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The Analysis Of Form And Content Of Phosphorus In Several Phosphorus-containing Substances By 31P NMR

Posted on:2016-05-21Degree:MasterType:Thesis
Country:ChinaCandidate:J LuoFull Text:PDF
GTID:2271330461494009Subject:Analytical Chemistry
Abstract/Summary:PDF Full Text Request
Phosphorus is a common chemical element, which is the component of nucleic acids, enzymes, biological membrane, bones, teeth and so on. It plays an important role in growth, energy metabolism. Phosphoruscontaining compound are in a wide range of foods, medicines, and environmental samples, which are very important for people’s lives. Therefore, to establish a rapid and effective method to analyze phosphorus-containing compounds is important to improve people′s lives.31P NMR is a widely used method of analyzing phosphoruscontaining compounds due to it is rapid, simple, and no interference, thus providing an enlarged signal-to-background ratio and improved sensitivities. More importantly, 31 P NMR only responses to phosphorus atom. In this paper, qualitative and quantitative analysis of phosphoruscontaining compounds in foods, medicines, pesticides and soils were developed base on 31 P NMR. These results indicated that this method possess several unique qualities, such as good reproducibility, high accuracy, and simple operation, without pretreatment, which is a new and reliable method of analyzing phosphorus-containing compounds. The main contents are summarized as follows:1.The content of ATP, ADP, AMP, sodium phosphate and sodium pyrophosphate were determined by 31 P NMR. The linear range of ATP, ADP, AMP were found to be 0.004 mol·L-1~0.080 mol·L-1, and the sodium phosphate and sodium pyrophosphate were 0.005mol·L-1~0.100 mol·L-1, respectively. The RSD were 0.40%~1.30% and the recovery were 96.9%~105.2%. The method has been applied to determination of ATP injection, the impurities of ATP injection were ADP and sodium phosphate, the content of ATP in line with the requirement of the pharmacopoeia.2. The content of methidathion, pirimiphos-methyl, profenofos and glufosinate-ammonium was determined by 31 P NMR with internal standard method. The experimental results exhibited that recoveries of this method reached 97.1% to 106.5% with relative standard deviations(RSDs) of 0.18% to 0.34%.The result of 31 P NMR was similar to the result of 1H NMR.3. The content of sodium tri-polyphosphate, sodium meta-phosphate, sodium pyrophosphate, sodium phosphate were determined by 31 P NMR. The experimental results exhibited that recoveries of this method reached 98.8% to 105.4% with relative standard deviations(RSDs) of 0.17% to 0.39%. These results indicated that the method was of good reproducibility and high accuracy. The method has been successfully applied to real samples. The impurities of sodium tri-polyphosphate were sodium meta-phosphate, sodium pyrophosphate and sodium phosphate and The impurities of sodium meta-phosphate were sodium pyrophosphate and sodium phosphate.4. Noodles, instant noodles and soils were pretreatment according to the method of GB for the determination of total phosphorus. The content was determined by 31 P NMR, and the result of RSD and recovery was good.
Keywords/Search Tags:31P NMR, phosphorus-containing substance, qualitative and quantitative, impurity
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