一种基于质子核磁共振光谱法的用于鉴定和测定药物样品中碘帕醇和碘他拉酸葡甲胺的简单方法。

A simple method for the identification and assay of iopamidol and iothalamate meglumine in pharmaceutical samples based on proton nuclear magnetic resonance spectroscopy.

作者信息

Hanna G M, Lau-Cam C A

机构信息

Department of Health and Human Services, Northeast Regional Laboratory, Food and Drug Administration, Jamaica, New York, New York, USA.

出版信息

Pharmazie. 2001 Feb;56(2):152-5.

PMID:11234344

Abstract

A proton nuclear magnetic resonance (PMR) spectroscopic method is described for the direct assay and identification of the triiodinated radiographic contrast agents iopamidol (nonionic type) and iothalamate meglumine (ionic type) in commercial solutions and as a bulk material. Samples were prepared by simply diluting an injectable solution with or dissolving a powdered sample in D2O. Sodium acetate was added to serve as an internal standard. Quantitations were based on the resonance signals for the protons of the CH3-CO-group at 1.58 ppm (iopamidol) or 2.25 ppm (iothalamate), CH3-N-group at 2.38 ppm (meglumine) and CH3-CO-group at 1.92 ppm (acetate). The mean +/- SD (n = sets of 10 samples each) recovery of iopamidol, iothalamic acid and meglumine from synthetic mixtures with the internal standard were 99.6 +/- 0.63, 99.7 +/- 0.66 and 99.9 +/- 1.18%, respectively; with the values ranging from 98.7-100.9% for iopamidol and iothalamate, and from 98.3-100.8% for meglumine.

摘要

描述了一种质子核磁共振（PMR）光谱法，用于直接测定和鉴别市售溶液及原料药中的三碘放射造影剂碘帕醇（非离子型）和碘他拉酸葡甲胺（离子型）。样品制备方法简单，可将注射用溶液稀释，或将粉末状样品溶于重水（D2O）中。加入醋酸钠作为内标。定量分析基于1.58 ppm处CH3-CO-基团质子的共振信号（碘帕醇）或2.25 ppm处（碘他拉酸）、2.38 ppm处CH3-N-基团（葡甲胺）以及1.92 ppm处CH3-CO-基团（醋酸盐）的共振信号。碘帕醇、碘他拉酸和葡甲胺从含内标的合成混合物中的平均回收率±标准差（n = 每组10个样品）分别为99.6±0.63%、99.7±0.66%和99.9±1.18%；碘帕醇和碘他拉酸的值在98.7 - 100.9%之间，葡甲胺的值在98.3 - 100.8%之间。