目的 建立定量核磁方法，同时测定复方阿胶浆（Compound E’jiao Jiang，CEJ）的药材提取液中多类成分的含量，为中间体的质量评价提供可靠的分析手段。方法 采用水信号预饱和脉冲序列Noesygppr1d采集样品的¹H-NMR图谱。通过文献调研、数据库检索以及加标实验的方式进行核磁谱峰归属。进一步确定各化合物的定量峰，采用内标法定量。开展方法学考察，考察项包括线性、精密度、稳定性、重复性、耐用性、准确度。另基于核磁共振氢谱的信噪比确定方法的检测限和定量限，并对3批中间体样本进行分析。结果 共指认22种化合物，其中17种可同时定量分析，包括缬氨酸、丙氨酸、异亮氨酸、焦谷氨酸、γ-氨基丁酸5种氨基酸，乙酸根、富马酸根、丙酮酸根、琥珀酸根、甲酸根、乳酸6种小分子有机酸根，葡萄糖、果糖、半乳糖、蔗糖4种糖类以及尿苷、胆碱。线性考察结果得出相关系数均不小于0.999 5，精密度考察结果显示，RSD均小于2.7%，重复性考察RSD均小于2.5%，耐用性及稳定性考察RSD均小于2.6%，加样回收实验得出平均回收率为90.0%～105.0%、RSD小于2.2%，分析值与参考值平均相对偏差小于4.0%。对3批样品进行定量分析，17种成分的测定结果均高于定量限，且满足线性范围。3批样品可定量部分占总固体含量的质量分数分别为71.09%、84.44%、70.09%。结论 各方法学考察均满足要求；研究开发的定量核磁方法检测时间短、制样方式简单，能有效提高分析效率，为CEJ的生产过程物质转移规律研究打下基础。

Objective To establish a quantitative nuclear magnetic resonance (NMR) method for simultaneous determination of multiple components of extract solutions in the production of Compound E’jiao Jiang (复方阿胶浆, CEJ), in order to provide a reliable analytical means for the quality evaluation of midbody. Method The ¹H-NMR spectra of the samples were acquired using the water suppression pulse sequence Noesygppr1d. Peak assignments of the NMR spectra were performed through literature research, database retrieval, and spiking experiments to further determine the quantitative peaks of each compound. Compounds were quantified via an internal standard method, with methodological validation encompassing linearity, precision, stability, repeatability, durability, and accuracy. Detection and quantification limits were based on the signal-to-noise ratio of the proton NMR spectra. Three batches of intermediaries were analyzed. Results A total of 22 compounds were identified, among which 17 compounds could be simultaneously quantitatively analyzed. These compounds include five amino acids (valine, proline, isoleucine, glutamic acid, and γ-aminobutyric acid), six organic acids (acetate, fumarate, pyruvate, succinate, formate, and lactate), four sugars (glucose, fructose, galactose, and sucrose), uridine and choline. Linearity showed correlation coefficients above 0.9995. Precision, repeatability, durability, and stability reflected RSDs below 2.7%. Spike recovery tests indicated an average recovery rate between 90.0% and 105%, with an RSD below 2.2%. Relative deviations between analyzed and reference values were under 4.0%. Quantitative analysis for three batches of samples showed that the determined results for all 17 components were above the quantification limit and within the linear range. The mass fraction of the quantifiable portion relative to the total solid content was 71.09%, 84.44%, and 70.09%, respectively. Conclusion Our method met stringent standards, with expedited detection and streamlined sample preparation, enhancing analytical efficiency and elucidating material transfer during its production.

国家中医药管理局“组分中药与智能制药多学科交叉创新团队”项目（ZYYCXTD-D-202002）