高效液相色谱-液-液分离净化法测定烟草中吡蚜酮

Xian Zhang, Xinsheng Cheng, Chuanqin Wang, Zheng Xi, Qiuhua Li
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引用次数: 15

摘要

本文首次建立了一种简便、可靠的高效液相色谱-紫外分光光度法测定烤烟中吡蚜酮残留量的方法。超声提取预处理和液-液分选程序通过去除测试中干扰吡吡嗪的水溶性和脂溶性成分,获得了较好的基线分离和干净的色谱。评价并验证了该方法的性能:检出限(LOD)为0.005μg。在0.200、0.500、1.000、5.000 mg.kg-1添加水平下,相对标准偏差(RSD)为1.2% (n=5),总回收率均在90%以上。该方法成功地测定了中国不同地区12份烤烟样品中吡蚜酮的残留量。
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Efficient High-Performance Liquid Chromatography with Liquid-Liquid Partition Cleanup Method for the Determination of Pymetrozine in Tobacco

For the first time, a novel, simple and reliable method for analysis of pymetrozine residues in flue-cured tobacco leaves has been developed utilizing HPLC-UV with liquid-liquid partition cleanup. Pre-treatment with ultrasonic extraction and liquid-liquid partition procedures gave preferable baseline separation and clean chromatograms by removing water-soluble and fat-soluble components which interfere with pymetrozine in the test. The performance of the method was evaluated and validated: the detection limit (LOD) was 0.005μg.mL-1, the relative standard deviation (RSD) was 1.2 % (n=5), and the overall recovery was above 90 % at fortification levels of 0.200, 0.500, 1.000, and 5.000 mg.kg-1. The proposed method was successfully employed for the determination of pymetrozine residues in twelve flue-cured tobacco samples collected from different regions of China.

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