Impurity detection method for lansoprazole-containing raw material medicine

Abstract

The invention provides an impurity detection method for a lansoprazole-containing raw material medicine; the method comprises the specific steps: weighing the lansoprazole-containing raw material medicine, placing the lansoprazole-containing raw material medicine into a brown volumetric flask, adding methanol, and dissolving to obtain a test sample solution; measuring to take a proper amount of the test sample solution, and adding a mobile phase to obtain a control solution; weighing a proper amount of impurities A, B, D and E, adding methanol, dissolving and diluting to obtain a mixed impurity stock solution; additionally taking the mixed impurity stock solution, adding the test sample solution to be used as a system suitability solution, and carrying out liquid phase detection, wherein a peak appearing order of the impurities in chromatography is D, E, A, a lansoprazole principal component peak and B, and the retention time of the lansoprazole component peak is 10-13 min; additionally taking the control solution, carrying out liquid phase detection, and controlling the peak height of the lansoprazole component peak to be 10% of the full scale of a recorder; and then measuring to take the test sample solution, carrying out chromatographic detection, and thus completing the impurity detection of the lansoprazole-containing raw material medicine. The lansoprazole related substance determination method has an acetonitrile-water system newly developed, and the system relieves the bearing pressure of a chromatographic column and makes results more accurate.

Description

technical field [0001] The invention relates to a method for detecting drug impurities, in particular to a method for determining related substances of lansoprazole raw materials and preparations. technical background [0002] Lansoprazole raw material is independently developed and produced by the company. The dosage forms developed for clinical use include freeze-dried powder injection (lansoprazole for injection), with a specification of 30mg; and lansoprazole enteric-coated tablets with a specification of 15mg. The clinical indications are gastric ulcer, duodenal ulcer, reflux esophagitis, Zollinger-Ellison syndrome (gastrinoma), and the relevant substances recorded in the current pharmacopoeia and related literature are high-efficiency liquid phase chromatography, [0003] The determination method of related substances originally submitted by our company for approval is as follows [0004] Chromatographic conditions: use octadecylsilane bonded silica gel as filler; me...

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Problems solved by technology

[0008] (1) The methanol system is highly viscous, and the column pressure is as high as 225bar. The chromatographic column is subjected to high pressure for a long time, which will lead to the loss of column bed filler, rapid column efficiency degradation, and chromatographic peak tailing

[0009] (2) The concentration of the test solution for the determination of related substances is high (2.0mg / ml), the chromatographic column has the risk of overcapacity, the symmetry of the main component peak is poor, and the symmetry factor of the main component peak is 2.30 (should be 0.95-1.05), which does not meet the requirements , and impurity D and E overlap, impurity B and the main component peak cannot be separated by baseline

The system does not meet the requirements, and the measurement results are not accurate at all

[0010] (3) The control of the impurity limit, the maximum single impurity is no more than 0.5%, and the total impurity is no more than 1.0%, which does not meet the relevant regulations of the "Technical Guidelines for Chemical Drug Impurity Research", and the standard needs to be improved

[0011] (4) Content determination solution preparation: the existing general laboratory balance can accurately weigh up to 10 mg, and the 50 mg sample is diluted to the measurement concentration in two steps, which is complicated to operate, and multi-step dilution will lead to large deviations in the measurement results

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