Method for determination of moxidectin content by <1>H-NMR
A technology of proton nuclear magnetic resonance spectroscopy and moxiketine, which is applied in the direction of analysis by using nuclear magnetic resonance, can solve the problems of high price, pollution, moisture absorption, etc., and achieve the effect of simple, accurate and repeatable
Active Publication Date: 2015-02-04
内蒙古佳瑞米精细化工有限公司
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Problems solved by technology
Due to the high price of standard samples, the long-term use cost is high, and even a small amount of moisture absorption, pollution or degradation of standard samples during storage will seriously affect the measurement results
Method used
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Embodiment 1
[0031] Weigh 99.20 mg of moxictine sample and 17.90 mg of 1,3,5-trimethylbenzene into the sample bottle, add CDCl 3 1mL, ultrasonic vibration for 1 minute to dissolve it, and then remove 74.0mg solution to 0.5mL CDCl 3 After mixing evenly, transfer to the NMR sample tube for 1 H-NMR test.
Embodiment 2
[0033] Weigh 99.86mg of moxictine sample and 12.80mg of hydroquinone into the sample bottle, add d 6 - DMSO1mL, ultrasonic vibration for 2 minutes to dissolve it, and then take out 65.0mg solution to 0.5mL d 6 - in DMSO, mix well and transfer to NMR sample tube for 1 H-NMR test.
Embodiment 3
[0035] Weigh 100.10 mg of moxictine sample and 8.06 mg of 1,3,5-trioxane into the sample bottle, add d 6 - DMSO 1mL, ultrasonic vibration for 2 minutes to dissolve it, and then take out 65.0mg solution to 0.5mL d 6 - in DMSO, mix well and transfer to NMR sample tube for 1 H-NMR test.
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Abstract
Belonging to the technical field of nuclear magnetic resonance detection methods, the invention discloses a method for determination of moxidectin content by <1>H-NMR. The method includes: adopting a cheap and easily obtainable compound as the internal standard, dissolving the internal standard substance and a moxidectin sample with a known liquid chromatogram normalized content in a deuterated reagent together, conducting dilution by the same deuterated reagent to certain concentration, then transferring the obtained solution into a nuclear magnetic sample tube to perform <1>H-NMR test, then carrying out integration on the quantitative peaks of the internal standard substance and moxidectin in the spectrogram respectively, introducing the obtained data into a calculation formula to conduct calculation, thus obtaining the moxidectin content, which is accord with the liquid chromatogram external standard detection method result provided by European Pharmacopoeia. The invention provides the new moxidectin content determination method, which has the advantages of cheap and easily obtainable internal standard substance, simplicity and accuracy and good reproducibility, etc.
Description
technical field [0001] The invention relates to the technical field of nuclear magnetic resonance detection methods, in particular to a method for determining the content of moxictine by proton nuclear magnetic resonance spectroscopy. The method is suitable for the detection of samples with a moxictine content of more than 70 wt.%. Background technique [0002] Moxictine is a single-component, semi-synthetic macrolide drug produced by Streptomyces fermentation. It has good anthelmintic activity, long-acting, and safe properties. It is currently widely used in veterinary clinics. Broad-spectrum, high-efficiency, new macrolide anthelmintic antibiotic (see: Parasites&Vectors 2009, 2(Suppl2), S5). The content of moxictine has been determined by high performance liquid chromatography (see: European Pharmacopoeia, 7th edition, 2010, 2529-2531; CN103399115, 2013) using a standard product with known content as an external standard. Due to the high price of standard samples, the lon...
Claims
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Inventor 戴耀李贺先林诚辉王荣良
Owner 内蒙古佳瑞米精细化工有限公司