Simultaneous Determination of Sodium Glycerophosphate and Phosphoric Acid in Concentrated Divitamins and Sodium Phosphate Syrup by Quantitative 31P-Nuclear Magnetic Resonance
10.19756/j.issn.0253-3820.231315
- VernacularTitle: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
- Author:
Xiang-Tu TU
1
;
Jun LI
;
Hong LEI
;
Ling-Ping XU
;
Mao-Fa ZENG
Author Information
1. 台州市食品药品检验研究院,台州 318000
- Keywords:
Quantitative 31P-nuclear magnetic resonance;
Concentrated divitamins and sodium phosphate syrup;
Sodium glycerophosphate;
Phosphoric acid
- From:
Chinese Journal of Analytical Chemistry
2024;52(7):1020-1027
- CountryChina
- Language:Chinese
-
Abstract:
A 31P-quantitative nuclear magnetic resonance(qNMR)method was established for simultaneous determination of sodium α-glycerophosphate,sodium β-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 31P-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(23.58 μg/mL for sodium glycerophosphate and 11.61 μg/mL for phosphoric acid)and limit of quantitation(78.60 μg/mL for sodium glycerophosphate and 38.70 μg/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 31P-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.
