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Method for determining content of cyclovirobuxine D

The technology of cyclovirobuxine and cyclovirobuxine is applied in the field of high-performance liquid chromatography determination method of pre-column derivatization, and can solve the problems of poor separation effect, undetermined appropriate dosage of derivatizing agent phenyl isocyanate, and the like, To achieve the effect of saving reagents, simple method and good reproducibility

Inactive Publication Date: 2007-01-03
GUANGZHOU CHEN LI JI PHARMA FACTORY
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

However, there are shortcomings such as poor separation of samples and impurities, and undetermined appropriate dosage of derivatizer phenyl isocyanate.

Method used

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  • Method for determining content of cyclovirobuxine D
  • Method for determining content of cyclovirobuxine D
  • Method for determining content of cyclovirobuxine D

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Embodiment 1 (crude drug: provided by Henan Longdu Pharmaceutical Factory)

[0035] Content determination was checked according to high performance liquid chromatography (Appendix VID of the Pharmacopoeia of the People's Republic of China in 2005).

[0036] Chromatographic conditions and system adaptability Octadecylsilane bonded silica gel was used as filler; acetonitrile-water (volume ratio 70:30) was used as mobile phase; detection wavelength was 242nm. The number of theoretical boards should not be less than 5000 based on the calculation of the D peak of the ring-dimensional boxwood star.

[0037] Preparation of phenyl isocyanate test solution Precisely measure 0.1ml of phenyl isocyanate, put it in a 100ml measuring bottle, add chloroform to the mark, shake well, and you get it.

[0038] Preparation of Reference Substance Solution Accurately weigh an appropriate amount of cyclovirbuxine D reference substance dried at 105°C to constant weight, add chloroform to make...

Embodiment 2

[0041] Embodiment 2 (crude drug: provided by Jiangsu Dongtai Shentian Botanical Medicine Co., Ltd.)

[0042] Content determination was checked according to high performance liquid chromatography (Appendix VID of the Pharmacopoeia of the People's Republic of China in 2005).

[0043]Chromatographic conditions and system adaptability Octadecylsilane bonded silica gel was used as filler; acetonitrile-water (volume ratio 70:30) was used as mobile phase; detection wavelength was 242nm. The number of theoretical boards should not be less than 5000 based on the calculation of the D peak of the ring-dimensional boxwood star.

[0044] Preparation of phenyl isocyanate test solution Precisely measure 0.1ml of phenyl isocyanate, put it in a 100ml measuring bottle, add chloroform to the mark, shake well, and you get it.

[0045] Preparation of Reference Substance Solution Accurately weigh an appropriate amount of cyclovirbuxine D reference substance dried at 105°C to constant weight, add c...

Embodiment 3

[0048] Embodiment 3 (dropping pills: provided by Guangzhou Chenliji Pharmaceutical Factory, made by the patent No. 03126723.8 technical scheme)

[0049] Content determination was checked according to high performance liquid chromatography (Appendix VID of the Pharmacopoeia of the People's Republic of China in 2005).

[0050] Chromatographic conditions and system suitability test Octadecylsilane bonded silica gel was used as filler; acetonitrile-water (volume ratio 70:30) was used as mobile phase; detection wavelength was 242nm. The number of theoretical boards should not be less than 5000 based on the calculation of the D peak of the ring-dimensional boxwood star.

[0051] Preparation of phenyl isocyanate test solution Precisely measure 0.1ml of phenyl isocyanate, put it in a 100ml measuring bottle, add chloroform to the mark, shake well, and you get it.

[0052] Preparation of Reference Substance Solution Accurately weigh an appropriate amount of cyclovirbuxine D reference s...

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Abstract

A High Performance Liquid Chromatography (HPLC) test method for testing the content of cyclovirobuxine-D in material and all kinds of dosage form (Huangyangningdiwan and so on) by pre-column deri-vatization, and the derivatizing reagent is isocyanic phenyl ester. Test each 0.2mg cyclovirobuxine-D with 1 mul / ml isocyanic phenyl ester solution 0.05- 0.6ml with the acetonitrile-water system as mobile phase with ultraviolet inspector. It can exactly test the content of cyclovirobuxine-D in material and all kinds of dosage form with easy operation, high precision, measurable dosage of derivatizing reagent and little side-effect.

Description

technical field [0001] The invention relates to a method for determining the content of cyclovir buxicine D in raw materials and various dosage forms (such as huangyangning dripping pills, huangyangning tablets, etc.), specifically a kind of pre-column derivatization High-performance liquid chromatography method, and the use of ultraviolet detector detection. technical background [0002] Buxus D is a total alkaloid extracted from Buxs mincrophylla Sieb.etZucc.var.sinica Rehd.et Wils. and plants of the same genus (the raw material of Buxus D, also known as Boxus Ning) in the main ingredient. There is no conjugated double bond in its chemical structure, so it has no absorption in the ultraviolet region, so it cannot be tested directly with an ultraviolet detector. [0003] At present, the 2005 edition of the Pharmacopoeia, page 276, uses a non-aqueous titration method for the determination of the content of cyclovirboxicin D. Although this method is simple, it has poor spec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/60G01N30/02G01N33/15
Inventor 何风雷许招懂杨能英王冰
Owner GUANGZHOU CHEN LI JI PHARMA FACTORY
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