To establish a low-field and high-field nuclear magnetic resonance (NMR) technique for the determination of pyridoxine hydrochloride. To compare the differences between the results of method validation and sample content.
Using deuterated water as the solvent and maleic acid as the internal standard,method validation of quantitative nuclear magnetic resonance (qNMR) was accomplished with both 80 MHz low-field NMR and 500 MHz high-field NMR instruments. The content of pyridoxine hydrochloride was also determined.
The linearity of pyridoxine hydrochloride was good in the range of 10-30 mg·mL-1,and the linear correlation coefficients were 0.999 8 and 0.999 6 for the low-field and high-field NMR,respectively. RSDs of the low-field and high-field NMR measurements were 1.4% and 0.040%,respectively. The contents were 100.4% and 100.8%,which were in agreement with the results from the mass balance method (100.0%). And the repeatability RSD was 0.20%. For the same concentration of the sample,the signal-to-noise ratio (S/N) of high-field NMR was about 100 times that of low-field NMR,and the half-peak width was 1/15 of that of low-field NMR.
Both low-field and high-field NMR instruments gave accurate results in the determination of pyridoxine hydrochloride content. However,low-field NMR was only suitable for compounds with simple structures. In the actual content determination,it is necessary to choose the appropriate instrument according to the structure and solubility of the sample to be tested.
| 科 Family | 属数 Number of genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) | 属 Genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) |
|---|---|---|---|---|---|---|
| 鹅膏菌科Amanitaceae | 2 | 11 | 5.26 | 鹅膏菌属 Amanita | 10 | 4.78 |
| 小菇科 Mycenaceae | 2 | 12 | 5.74 | 丝盖伞属 Inocybe | 5 | 2.39 |
| 多孔菌科 Polyporaceae | 8 | 14 | 6.70 | 蜡蘑属 Laccaria | 5 | 2.39 |
| 红菇科 Russulaceae | 3 | 23 | 11.00 | 小皮伞属 Marasmius | 6 | 2.87 |
| 小菇属 Mycena | 11 | 5.26 | ||||
| 光柄菇属 Pluteus | 5 | 2.39 | ||||
| 红菇属 Russula | 17 | 8.13 | ||||
| 栓菌属 Trametes | 5 | 2.39 |