核磁定量的精度？

有文献提及在某 600 兆仪器检测的定量准确度 2%.

核磁共振定量还在研究阶段吧……

有人公开对外收样品了吗？

我们去年做了"替米考星"的NMR定量,文章发表在<分析测试学报>

有些药物是用NMR定量的,比如GENTAMICIN,(20年前英国药典),当时我们为出口单位做检测.这方面的资料不少.国外多一些.

楼主可以参考一下
Quantitative nuclear magnetic resonance (QNMR) spectroscopy for assessing the purity of technical grade agrochemicals: 2,4-dichlorophenoxyacetic acid (2,4-D) and sodium 2,2-dichloropropionate (Dalapon sodium).

Comparison of quantitative NMR spectroscopy (QNMR) with chromatographic methods such as gas chromatography (GC) or high-pressure liquid chromatography (HPLC) for the determination of the purity of and impurities in technical grade agrochemicals, 2,4-dichlorophenoxyacetic acid (2,4-D), 1, and Dalapon sodium (sodium 2,2-dichloropropionate), 10, has revealed that QNMR is more precise and accurate than the chromatographic methods. Quantitative impurity profiling of technical grade 1 is rapid and accurate using 600 MHz (1)H NMR. Extra dispersion at the relatively high frequency allowed full assignment of the NMR spectrum of 1 and its related organic impurities in technical samples. The percentage purity of 1 was measured by the difference QNMR method, which involves summing the amounts of impurities and subtracting from 100%. Results are superior in consistency to those obtained by chromatographic methods. The percentage purity of Dalapon sodium, 10, in technical grade batches is readily obtained by (1)H QNMR, using either the difference method or the internal standard method, using dimethyl sulfone (DMSO2) internally as a reference material, that is chemically unrelated to the analyte. The latter method also allows the simultaneous identification and quantification of impurities, many of which are either not accessible to or detectable by the chromatographic methods. Uncertainty budgets for the QNMR method are presented and demonstrate that the major contributors to uncertainty lie in the weighing of the chemicals and in purity of the standard reference material prior to the QNMR experiment

请问核磁内标法（绝对测量法）定量分析不需引进任何校正因子，不需制作标准曲线吗？高效液相色谱为何需制作标准曲线？它们定量的原理差不多呀？
请问核磁定量检测方法的专属性好，指什么？
请问核磁定量检测方法的耐用性指什么？

我做了相关实验，以精确称量的样品与内标的质量之比为横坐标X，样品与内标的积分面积之比为纵坐标Y，作线性回归。回归方程: y = 0.4487x +0.0093，线性相关系数r = 0.999 5。图谱在附件中，线性如何？

取9号样品在核磁仪上平行实验的Au/ Aa相对标准偏差(%)为0.0185%，仪器精密度很好吧？

为何没有人回复呢？请做过核磁定量的各位大侠多指点。

奇怪，我上传的图谱怎么不出现？上传三次了

图谱

核磁的精确度 (弱项) 主要在积分的准确性. 要积分精确要注意谱图清晰 (足够的扫描 wft, aph, dc, bc), 切线水平 (调 tlt/lvl).