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Determination of Reference Standards of Four Moxifloxacin Hydrochloride Impurities by Quantitative Proton Nuclear Magnetic Resonance
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Yu HE, Yajun ZHANG, Jingxin XIE, Qing WANG, Changjun SHAO, Huimin SUN, Yong LU*, Xianfu WU*
Chinese Pharmaceutical Journal | 2024, 59(12) : 1151 - 1155
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Chinese Pharmaceutical Journal | 2024, 59(12): 1151-1155
Determination of Reference Standards of Four Moxifloxacin Hydrochloride Impurities by Quantitative Proton Nuclear Magnetic Resonance
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Yu HE, Yajun ZHANG, Jingxin XIE, Qing WANG, Changjun SHAO, Huimin SUN, Yong LU*, Xianfu WU*
Affiliations
  • National Institutes for Food and Drug Control, Beijing 102629, China
Published: 2024-06-22 doi: 10.11669/cpj.2024.12.011
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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.

quantitative proton nuclear magnetic resonance  /  moxifloxacin hydrochloride impurity  /  reference standard  /  characterization  /  content determination
Yu HE, Yajun ZHANG, Jingxin XIE, Qing WANG, Changjun SHAO, Huimin SUN, Yong LU, Xianfu WU. Determination of Reference Standards of Four Moxifloxacin Hydrochloride Impurities by Quantitative Proton Nuclear Magnetic Resonance[J]. Chinese Pharmaceutical Journal, 2024 , 59 (12) : 1151 -1155 . DOI: 10.11669/cpj.2024.12.011
Year 2024 volume 59 Issue 12
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doi: 10.11669/cpj.2024.12.011
  • Receive Date:2023-12-11
  • Online Date:2025-11-25
  • Published:2024-06-22
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  • Received:2023-12-11
Affiliations
    National Institutes for Food and Drug Control, Beijing 102629, China
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表12种不同金属材料的力学参数

Family
属数
Number of
genus
种数
Number of
species
占总种数比例
Percentage of
total species (%)

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
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