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摘要：本论文建立了对中药复方药物中有效成分黄芩苷类似物的核磁共振定量测定方法，并以其中主要成分黄芩苷的含量来表示黄芩苷类似物总含量。选择内标为邻苯二甲酸氢钾，以其质子峰(δ=8.204)作为内标峰，待测物定量峰的化学位移在δ=8.075ppm处，溶剂为氘代DMSO。利用样品中几种主要中药成分的浸膏和辅料进行核磁实验，证明其他中药成分和辅料对所选的定量峰无干扰。考察了实验条件的影响，并选择采样次数NS为128次，延迟时间D1为1.0s，脉冲宽度P1为3.0μs。并作出标准曲线，相关系数为0.999997，线性良好，且斜率与理论值十分接近，故可用内标法直接测定。实际测定了一清胶囊和三黄片两种复方中药的优尔个样品中黄芩苷类似物的总含量。用核磁共振绝对定量法进行计算，得到的结果与文献报道中利用高效液相色谱法得到的结果十分接近，RSD小于3%，其回收率在99.72%以上，且溶液稳定性良好。此外，对复方中药中另一类有效成分盐酸小檗碱类似物的定量测定方法进行了探索。8837
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关键词：定量；核磁共振；一清胶囊；三黄片；黄芩苷；盐酸小檗碱
Quantitative analysis of compound Chinese medicine by 1H-NMR
Abstract: The quantification of baicalin analogues in compound Chinese medicine using 1H NMR spectroscopy is established, and instead of the total content of the baicalin analogues by the content of the baicalin which is the most in the baicalin analogues. The internal standard is potassium hydrogen phthalate where at the peak of the chemical shift is 8.204ppm. The peak of chemical shift that the baicalin is at 8.075ppm and the solvent is deuterated DMSO. Detecting auxiliary material and some extract of the other main herbs in the compound Chinese medicine，proving that these auxiliary material and herbs have no interference for the peak of baicalin. Then delay time D1=1.0s, pulse width P1=3.0μs and number of transient NS=128 times were selected. In order to use internal standard method directly, we make standard curve of baicalin, R=0.999997, the linear is excellent. Furthermore, the slope is approach to the theoretical value. Three Yiqing capsules and three sanhuang tablets were measured. Results from the NMR quantifications were compared with those obtained from determinations by HPLC and the RSD is less than 3%, the recovery rate of baicalin is more than 99.72%. The stability of solution is good. What’s more, we explore the quantification of another main component in compound Chinese medicine which is berberine hydrochloride analogues.
Key Words: quantitation; 1H-NMR; Yiqing capsule; sanhuang tablet; baicalin; berberine hydrochloride
目 录
1 前言 1
1.1 选题意义 1
1.2 文献进展状况 1
1.2.1 NMR定量 1
1.2.1.1 内标法（绝对定量法） 2
1.2.1.2 相对测量法 2
1.2.1.3 外标法 2
1.2.2 qHNMR技术在定量方面的应用 2
1.2.2.1 qHNMR技术在药物定量方面的应用 3
1.2.2.1.1 应用实例 3
1.2.2.1.2 展望 5
1.2.2.2 qHNMR技术在其他方面的应用 6
2 实验部分 7
2.1 仪器与试剂 7
2.1.1 仪器 7
2.1.2 试剂与药品 7
2.2 复方中药中黄芩苷类似物的核磁共振定量测定 7
2.2.1 复方中药中黄芩苷类似物定量测定方法 7
2.2.2 复方中药中黄芩苷核磁共振定量内标物的选择 8
2.2.3 实验条件对黄芩苷定量峰的影响 8