目的:建立定量核磁共振氢谱(1H qNMR)法测定若干药用辅料中水分。方法:以苯磺酸钠为内标,重水为溶剂,采用核磁共振氢谱绝对定量法测定空白试样中水的含量,并在此基础上,与空白值进行比对,建立样品水含量定量计算公式,并对样品中水分进行测试和计算。结果:方法学研究表明,该方法具有良好的线性关系(r=0.999 1),线性范围为试样绝对含水量0.032~0.561 mg,精密度试验 RSD 为0.039%,重复性试验RSD为0.51%,平均加样回收率为98.7%,1H qNMR法测得DMSO-1、DMSO-2、苯磺酸钠、乙酸钠中水分分别为0.23%、0.28%、0.46%、0.28%,与2020年版《中华人民共和国药典》经典方法试验结果基本一致。结论:建立的1H qNMR法操作快速、简便,样品用量少,结果较准确,可用于一些药用辅料中水含量的测定。
Objective: To establish a quantitative nuclear magnetic resonance hydrogen spectroscopy(1H qNMR) method for determining the moisture content in several pharmaceutical excipients. Methods: Using sodium benzenesulfonate as the internal standard and heavy water as the solvent, the water content in the blank sample was determined by absolute quantification using nuclear magnetic resonance spectroscopy. By comparing with the blank value, a quantitative calculation formula for the water content in the sample was established, and the water content in the sample was tested and calculated. Results: Methodological studies had shown that this method had a good linear relationship(r=0.999 1), with a linear range of 0.032-0.561 mg absolute water content in the sample, the precision RSD was 0.039%, repeatability RSD was 0.43%, and the average recovery was 98.7%. The 1H qNMR method measured the water content in DMSO-1, DMSO-2, sodium benzenesulfonate, and sodium acetate to be 0.23%, 0.28%, 0.46%, and 0.28%, respectively, which were essentially consistent with the results obtained from the method described in the Chinese Pharmacopoeia(2020). Conclusion: The 1H qNMR method established is fast, simple to operate, with a small sample size and accurate results. It can be used for the determination of water content in some pharmaceutical excipients.
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