定量核磁共振磷谱同时测定浓维磷糖浆中甘油磷酸钠和磷酸的含量  

Simultaneous Determination of Sodium Glycerophosphate and Phosphoric Acid in Concentrated Divitamins and Sodium Phosphate Syrup by Quantitative 31P-Nuclear Magnetic Resonance

作　　者：屠相土 李俊 雷虹 徐玲萍 曾茂法 TU Xiang-Tu;LI Jun;LEI Hong;XU Ling-Ping;ZENG Mao-Fa(Taizhou Institute for Food and Drug Control,Taizhou 318000,China)

机构地区：[1]台州市食品药品检验研究院,台州318000

出　　处：《分析化学》2024年第7期1020-1027,共8页Chinese Journal of Analytical Chemistry

摘　　要：建立了定量核磁共振磷谱法(^(31)P-qNMR)同时测定浓维磷糖浆中α-甘油磷酸钠、β-甘油磷酸钠和磷酸含量的方法.考察了qNMR实验条件对测定结果的影响,选择六甲基磷酰三胺为内标、20%重水溶液(V/V)为溶剂,选择zgig脉冲序列、延迟时间30 s、扫描次数64次为实验条件,进行采样测试获取^(31)P-qNMR谱,其中,六甲基磷酰三胺、α-甘油磷酸钠、β-甘油磷酸钠和磷酸的定量共振峰分别为δ29.80、δ0.69、δ0.17和δ0.03(供试品溶液pH≈4.8).结果表明,^(31)P-qNMR法测定α-甘油磷酸钠、β-甘油磷酸钠和磷酸的检出限分别为23.58、23.58和11.61μg/mL,定量限分别为78.60、78.60和38.70μg/mL,线性相关系数(R)均大于0.999,精密度小于0.6%,平均回收率为99.8%~103.2%,相对标准偏差(RSD)为0.41%~1.98%.本研究建立的^(31)P-qNMR方法测定结果准确,稳定可靠.采用本方法测定了7批次不同厂家的浓维磷糖浆样品,其中,总磷量检测结果与比色法一致;甘油磷酸钠含量(α型与β型之和)偏低,约为标示量的82%;磷酸含量偏高.本方法操作简单、专属性强,适合作为浓维磷糖浆质量控制的方法.A ^(31)P-quantitative nuclear magnetic resonance(qNMR)method was established for simultaneous determination of sodiumα-glycerophosphate,sodiumβ-glycerophosphate and phosphoric acid in concentrated divitamins and sodium phosphate syrup.The qNMR experimental conditions were optimized,including hexamethylphosphoramide as internal standard,20%deuterium oxide solution as solvent,zgig pulse sequence,delay time of 30 s,and scan number of 64.The ^(31)P-NMR peaks atδ29.80 of hexamethylphosphoramide,δ0.69 of sodiumα-glycerophosphate,δ0.17 of sodiumβ-glycerophosphate andδ0.03 of phosphoric acid were chosen as the quantitative peaks(pH of the test solution was around 4.8).Method validation was performed in terms of precision(Relative standard deviation less than 0.6%),linearity(Correlative coefficient greater than 0.999),limit of detection(23.58μg/mL for sodium glycerophosphate and 11.61μg/mL for phosphoric acid)and limit of quantitation(78.60μg/mL for sodium glycerophosphate and 38.70μg/mL for phosphoric acid).The recoveries were 99.8%‒103.2%,and relative standard deviations were 0.41%‒1.98%.The results showed that the reliability of ^(31)P-qNMR method were suitable for its intended use.Seven batches of concentrated divitamins and sodium phosphate syrups were tested by the established method,of which the total phosphorus content was consistent with that of colorimetry method,but the content of sodium glycerophosphate(Sum ofαtype andβtype)was relatively low,about 82%of the labeled amount.The content of phosphoric acid was high.This method simplified sample pretreatment and had high specificity,and was more suitable for determination and quality control of concentrated divitamins and sodium phosphate syrup.

关 键 词：定量核磁共振磷谱法 浓维磷糖浆 甘油磷酸钠 磷酸 

分 类 号：TQ460.72[医药卫生—药物分析学] O657.2[化学工程—制药化工]