蒽加氢产物的结构指认和定量核磁共振分析

本文利用多种液体核磁共振（NMR）技术,综合分析了在三个不同反应条件下蒽催化加氢反应获得的产物混合物.利用二维扩散排序谱（DOSY）和一维选择性激发谱（selTOCSY）确定了产物中含有的二氢蒽、四氢蒽、对称八氢蒽和非对称八氢蒽;利用¹H NMR、¹³C NMR、DEPT135、¹H-¹H COSY、¹H-¹³C HSQC实验对二氢蒽、四氢蒽和对称八氢蒽的¹H和¹³C NMR信号进行了详细归属;利用定量核磁共振氢谱（QNMR）计算得到了蒽的转化率和产物的选择性.本研究可用于指导优化催化反应条件,提高产物对称八氢蒽的选择性,同时为稠环类芳烃催化加氢产物的分析提供系统的NMR技术方案.     

High performance liquid chromatography - Quantitative nuclear magnetic resonance - High performance liquid chromatography for purity measurement of human insulin

Quantitative Nuclear Magnetic Resonance (qNMR) is a reliable quantitative spectroscopic technique, wherein the intensity of a resonance line is directly proportional to the number of resonant nucleus, and the absolute content of the compound can be determined, this means the inorganic stabilizer in the sample would not affect the result of qNMR. High performance liquid chromatography (HPLC) is a common analytical method with a high separation capacity. This study combined HPLC and qNMR, to measure the purity of Human Insulin (HI). It started from an original HI. The first step is purifying the original HI by HPLC to get a purified HI, with organic purity of 99.78%. The second step is assessing the absolute content of the purified HI by qNMR, and got 40.25%. The third step is measuring the purity of original HI by HPLC again, using the purified HI as the reference material. This method, called HPLC-qNMR-HPLC, is more accurate (84.12%?±?1.14%) than the traditional IDMS (isotope dilution mass spectrometry) method (86.6%?±?3.4%). This study expanded the application of qNMR to proteins with molecular weight of about 5800, and showed that this method can be widely used in measuring the purity of macromolecular proteins.     

核磁共振法定量测定替米考星含量

用核磁共振(^1H NMR)法测定了药品替米考星(tilmicosin)的含量，给出了完整的实验条件和注意事项，线性实验测得线性回归系数为0.9985，重复性实验测得RSD为0．327％。表明此方法做为一种药物的定量方法具有简单易行、结果准确的优点，可用做某些没有对照品的药物定量方法的补充。     

An uncertainty budget for the determination of the purity of glyphosate by quantitative nuclear magnetic resonance (QNMR) spectroscopy

An uncertainty budget is presented for the results of measurements of purity of the agrochemical glyphosate using ¹H and ³¹P quantitative nuclear magnetic resonance (QNMR) spectroscopy. The budget combines intralaboratory precision from repeated independent measurements of a batch, and other Type A and Type B effects. Consideration of correlation of uncertainties in ratios of mass determinations has been included. Expanded uncertainties of the purity for single determinations of purity by ¹H and ³¹P QNMR are 0.66% and 0.82% (95% confidence interval, k=2), respectively.