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正交试验法优化联苯菊酯在茶叶和土壤中的提取及检测方法

Optimization of the Extraction and Detection Methods for Bifenthrin in Tea and Soil by Orthogonal Design

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【作者】 郑坤明李小琴贾贵妃龚瑾张侃侃薛伟张钰萍陈泠竹胡德禹

【Author】 ZHENG Kun-ming;LI Xiao-qin;JIA Gui-fei;GONG Jin;ZHANG Kan-kan;XUE Wei;ZHANG Yu-ping;CHEN Ling-zhu;HU De-yu;Research and Development Center for Fine Chemicals, State Key Laboratory Breeding Base of Green Pesticide and Agricultural Bioengineering, Key Laboratory of Green Pesticide and Agricultural Bioengineering, Ministry of Education,Guizhou University;

【机构】 贵州大学精细化工研究开发中心绿色农药与农业生物工程国家重点实验室培育基地和教育部重点实验室

【摘要】 [目的]考察提取溶剂种类及用量、净化剂和色谱柱4大因素对联苯菊酯在茶叶和土壤中的提取和分析的影响。建立优化的气相色谱检测茶叶和土壤中联苯菊酯残留的分析方法,提高测定效率。[方法]在单因素条件下设计了正交试验L9(34),采用方差分析考察各因素的影响,得到最佳条件。[结果]在优化的条件下,联苯菊酯在0.0540.00 mg/L范围内具有较好的线性关系,其相关系数均大于0.999,在土壤和茶叶中的检出限分别为1.22、2.04μg/kg,定量限分别为4.05、6.81μg/kg。在0.05、0.40、4.00、8.00 mg/kg 4个添加水平下,联苯菊酯在茶叶和土壤中的回收率分别为87.92%98.53%和87.53%100.46%,日内相对标准偏差分别为2.09%4.33%和3.52%5.46%,日间分别为3.33%5.78%和1.27%4.53%。[结论]该检测方法快速简便、定量准确、精密度良好,可以满足联苯菊酯在茶叶和土壤实际样品中残留检测的要求。

【Abstract】 [Aims] To optimize the pretreatment method for detecting bifenthrin in tea and soil, the effects of the kinds and dose of extraction solvents, absorbents and columns on the extraction and detection were investigated to gain best extraction and analysis efficiency. An optimized gas chromatography method was developed to determine the residues of bifenthrin in tea and soil. [Methods] Based on the single factor experiments, the orthogonal test L9(34) was designed and analysis of variance was employed to analyze the role of each factor and perform method validation for determination of bifenthrin in the two matrices. Thus, get the best condition. [Results] Employing the optimized method, good linearity was obtained(correlation coefficient > 0.999) in the range of 0.05-40.00 mg/L. The limits of detection for bifenthrin in soil and tea were 1.22 and 2.04 μg/kg, respectively. The limits of quantification for bifenthrin in soil and tea were 4.05 and 6.81 μg/kg, respectively. With the matrix-matched calibration, the average recoveries of bifenthrin in tea and soil at four spiked levels were 87.92-98.53 and 87.53-100.46%, respectively. The relative standard deviations with intra-day were 2.09-4.33 and 3.52-5.46%, respectively. The relative standard deviations of bifenthrin with inter-day were 3.33-5.78 and 1.27-4.53%, respectively. [Conclusions] The method is quick, easy, effective,sensitive and accurate, which can be applied to the residual analysis of bifenthrin in actual tea and soil samples.

【关键词】 联苯菊酯气相色谱茶叶土壤方差分析
【Key words】 bifenthringas chromatographyteasoilanalysis of variance
【基金】 贵州大学研究生创新基金项目(2015052);国家自然科学基金项目(21367007)
  • 【分类号】TQ450.263
  • 【被引频次】1
  • 【下载频次】207
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