Fresh Dual Presaturation Method for Analyzing H<sub>2</sub>O-Rich Samples Using Quantitative <sup>1</sup>H NMR
Fresh Dual Presaturation Method for Analyzing H<sub>2</sub>O-Rich Samples Using Quantitative <sup>1</sup>H NMR
复制标题
使用定量 <sup>1</sup>H NMR 分析富含 H<sub>2</sub>O 样品的新鲜双预饱和方法
DOI：
10.1021/acs.analchem.2c05639
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发表时间：
2023
影响因子：
7.4
通讯作者：
Saito Naoki
中科院分区：
文献类型：
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作者：
Saito Naoki
建立了一种新的双压力饱和（pre-SAT）方法，以准确地定量分析富氢样品的1h NMR谱中被抑制的水信号附近的分析物。该方法除了水预sat外，还包括一个额外的假预sat，每个分析物信号都有合适的偏移量。使用含有l-苯丙氨酸（Phe）或l-缬氨酸（Val）和3-（三甲基硅基）-1-丙磺酸-d6钠盐（DSS-d6）的D2O溶液观察4.66 ppm时的剩余HOD信号。当使用传统的单预sat方法抑制HOD信号时，在3.89 ppm时NCH信号中Phe的测量浓度最大降低了48%，而双预sat方法使NCH信号中Phe的测量浓度降低了不到3%。所提出的双预sat方法在10 vol % D2O/H2O溶液中实现了甘氨酸（Gly）和马来酸（MA）的精确定量。测定的Gly浓度为513.5±8.9 mg kg-1， MA为512.2±10.3 mg kg-1，对应的样品制备值Gly为502.9±1.7 mg kg-1， MA为506.7±2.9 mg kg-1（±后的数字表示扩展不确定度（k= 2））。
A fresh dual presaturation (pre-SAT) method was developed to quantify analytes accurately near the suppressed water signal in1H NMR spectra obtained from H2O-rich samples. The method includes an extra dummy pre-SAT with a suitable offset for each analyte signal in addition to the water pre-SAT. The residual HOD signal at 4.66 ppm was observed using D2O solutions containingl-phenylalanine (Phe) orl-valine (Val) and an internal standard of 3-(trimethylsilyl)-1-propanesulfonic acid-d6sodium salt (DSS-d6). When the HOD signal was suppressed using the conventional single pre-SAT method, the measured concentration of Phe from the NCH signal at 3.89 ppm decreased by a maximum of 48%, whereas the dual pre-SAT method gave a reduction in the Phe concentration measured from the NCH signal of less than 3%. The proposed dual pre-SAT method achieved accurate quantification of glycine (Gly) and maleic acid (MA) in a 10 vol % D2O/H2O solution. The measured concentrations of Gly of 513.5 ± 8.9 mg kg–1and MA of 512.2 ± 10.3 mg kg–1corresponded to sample preparation values of Gly of 502.9 ± 1.7 mg kg–1and MA of 506.7 ± 2.9 mg kg–1(the number after “±” indicates the expanded uncertainty (k= 2)).