固相萃取-离子色谱法测定鲜笋中的草甘膦含量

丁敏; 方燕; 陆军; 王衍彬; 倪荣新; 胡静波; 杨柳

doi:10.3969/j.issn.1001-3776.2021.06.010

固相萃取-离子色谱法测定鲜笋中的草甘膦含量

Determination of Glyphosate in Fresh Bamboo Shoot by Solid Phase Extraction-Ion Chromatography

摘要

摘要: 建立了固相萃取-离子色谱法测定毛竹Phyllostachys edulis冬笋中草甘膦含量的方法：以超纯水为提取剂，高速涡旋振荡器提取，离心后经弗罗里硅土小柱完成净化，再使用高容量阴离子交换柱IonPac AS19 （250 mm ×4 mm）分离，以氢氧化钾（KOH）溶液为流动相，等度淋洗，进样量为25 μL，柱温为40℃，流速为1.0 mL·min-1；以标准溶液的浓度为横坐标，相应峰面积为纵坐标绘制标准曲线为：y = 0.995 9x+0.005 8，以3倍噪声为检出限，计算得到检出限为0.02 mg·kg-1。使用本方法，以低（0.2 mg·kg-1）、中（1.0 mg·kg-1）、高（2.0 mg·kg-1）浓度的草甘膦添加标准溶液的回收率分别为88.7%、91.4%、91.5%，相对标准偏差为1.3% ~ 2.5%（n = 6）。本方法受其它阴、阳离子及酸碱度条件等影响较小，可满足国家标准的检测要求，且具有灵敏度高，选择性好，操作简单的特点，具有一定的推广价值。

Abstract: Experiments were conducted on determination of glyphosate in fresh bamboo shoot by solid phase extraction ion- chromatography. Extraction was implemented by high speed vortex with extractant of ultrapure water, centrifuged and then purified by florisil column. Separation was made by high capacity anion exchange column, with potassium hydroxide solution as mobile phase with isocratic elution, injection volume of 25 μL, column temperature of 40℃ and flow rate of 1.0 ml/min. The recovery rate of 0.2,,1.0 and 2.0 mg/kg of glyphosate was 88.7%, 91.4% and 91.5%, and the relative standard deviation was 1.3%-2.5% (n = 6).

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