Detection method of higenamine hydrochloride injection related substances

A technology of higenamine hydrochloride and injection, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of undetectable degraded impurities, etc., and achieve the effects of short time, high precision and good stability

Inactive Publication Date: 2019-11-12
珠海润都制药股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The method discloses a method for determining the related substances of higenamine hydrochloride, which can measure the impurities of higenamine hydrochloride and its intermediates, but higenamine hydrochloride can be degraded under alkaline and oxidative conditions Impurities, these degraded impurity peaks overlap with the peaks of excipients in higenamine hydrochloride injection, and the original detection method cannot detect the degradation impurities in higenamine hydrochloride injection that overlap with the peaks of excipients

Method used

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  • Detection method of higenamine hydrochloride injection related substances
  • Detection method of higenamine hydrochloride injection related substances
  • Detection method of higenamine hydrochloride injection related substances

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0078] (1) Experimental materials and instrument conditions

[0079] Instrument: High Performance Liquid Chromatography: Agilent 1260; Chromatographic Column: CAPCELL PAK C18 MG (S-5) 4.6mm×250mm; Flow Rate: 1.0ml / min; Column Temperature: 30°C; Injection Volume: 20μl; Detection Wavelength: 284nm, mobile phase: A2: 0.05% EDTA disodium solution; mobile phase B2: methanol;

[0080]

[0081] (2) Experimental steps

[0082] Diluent: 0.05% EDTA disodium solution;

[0083] Blank solution 2: diluent;

[0084] Reference solution: Accurately weigh 25mg of higinarine hydrochloride reference substance, put it in a 50ml measuring bottle, add diluent to dissolve and dilute to the mark, and shake well. Accurately measure 1.0ml, put it in a 100ml measuring bottle, add diluent to dilute to the mark, and shake well.

[0085] Sensitivity solution: Accurately measure 1.0ml of reference solution, put it in a 20ml measuring bottle, add diluent to dilute to the mark, and shake well.

[0086]...

Embodiment 2

[0107] Embodiment 2 detection method system applicability test of the present invention

[0108] The system suitability was checked at the beginning of the sequence; the system suitability was realized by measuring the repeatability of the reference solution, and the RSD% of the peak area of ​​higenamine hydrochloride in the reference solution was less than or equal to 10.0%. At the same time, the signal-to-noise ratio of the main peak of the sensitivity solution is required to be greater than or equal to 10. Prepare blank solution 2, auxiliary material blank solution, reference solution, and sensitivity solution as described in Example 1. After the system is stable, run the system gradient blank once, and then enter blank solution 2 for 1 needle, auxiliary material blank solution for 1 needle, and refer to 5 needles of specific solution, 1 needle of sensitivity solution, and record the chromatogram.

[0109]

Embodiment 3

[0110] Embodiment 3 Detection method specificity test of the present invention

[0111] The specificity research of the method investigates the peak identification and selectivity, and the separation between the main peak and the adjacent impurity peaks is required to be ≥1.5, the signal-to-noise ratio (S / N) of the sensitivity solution is ≥10, and the blank solvent has no obvious interference to the detection. After the system is balanced, inject 1 needle of blank solution 2, 1 needle of reference solution, 1 needle of excipient blank solution, 1 needle of impurity A reference solution, 1 needle of impurity B reference solution, 1 needle of mixed reference solution, and test solution S1 needle, test solution P 1 needle, record the chromatogram, and obtain the specificity detection results as follows.

[0112]

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Abstract

The invention belongs to the field of drug analysis technologies and relates to a detection method of higenamine hydrochloride injection related substances. According to the detection method, a high-performance liquid chromatographic method which is convenient and fast to use is utilized to detect the higenamine hydrochloride injection related substances, and the detection method can be used for detecting the mass of a higenamine hydrochloride injection; the chromatographic peak separation degree of the higenamine hydrochloride injection related substances to which auxiliary materials are added is high, high system applicability is achieved, and meanwhile the specificity, precision and solution stability all conform to standards; the detection method, capable of eliminating auxiliary material interference, of the higenamine hydrochloride injection related substances is proposed for the first time and has the advantages of being high in accuracy, high in precision, good in reproducibility, good in stability, high in specificity and the like; and meanwhile the detection method is easy to operate, short in time consumption and low in cost.

Description

technical field [0001] The invention relates to a method for testing related substances in higenamine hydrochloride injection, which belongs to the technical field of drug analysis. Background technique [0002] Higenamine hydrochloride, English name: higenamine hydrochloride, chemical name: 1-(4-hydroxy-benzyl)-6,7-dihydroxy-1,2,3,4-tetrahydroisoquinoline hydrochloride Salt, molecular formula: C 16 h 17 NO 3 .HCl, the chemical structure is as follows: Higendaline hydrochloride has characteristics similar to dobutamine. It is a clinical myocardial stress test drug with development prospects, which can increase heart rate, reduce diastolic blood pressure, increase left ventricular ejection fraction, and improve sinus node conduction function. Improvement, good curative effect on sinus bradycardia, myocardial contractility significantly enhanced. [0003] During the preparation and storage of drugs, the analysis and detection of possible impurities is very important for ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/36G01N30/74G01N30/86
CPCG01N30/02G01N30/06G01N30/36G01N30/74G01N30/8679G01N2030/027
Inventor 姜春来黄俊鹏陈新民刘杰谢斌关东兰柳琴
Owner 珠海润都制药股份有限公司
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