Studies On The Quantitative Analysis Of Several Phosphorus-containing Compounds By ³¹P NMR

Phosphorus is indispensable to the growth and development of animals and plants.Phosphorus-containing compound are in a wide rage of present in samples of foods,medicines,phosphate fertilizers samples,they are closely related to industrial and agricultural production and people's lives.Therefore,it is of great practical significance to establish a rapid and effective method for analyzing phosphorus-containing compounds.Nuclear Magnetic Resonance Phosphorus Spectroscopy(³¹P NMR)is an analysis and detection technique widely used for qualitative and quantitative analysis of phosphorus-containing compounds.These signals of phosphorus atoms are generated by ³¹P NMR without interferential signals of other atoms,which is fast and accurate.In this paper,³¹P NMR spectrum is used to detect the contents of phosphorus in several drugs,chemical products and phosphate fertilizers.In a word,it is very reliable for the analysis and detection of phosphorus compounds because of its good resolution,high accuracy and good reproducibility.The main research contents of this paper are as follows:1.A method for simultaneous detection of the main components and related substances of the drugs etidronate disodium?ED?and citicoline sodium by ³¹P NMR was established.Good linearity was achieved for etidronate disodium,phosphite,phosphate in the range of 0.00125?0.400,0.00125?0.400 and 0.001?0.400 mol·L^-1,respectively.The RSD value of precision was 0.10%?0.43%and the average recovery of the tablets were 99.2%?101.8%.The method was applied to determination of etidronate disodium tablets,the related substances of etidronate disodium tables were phosphate and phosphite,and the content of etidronate disodium was in line with the requirement of the pharmacopoeia.The content of citicoline sodium and its impurities cytidine 5'-monophosphate and calcium phosphorylcholine chloride were determined by ³¹P NMR,the linear range of citicoline sodium were found to be 0.005?0.080mol·L^-1,and the cytidine 5'-monophosphate and calcium phosphorylcholine chloride were 0.0025?0.080 mol·L^-1,respectively.The RSD was 0.28%?0.53%and the recovery was 99.15%?100.92%.This method was applied to determination of citicoline sodium capsules,the content of the main component of citicoline sodium in citicoline sodium capsules was 98.59%,and the content of phosphorus-containing impurities was below the detection limit.2.The content of main components and impurities in chemical products sodium hypophosphite and phosphorous acid were determined by ³¹P NMR.Good linearity was achieved for phosphate,phosphite and Hypophosphite in the range of 0.001?0.200,0.005?0.400 and 0.01?0.400 mol·L^-1,respectively.The RSD was 0.03%to 0.15%and the recovery was 98.37%to 100.13%.the impurities of sodium hypophosphite were phosphate and phosphite.The contents of phosphorous acid and impurities phosphoric acid in phosphorous acid chemical products were determined by ³¹P NMR with internal standard method.The RSD was 0.09%to 0.25%and the recovery was 98.44%to99.94%.These results indicated that the method was good reproducibility and high accuracy.3.The superphosphate phosphate fertilizer was extracted according to the method of GB,and the content of water-soluble phosphorus,weak acid-soluble phosphorus and strong acid-soluble phosphorus in the superphosphate phosphate fertilizer were determined by ³¹P NMR as30.44 mg,98.24 mg,614.74 mg.As a result,the content of available phosphorus and total phosphorus in the superphosphate phosphate fertilizer can be obtained,and the results of RSD and recovery were good.