离子色谱法检测土壤中草甘膦

石丁夫 祖艳红 陈瑞瑞 杜李继 王凯 刘玉军 陈龙胜

摘要[目的]利用草甘膦易溶于水的特点，建立一种离子色谱法测定土壤样品中草甘膦残留量的方法。[方法]结合影响草甘膦检测精确度的单因素试验，确定测定土壤中草甘膦残留量的最佳离子色谱检测方法，并对该方法的准确性和精密度进行验证。[结果]测定的草甘膦浓度在0.10～2.00 mg/L线性关系良好，相关系数（r）为0.999 7;其定性检出限（LOD）和定量检出限（LOQ）分别为0.05 mg/L（S/N>3）、0.10 mg/L（S/N>10）;通过连续进样测得其保留时间、峰面积和峰高的相对标准偏差（RSD）分别为0.09%、0.84%和0.50%;在 0.50～2.00 mg/L加标范围内，土壤中草甘膦的平均回收率为106%～113%。[结论]相对于常用的液相色谱检测法，此法无需柱前或柱后衍生、萃取、浓缩等繁琐步骤，前处理方法简单高效。该方法的回收率和精密度较好，受其他离子干扰小，且简单、快速，可满足对土壤草甘膦残留检测的要求。

关键词土壤;草甘膦;离子色谱法;检测

中图分类号O 65文献标识码A

文章编号0517-6611（2019）18-0209-02

doi：10.3969/j.issn.0517-6611.2019.18.058

开放科学（资源服务）标识码（OSID）：

Detection of Glyphosate in Soil by Ion Chromatography

SHI Ding-fu，ZU Yan-hong，CHEN Rui-rui et al（Anhui Engineering Technology Research Center for Extraction and Isolation of Active Components， Anhui Academy of Science and Technology，Hefei，Anhui 230000）

Abstract[Objective]Taking the advantage of the characteristics of glyphosate，which was soluble in water，a method for determining the residual amount of glyphosate in soil samples by ion chromatography is established.[Method]Combining the experiments of single factor impacting the accuracy of detecting glyphosate，weve confirmed the best determination of testing glyphosate residues in soil sample，and verified the accuracy and precision of this method.[Result]The experiment got a good linear relationship and a well correlation coefficient （r =0.999 7） in the concentration range of 0.10-2.00 mg/L; the limits of detection （LOD） and limits of quantification （LOQ） were 0.05 mg/L （S/N>3） and 0.10 mg/L （S/N>10），respectively; the relative standard deviation （RSD%） of retention time，peak area and peak height measured by continuous sampling was 0.09%，0.84% and 0.50%，respectively; in the concentration range of 0.50-2.00 mg/L，the average recovery rate of glyphosate in soil sample between 106% to 113%.[Conclusion]Compared with the commonly used liquid chromatography method，this method does not require complicated steps such as pre-column or post-column derivatization，extraction，concentration，etc.，and the pretreatment method is simple and efficient.The method has a well recovery yield and good precision，and was hardly influenced by other anions，would satisfy the requirement for glyphosate residue detection in soil sample.

Key wordsSoil; Glyphosate; Ion chromatography method; Detection

草甘膦（Glyphosate，N-（phosphonomethyl）glycine）是目前應用最广泛的一种广谱性有机膦除草剂，能有效抑制一年或多年生杂草[1]，但由于其对人体和环境的危害性[2-3]，其残留量的检测近年来一直是农残检测的热点。

由于草甘膦沸点较高且难溶于常用有机试剂，直接使用气相色谱法或气相色谱质谱法对草甘膦成分检测报道较少，往往都是对其酯化或酰基化以使其沸点降低后再进样分析[4-5]。目前草甘膦的仪器分析方法主要是液相色谱法，该法虽然检测灵……