基于低场核磁共振的烤烟烟叶石油醚提取物含量检测方法
Determination of petroleum ether extracts in flue-cured tobacco leaves by low-field nuclear magnetic resonance
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摘要: 针对当前传统索氏提取法在烤烟烟叶石油醚提取物含量检测上存在的检测速度慢、操作繁琐、溶剂污染等问题,采用低场核磁共振法检测烟叶中石油醚提取物含量,优化烘干时间、样品质量、回波时间、重复扫描次数等参数,验证最优参数下检测方法的重复性和精密度,并与传统索氏提取法的检测结果进行对比。结果表明:将过40目筛的3.0 g烟叶粉末置于80 ℃烘干4 h,在回波时间0.25 ms和重复扫描次数8次的条件下进行石油醚提取物含量检测,检测结果良好,标准曲线R2达到0.999 81,重复性的相对标准差为1.45%～2.99%,日内、日间精密度分别为2.61%、1.10%。低场核磁共振法与索氏提取法的石油醚提取物含量检测结果间的相关系数达0.998 55,绝对误差为0.02%~0.35%,相对误差为0.26%~3.69%。相较于传统索氏提取法,低场核磁共振方法简单、快速、准确,且无溶剂污染,适用于大批量烟叶石油醚提取物的准确定量。Abstract: In response to the problems of slow detection speed, cumbersome operation, and solvent pollution in the detection of petroleum ether extract in tobacco leaves using the current traditional Soxhlet extraction method, low field nuclear magnetic resonance technology was used to detect the petroleum ether extract content in tobacco leaves. The detection parameters such as drying time, sample quality, echo time, and number of repeated scans were optimized to verify the repeatability and accuracy of the method, and the detection results were compared with the traditional Soxhlet extraction method. The results showed that 3.0 g of tobacco leaf powder passing through a 40 mesh sieve was dried at 80 ℃ for 4 hours. Under the conditions of echo time of 0.25 ms and 8 repeated scans, the petroleum ether extract detection results were good. The standard curve R2 reached 0.999 81, and the relative standard deviation of repeatability was 1.45% to 2.99%. The intra day and inter day precision were 2.61% and 1.10%, respectively. The correlation coefficient between the detection results of this method and the Soxhlet extraction method reaches 0.998 55, with an absolute error within 0.02%~0.35% and a relative error within 0.26%~3.69%. Compared with the traditional Soxhlet extraction method, this method is simple, fast, accurate, and solvent free, making it suitable for the accurate quantification of petroleum ether extracts from large quantities of flue-cered tobacco leaves.
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