高效液相色谱法测定小麦面粉中吡蚜酮残留量

Determination of pymetrozine residue in wheat flour by high performance liquid chromatography

中文关键词:  吡蚜酮  高效液相色谱法  小麦  固相萃取  农药残留

英文关键词:pymetrozine  high performance liquid chromatography  wheat  solid phase extraction  pesticide residue

中文摘要:

      目的 采用固相萃取技术净化小麦面粉样品, 建立以反相高效液相色谱法分离、紫外检测器测定的小麦面粉中吡蚜酮残留量分析方法。方法 试样用乙腈-氨水溶液涡旋振荡提取, 二氯甲烷萃取, 浓缩后, 采用SPE-C18固相萃取柱净化, 用液相色谱法, 以C18色谱柱为分离柱, 以乙腈-水为流动相, 在299 nm波长下检测, 外标法定量。结果 在质量浓度0.01～5.0 μg/mL范围内, 吡蚜酮的峰面积与其浓度的线性关系良好, 标准曲线方程为Y=193.21X-1.6338, 相关系数为0.9999, 在选定的仪器条件下, 吡蚜酮最小检出量为2×10-11 g, 分别在0.01、0.10、1.00 mg/kg 3个添加水平进行添加回收试验, 平均回收率为86.9%～100.9%, 添加回收率试验表明, 小麦面粉中吡蚜酮的最低检出浓度为0.01 mg/kg。结论 该方法检测灵敏度高, 线性范围宽, 准确度和精密度满足农药残留检测需要, 适用于小麦面粉中吡蚜酮残留量检测。

英文摘要:

      Objective To establish a method for the determination of pymetrozine residue in wheat flour by solid phase extraction followed by reversed phase high performance liquid chromatography with UV detector. Methods The pymetrozine residue was extracted by acetonitrile-ammonia water from the wheat flour, extracted by dichloromethane and purified by SPE-C18 solid-phase extraction column, then detected by liquid chromatography at 299 nm with C18 column as separation column, acetonitrile-water as mobile phase, and quantitated with external standard quantitative method. Results In the range of 0.01~5.0 μg/mL, there was a good linear relationship between peak area and concentration, with the standard curve equation of Y=193.21X -1.6338 and the correlation coefficient of 0.9999. The detection limit was 2×10-11 g at the chosen chromatographic condition. The average recovery rate was 86.9%～100.9% with the spiked concentrations of 0.01, 0.10, 1.00 mg/kg, and the limit of quantitation was 0.01 mg/kg. Conclusion The method is sensitive, accurate, precise and with a wide linear range, and suitable for the detection of pymetrozine residue in wheat flour.