核磁共振磷谱法测定磷酸氢钙咀嚼片中药物含量  

Determination of phosphorus content in calcium hydrogen phosphate tablets by^(31)P-qNMR

作　　者：夏哲炜 曾垣烨 朱海菲 李育 陈啸飞 XIA Zhewei;ZENG Yuanye;ZHU Haifei;LI Yu;CHEN Xiaofei(School of Pharmacy,Naval Medical University,Shanghai 200433,China)

机构地区：[1]海军军医大学药学系,上海200433

出　　处：《药学实践与服务》2024年第9期399-401,406,共4页Journal of Pharmaceutical Practice and Service

摘　　要：目的建立一种高精密度和高专属性的核磁共振磷谱定量方法(31P-qNMR),用于检测磷酸氢钙咀嚼片中含磷药物的含量。方法使用六甲基磷酸酰胺作为内标,采集磷酸氢钙咀嚼片剂溶液的磷谱数据。研究磷酸氢钙在浓度范围1.0~9.0 mg/ml内的线性关系,并进行加样回收率和重复性实验。结果磷酸氢钙与内标的峰面积比在1.0~9.0 mg/ml范围内显示出良好的线性关系,回归方程为A=0.0043+0.1836C。低、中、高3种浓度的加样回收率分别为98.0%、98.1%、98.4%,相对标准偏差(RSD)分别为0.31%、0.68%、0.62%(n=9)。测定得到的磷酸氢钙咀嚼片中磷酸氢钙的平均含量为98.1%。结论成功建立了一种精密度高且专属性强的磷酸氢钙咀嚼片含量检测方法。该方法无需自身对照物,前处理过程简便,检测速度快,为含磷药品质量控制提供了新的技术支撑。Objective To establish a high-precision and high-specificity quantitative nuclear magnetic resonance phosphorus spectrometry method(^(31)P-qNMR)for detecting the phosphorus content in calcium hydrogen phosphate chewable tablets.Methods Hexamethyl phosphoramide was used as an internal standard,phosphorus spectrum data of calcium hydrogen phosphate chewable tablets solution was collected.The linear relationship of calcium hydrogen phosphate within the concentration range of 1.0 to 9.0 mg/ml was studied,and sample recovery rate and repeatability experiments were conducted.Results Calcium hydrogen phosphate and the internal standard demonstrated a good linear relationship within the concentration range of 1.0 to 9.0 mg/ml,with a regression equation A=0.0043+0.1836C.The recovery rates for low,medium,and high concentrations were 98.0%,98.1%,and 98.4%,respectively,with relative standard deviations(RSD)of 0.31%,0.68%,and 0.62%,respectively(n=9).The average content of calcium hydrogen phosphate in the chewable tablets was determined to be 98.1%.Conclusion This study successfully established a high-precision and highly specific method for quantifying the content of calcium hydrogen phosphate in chewable tablets,which did not require a self-reference substance,was simple in sample preparation,and had a fast detection speed.The method could provide a new technical support for the quality control of phosphorus-containing drugs.

关 键 词：核磁共振磷谱 定量核磁共振 含量测定 磷酸氢钙 

分 类 号：R927.2[医药卫生—药学]