Method for rapidly measuring purity of bulk pharmaceutical chemical of lincomycin hydrochloride on basis of hydrogen-nuclear magnetic resonance

Abstract

The invention discloses a method for rapidly determining the purity of lincomycin hydrochloride bulk drug based on hydrogen nuclear magnetic resonance, which comprises the following steps: (1) measuring the longitudinal relaxation time T of each quantitative target peak of lincomycin hydrochloride and an internal standard 1 ; (2) According to the measured T 1 The values ​​set the dip angle and relaxation delay time (d 1 ), the tilt angle is 30-90°, the relaxation delay time (d 1 )≥(7 / 3×T 1 max~5×T 1 max); (3) set other relevant detection parameters of nuclear magnetic resonance spectrometer, measure the integral area of ​​each quantitative target peak in lincomycin hydrochloride and internal standard, calculate lincomycin hydrochloride purity according to the following formula: W% =(m IS ×H IS ×A S × M S ×100%) / (M IS ×A IS ×H S × m S ). The invention has the advantages of simple operation, cheap and easy-to-obtain internal standard substance, accurate result and good repeatability, and the like.

Description

technical field [0001] The invention belongs to the technical field of medical analysis, and in particular relates to a detection method for rapidly determining the purity of lincomycin hydrochloride bulk drug based on hydrogen nuclear magnetic resonance. Background technique [0002] Lincomycin hydrochloride is mainly used clinically for various infections caused by sensitive bacteria, such as pneumonia, meningitis, endocarditis, tonsillitis and urinary system infections, etc. It mainly acts on the 50S subunit of ribosomes of sensitive bacteria, Prevents the elongation of the peptide chain, thereby inhibiting the protein synthesis of bacterial cells. It has a good effect on Gram-positive cocci, especially on Staphylococcus aureus and pneumococcus. At present, there are many domestic pharmaceutical companies producing injections, capsules, tablets, ointments and eye drops of this type of medicine, which are medical varieties with a good basis for clinical application. [0...

AI Technical Summary

Problems solved by technology

Yet use said method to measure lincomycin hydrochloride purity then there are following deficiencies: (1) instrument noise is high, and selectivity is poor, can't detect the impurity that may exist in the synthetic process of lincomycin hydrochloride without ultraviolet absorption; (2) Solvent residues that may exist in the sample cannot be detected, such as water, ethanol, acetonitrile, etc. It is still necessary to combine gas chromatography and other methods to deduct the solvent residue to obtain its true purity; (3) peak shape and peak time are affected by the water phase The ratio of the buffer salt and the pH value have a greater influence, which in turn affects the purity measurement results; (4) high-purity lincomycin hydrochloride standard substance is required during quantification, which is expensive, and the long-term use cost is high. Moisture absorption, pollution or degradation will seriously affect the measurement results

[0004] The proton nuclear magnetic resonance method has been widely used in the structural analysis and qualitative analysis of organic compounds due to its high sensitivity, high accuracy, and rapid analysis. However, due to the large number of parameters that affect the measurement accuracy, and the huge differences in the structure and properties of the compounds, and there is no clear rule to follow in parameter setting, it is very difficult to construct a system for accurately determining the purity of compounds based on proton nuclear magnetic resonance.

At present, there is no report on the determination of the purity of lincomycin hydrochloride raw material based on proton nuclear magnetic resonance

Images