Reque法结合高效液相色谱-高分辨质谱法测定粮谷中克瘟散残留量

Determination of edifenphos residue in grain by Reque method combined with high performance liquid chromatography-high resolution mass spectrometery

中文关键词:  克瘟散  Reque  高效液相色谱-高分辨质谱法  粮谷

英文关键词:edifenphos  Reque  high performance liquid chromatography-high resolution mass spectrometery  grain

中文摘要:

      目的 建立Reque法结合高效液相色谱-高分辨质谱法测定粮谷中克瘟散残留量。方法 本研究优化了粮谷中克瘟散残留量测定前处理方法, 分析液相色谱-高分辨质谱仪的仪器条件、检出限、线性范围、回收率等关键参数。样品通过90%乙腈溶液提取, 由Reque净化柱净化, 经配备Phenomenex Kinetex F5色谱柱的液相色谱分离, 通过高分辨质谱扫描进行定性、定量分析。结果 粮谷中克瘟散在1~100 ng/mL范围内具有良好的线性关系(r>0.999)。5种粮谷的检出限均为10 ng/g, 方法准确度和精密度通过加标回收实验进行验证, 在10、20、100 ng/mL的加标水平下, 回收率范围为90.6%~109.8%, 相对标准偏差为2.10%~5.20%。结论 本方法能够快速、灵敏、准确地测定粮谷中克瘟散的残留量, 适用于多种粮谷中克瘟散残留量的检测。

英文摘要:

      Objective To establish a method for the determination of residue of edifenphos in grain by Reque method combined with high performance liquid chromatography-high resolution mass spectrometry. Methods In this study, the pre-treatment method for the determination of residue of edifenphos in grain was optimized, and the key parameters such as instrument condition, limit of detection, linear range and recovery rate of liquid chromatography-high resolution mass spectrometer were analyzed. Samples were extracted with 90% acetonitrile solution, purified by Reque purification column, separated by liquid chromatography with Phenomenex Kinetex F5 column, and analyzed qualitatively and quantitatively by high resolution mass spectrometry. Results The edifenphos in grain had a good linear relationship (r>0.999) in the range of 1–100 ng/mL. The limits of detection of 5 kinds of grains were all 10 ng/g. The accuracies and precisions of the method were verified by standard recovery experiments. Under the standard addition levels of 10, 20 and 100 ng/mL, the recovery ranged from 90.6% to 109.8%, and the relative standard deviation ranged from 2.10% to 5.20%. Conclusion The method can quickly, sensitively and accurately determine the residue of edifenphos in grain, and is suitable for the detection of edifenphos residue in many kinds of grain.