A kind of detection method of cinnarizine related substance

A technology of related substances and detection methods, which is applied in the detection field of cinnarizine-related substances, can solve the problems of unrecorded cinnarizine, etc., and achieve the effect of accurate and reliable results, simple method and high separation degree

Active Publication Date: 2021-02-19
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the Chinese Pharmacopoeia does not record the detection methods of cinnarizine-related substances. With the improvement of the requirements for drug quality control in my country, the establishment of standards and detection methods for related substances has become the key to improve and better control the quality of cinnarizine. Urgent request

Method used

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  • A kind of detection method of cinnarizine related substance
  • A kind of detection method of cinnarizine related substance
  • A kind of detection method of cinnarizine related substance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] instrument:

[0035] High performance liquid chromatography, Waters, 2695-2487; electronic balance, SQP; pH meter, Shanghai Jingke PHS-3C.

[0036] Reagent:

[0037] Acetonitrile (chromatographically pure), Anhui Shilian Special Solvent Co., Ltd.; methanol (chromatographically pure), Anhui Shilian Special Solvent Co., Ltd.; glacial acetic acid (analytical pure), Tianjin Yongda Chemical Reagent Co., Ltd.; ammonium acetate (analytical pure) , Tianjin Yongda Chemical Reagent Co., Ltd.

[0038] Chromatographic conditions:

[0039] Chromatographic column: Venusil XBP C18 (4.0×100mm); flow rate, 1.0ml / min; detection wavelength, 230nm; sample concentration, 2.5mg / ml; injection volume, 10μl.

[0040] mobile phase:

[0041] Phase A: 10g / L ammonium acetate solution (pH5.0); Phase B: 0.02% glacial acetic acid in acetonitrile solution.

[0042] Elution was performed according to the following gradient program:

[0043] .

[0044] Solution preparation:

[0045] Preparation...

Embodiment 2

[0080] Chromatographic conditions:

[0081] Chromatographic column: Venusil XBP C18 (4.0×100mm); flow rate, 0.8ml / min; detection wavelength, 230nm; sample concentration, 2.5mg / ml; injection volume, 10μl.

[0082] Others are all the same as in Example 1.

[0083] Precisely measure 10 μL each of the blank solvent, mixed reference solution, test solution and control solution, inject them into the liquid chromatograph, and record the chromatograms.

[0084] The detection results of related substances in the mixed reference solution are shown in Table 7, and the obtained HPLC collection of samples is shown in Table 7. Figure 4 ,pass Figure 4 It can be seen that all impurity peaks have been completely separated, and eight impurity peaks with retention times (t) of 2.619, 5.344, 10.942, 11.932, 13.208, 14.069, 17.953, and 22.073min were separated, especially those with the main The component peak (t=10.942min) is completely separated from the impurity peak impurity B (t=11.932mi...

Embodiment 3

[0094] Chromatographic conditions:

[0095] Chromatographic column: Venusil XBP C18 (4.0×100mm); flow rate, 1.2ml / min; detection wavelength, 230nm; sample concentration, 2.5mg / ml; injection volume, 10μl.

[0096] Others are all the same as in Example 1.

[0097] Precisely measure 10 μL each of the blank solvent, mixed reference solution, test solution and control solution, inject them into the liquid chromatograph, and record the chromatograms.

[0098] The detection results of related substances in the mixed reference solution are shown in Table 10, and the resulting HPLC spectrum is shown in Table 10. Figure 7 ,pass Figure 7 It can be seen that all impurity peaks have been completely separated, and eight impurity peaks with retention times (t) of 1.767, 3.939, 9.318, 10.013, 11.009, 12.270, 15.597, and 19.572min were separated, especially those with the main The impurity peak impurity B (t=10.013min) adjacent to the component peak (t=9.138min) has been completely separa...

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Abstract

The invention provides a method for detecting related substances of cinnarizine. The method is high-performance liquid chromatography, adopts C18 chromatographic column to implement separation, and utilizes ultraviolet detector to carry out quantitative analysis. The chromatographic conditions are: ammonium acetate solution is used as the flow Phase A, with acetonitrile solution of glacial acetic acid with a volume percentage of 0.2% as mobile phase B, gradient elution was carried out, wherein the concentration of ammonium acetate solution was 10g / L, pH=4.8-5.2; flow rate was 0.8-1.2mL / min; detection wavelength is 225-235nm. The method of the invention can effectively separate the impurities of cinnarizine, has high separation degree, is simple and easy to operate, has accurate and reliable results, good reproducibility and high sensitivity. The invention fills up the gap in the field of detection of related substances of cinnarizine in Chinese Pharmacopoeia, and provides reliable guarantee for improving and better controlling the quality of cinnarizine products.

Description

technical field [0001] The invention relates to a method for detecting impurities in medicine, in particular to a method for detecting related substances of cinnarizine. Background technique [0002] Cinnarizine (English name: Cinnarizine, molecular formula: C 26 h 28 N 2 , molecular weight: 368.52) is white or off-white crystal or crystalline powder, odorless, soluble in chloroform, soluble in boiling ethanol, almost insoluble in water. [0003] Cinnarizine, also known as Naoyizine and Cinnarizine, acts on vascular smooth muscle to dilate blood vessels and significantly improve blood circulation. Moreover, it has antagonistic effects on various vasoconstrictor substances (such as: 5-hydroxytryptamine, epinephrine, vasopressin, etc.), can relieve vasospasm, and has the effect of preventing vascular embrittlement at the same time. It is clinically applicable to the treatment of cerebral thrombosis, cerebral embolism, cerebral arteriosclerosis, cerebral hemorrhage recovery...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/34G01N30/74
CPCG01N30/02G01N30/34G01N30/74
Inventor 李志伟孙盺刘亚丽马欣宁赵盼琢张晓晓刘玉真姚军
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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