高效液相色谱法检测小麦和土壤中叶菌唑的残留-食品安全质量检测学报.DOCVIP

PAGE 4 食品安全质量检测学报 第8卷 第2期 周自豪, 等: 高效液相色谱法检测小麦和土壤中叶菌唑的残留 PAGE 5 第8卷 第2期 食品安全质量检测学报 Vol. 8 No. 2 2017年2月 Journal of Food Safety and Quality Feb. , 2017 *通讯作者: 王鸣华, 教授, 博士生导师, 主要研究方向为农药残留及环境毒理研究。E-mail: wangmha@ *Corresponding author: WANG Ming-Hua, Professor, Doctoral Supervisor, College of Plant Protection, Nanjing Agricultural University, Nanjing 210095, China. E-mail: wangmha@ 高效液相色谱法检测小麦和土壤中叶菌唑的残留 周自豪, 程冰峰, 王鸣华* (南京农业大学植物保护学院, 南京 210095) 摘 要: 目的 建立固相萃取-高效液相色谱法测定土壤、麦粉和小麦植株中叶菌唑残留的方法。方法 土壤、麦粉和小麦植株样品采用乙腈提取, 经Silica-SPE固相萃取柱净化, Eclicpse Plus C18色谱柱分离, 采用高效液相色谱法进行检测, 以外标法定量。结果 叶菌唑在0.1~10 mg/L范围内呈良好的线性关系, 标准曲线方程为Y=37.395X-1.0902, 相关系数为0.9999。在加标水平为0.05~2.0 mg/kg范围内, 叶菌唑在土壤、麦粉和小麦植株中的平均回收率为87.2%~100.9%, 相对标准偏差为0.2%~8.7%。叶菌唑的最低检测浓度为0.05 mg/kg。结论 该方法简便、快速、准确, 可为叶菌唑在小麦中的残留分析提供技术依据。 关键词: 叶菌唑; 高效液相色谱法; 固相萃取; 小麦; 残留分析 Determination of metconazole residues in wheat and soil by high performance liquid chromatography ZHOU Zi-Hao, CHENG Bing-Feng, WANG Ming-Hua* (College of Plant Protection, Nanjing Agricultural University, Nanjing 210095, China) ABSTRACT: Objective To establish a method for the determination of metconazole residues in soil, wheat flour and wheat plant by solid phase extraction-high performance liquid chromatography (SPE-HPLC). Methods The metconazole from soil, wheat flour and wheat plant samples were extracted with acetonitrile, cleaned up by a Silica-solid phase extraction column (Silica-SPE), separated by an Eclicpse Plus C18 column, and detected by HPLC with the external standard method for quantification. Results Metconazole had a good linear relationship in the range of 0.1 to 10 mg/L. The standard curve equation was Y=37.395X-1.0902 with the correlation coefficient of 0.9999. The average recoveries of metconazole in soil, wheat flour and wheat plant spiked in the range of 0.05~2.0 mg/kg were 87.2%~100.9% with the relative standard deviations (RSDs) of 0.2%~8.7%. The limit of quantification was 0.05 mg/kg. Conclusion Th