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食品研究与开发:2019,40(18):154-159
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食品中磺酰脲类除草剂的高效液相色谱分析
(西安市疾病预防控制中心,陕西西安710054)
The Determination of Sulfonylurea Herbicides in Food by High Performance Liquid Chromatography
(Xi'an Center for Disease Control and Prevention,Xi'an 710054,Shaanxi,China)
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投稿时间:2018-11-15    
中文摘要: 建立一种同时测定磺酰类除草剂的高效液相色谱法(high performance liquid chromatography,HPLC)方法,以利于对农产品质量进行准确定量与有效监管。7 种磺酰脲类除草剂(甲磺隆、氯磺隆、苄嘧磺隆、苯磺隆、吡嘧磺隆、甲磺胺磺隆和丙苯磺隆)经甲醇提取,C18 固相萃取小柱萃取净化后,高效液相色谱测定,用C18 色谱柱分离,以乙腈-甲醇-盐酸为流动相,梯度洗脱,紫外检测器在波长为220、230、240 nm 处测定。方法的线性范围为0.5 μg/mL~100.0 μg/mL,检出限为0.011 μg/mL~0.025 μg/mL,标准溶液测定的保留时间和峰面积的相对标准偏差分别为0.18%~0.89%和2.57%~5.57%。将所建立的方法用于大豆、玉米和大米样品的分析,标回收率在81.0%~116.1%。本法准确快速,20 min 内可完成一次分析周期,适用于食品样品中磺酰脲类除草剂的快速测定。
Abstract:The method for the simultaneous determination of the sulfonylurea herbicides by high performance liquid chromatography (HPLC)was established to accurately quantify and effectively supervise the product.After being dissolved with ethanol and exctracted with C18 solid phase extraction,7 kinds of sulfonylurea herbicide was analyzed by HPLC.C18 column and acetonitrile-methanol-hydrochloric acid as mobile phase with gradient elution was used throughout the experiment.The wavelength of ultraviolet detector was 220,230 nm and 240 nm.The linear range of the method were 0.5 μg/mL-100.0 μg/mL and the detection limit were 0.011 μg/mL-0.025 μg/mL.The relative standard deviation of retention time and peak area for the determination of standard solution were 0.18%-0.89%and 2.57%-5.57%respectively.The average recovery was 81.0%-116.1%.The method was quick and accurate.The chromatographic determination only was needed 20 min.It is suitable for the determination of 7 kinds of sulfonylurea herbicide in food.
文章编号:201918027     中图分类号:    文献标志码:
基金项目:陕西省重点研发计划项目(2017SF-384)
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