纯油定标法确定核磁共振仪标准曲线的研究

Study on Calibration Curve in NMR using Pure Oil

提出以纯油 (豆油或菜籽油 )制定标准曲线 (简称定标 )的方法 ,用于大豆和油菜种子中含油量的测定 .对测定结果的准确度、重现性、回收率等进行评价 ,并进一步与索氏抽提法进行比较 .结果表明 :当ATT值取 2 2db ,纯油质量为 0 .6 0 0 0～ 0 .72 0 0 g时定标 ,可用于大豆种子含油量的测定 ;同时ATT值取 31db ,纯油质量为 1.30 0 0～2 .2 0 0 0 g时定标 ,可用于油菜种子含油量的测定 .该定标方法测定种子含油量与索氏抽提法测定的含油量比较 ,差异均不显著 ,且相关系数r在 0 .95 6 6以上 .试验证明该方法准确可靠 。

A calibration curve method using pure oil (soybean oil or rapeseed oil) was proposed to determine the oil content of soybean and rapeseed seeds in NMR. The accuracy,repeatability and recovery of the determined result were also evaluated and compared with Soxhlet determination. The result showed that the calibration curve generated when ATT as 22 db and the weight of pure oil as 0.600 0～0.720 0 g may be used to determine the oil contents of soybean seed, accordingly, when ATT as 31 db and the weight of pure oil as 1.300 0～2.200 0 g may be used to determine the oil contents of rapeseed seed. There were no significant differences in oil content of seed between this method and Soxhlet method, the coefficient of correlation were above 0.956 6. The method was proved to be accurate, reliable and easy to operate.