OBJECTIVE To establish a quantitative proton nuclear magnetic resonance (qHNMR) method for determination of the reference standards of moxifloxacin hydrochloride impurities A, B, C and D. METHODS Proton nuclear magnetic resonance (1H-NMR) spectra of four reference standards of impurities were obtained in dimethylsulfoxide-d6 (DMSO-d6) or chloroform-d (CDCl3) using a nuclear magnetic resonance spectrometer. The internal standard was 1,3,5-trimethoxybenzene. All 1H-NMR spectra for quantitative analysis were measured with noesyigld1d pulse sequence using the following experimental parameters: 32 number of scans (NS), relaxation delay time (D1) of 30 s, 25 ℃ testing temperature. RESULTS The quantitative peak signals of four moxifloxacin hydrochloride impurities and 1, 3, 5-trimethoxybenzene were well separated on 1H-NMR spectra, and the linear relationship was good within the linear range (r2>0.999 4). The injection precision and repeatability of the method were good. The contents of four reference standards of impurities determined by qHNMR method were basically consistent with those determined by mass balance method. CONCLUSION The established qHNMR method is accurate, reliable, simple, fast, which provides a new way for content determination of these impurities and can also be used as a mutual verification method for the calibration results of these reference substance by the mass balance method.
| 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 |