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中国农学通报 ›› 2012, Vol. 28 ›› Issue (6): 217-221.

• 植物保护 农药 • 上一篇    下一篇

河水中噻菌灵和敌百虫的SPE-RP-HPLC分析

高智席 吴艳红 黎司 胡明华 牟青松 曾启华   

  • 收稿日期:2011-10-28 修回日期:2011-12-03 出版日期:2012-02-25 发布日期:2012-02-25
  • 基金资助:

    贵州省科技厅社会发展攻关项目;贵州省教育厅自然科学项目;遵义市科技局自然科学项目

Analysis of Thiabendazole and Trichlorfon in River Water by RP-HPLC with Solid-phase Extraction

  • Received:2011-10-28 Revised:2011-12-03 Online:2012-02-25 Published:2012-02-25

摘要:

为了对河水中噻菌灵和敌百虫残留进行高效的富集纯化和测定,建立了噻菌灵和敌百虫固相萃取-反相高效液相色谱法进行检测。河水中的噻菌灵和敌百虫用3 mol/L Empore 6 mL C18固相萃取小柱进行固相萃取。以Shim-pack VP-ODS 150 mm × 4.6 mm柱为分析柱,优化得到高效液相色谱分离条件:流动相为乙腈:水=75:25(V/V),流速为0.8 mL/min,进样量20 μL。结果表明,噻菌灵和敌百虫在0.13~97.92 μg/mL (r=0.9961)、0.02~50 μg/mL (r=0.9994)浓度范围内与峰面积成良好线性关系,检出限分别为0.09 μg/mL、0.01 μg/mL,噻菌灵和敌百虫的回收率为87.6%~101.3%,相对标准偏差为1.7%~2.77%。可以看出,该方法操作简便快速,可作为河水中噻菌灵和敌百虫含量监测的控制方法。

关键词: 测度, 测度

Abstract:

For better enrichment and purity of thiabendazole and trichlorfon in river water, a reversed-phase high performance liquid chromatograghic method with solid-phase extraction was used for the residue dynamic analy-sis of thiabendazole and trichlorfon. Water was subjected to solid-phase extraction (SPE) using 3 mol/L Empore 6 mL C18. The analytical column of HPLC was Shim-pack VP-ODS 150 mm × 4.6 mm with a mobile phase of CH3CN:H2O = 75:25 (V/V), flow rate 0.8 mL/min, injection volume 20 μL. The SPE-HPLC method showed good linearity of thiabendazole and trichlorfon was obtained over the range of 0.13-97.92 μg/mL (r=0.9961), 0.02-50 μg/mL (r=0.9994). The detection limits were 0.09 μg/mL and 0.01 μg/mL for thiabendazole and trichlorfon. The average recoveries ranged from 87.6%-101.3% with relative standard deviation 1.7%-2.77%. In conclusion, the method was fast and simple for the residue detection and analysis of thiabendazole and trichlorfon in river water.