隆，门洛隆，氟甲磺隆，氯代甲苯隆，异丙隆，对呋喃，间溴呋喃，亚麻嘧啶）及其最常见降解产物之一（3-chloro-4）的方法-甲基苯基脲）的开发。使用二极管阵列紫外检测的液相色谱法（LC-DAD UV）和正离子电喷雾质谱法（LC-ESI-MS）分离，鉴定和定量这些分析物。 LC-DAD紫外法可在约27分钟内完成色谱分离;但是，由于无需完全分离色谱峰，因此使用LC-MS时可将分析时间缩短至不到13分钟。固相萃取用于同时萃取水样品中的磺酰脲类（酸性）和苯脲类（中性化合物）。评估了不同类型的吸附剂：基于二氧化硅的C_（18）和两种聚聚吸附剂，Oasis HLB和LiChrolut EN。使用聚（二乙烯基苯-co-N-乙烯基吡咯烷酮）共聚物Oasis HLB可获得最佳结果。按顺序优化了其他参数，如洗脱溶剂和样品量最大限度地提高提取效率;联合提取的酸性和中性除草剂的回收率在70％至95％之间，而无需酸化样品.SPE LC-DAD UV和SPE-LC-MS均用于加标河水和两种方法在河水中的检出限均低于50ng L〜（-1）。

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