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Detection method for cis-isomer in vitamin K2 medicine

A cis-isomer and detection method technology, applied in the field of detection of vitamin K2 drug impurities, can solve the problems of low precision, inability to accurately control the content of cis-isomer, poor specificity, etc., achieve high sensitivity, facilitate Promotional use, good specific effect

Inactive Publication Date: 2009-07-01
天津康鸿医药科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the limitations of this method are as follows: poor specificity, low precision, incapable of accurate detection and quantification, and thus unable to accurately control the content of cis-isomers in medicines

Method used

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  • Detection method for cis-isomer in vitamin K2 medicine
  • Detection method for cis-isomer in vitamin K2 medicine
  • Detection method for cis-isomer in vitamin K2 medicine

Examples

Experimental program
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Embodiment 1

[0015] HPLC analysis conditions: HPLC analysis adopts high performance liquid chromatograph Waters 2695_996 equipped with diode array detector, and Agilent Prep-SIL (5μm4.6×250mm) silica gel column of Agilent Company. The mobile phase was n-hexane-n-butyl ether (volume ratio 95:5), the detection wavelength was 270nm, and an autosampler was used to inject 20 μl each time.

[0016] Respectively take an appropriate amount of menadione trans isomer and cis isomer, accurately weigh, and use the above-mentioned mobile phase to prepare a solution with a concentration of 1 mg / ml, analyze using the above-mentioned instruments and conditions, and obtain the HPLC chromatogram, Such as figure 1 shown. Under this chromatographic condition, the retention time of the trans isomer of menadione is 22.863min, the retention time of the cis isomer of menadione is 19.958min, and the separation degree of the two is greater than 1.5, which can reach Baseline separation.

Embodiment 2

[0018] Get 3 parts of menadione products as samples, analyze according to the HPLC analysis conditions in Example 1, calculate according to the cis-isomer peak area and the contrast solution peak area in the liquid chromatogram obtained, by external standard method Content of cis isomer. Table 1 shows the test results of the three samples. As can be seen from Table 1, there is little difference in the cis-isomer content in them, but they are all lower than the detection limit (2% ).

[0019] Table 1 Content of cis isomer in samples

[0020]

Embodiment 3

[0022] Take a 1mg / ml menadione sample solution, add hydrochloric acid solution, sodium hydroxide solution, and hydrogen peroxide solution respectively to carry out acid, alkali, and oxidative destruction reactions. Take 1mg / ml menatetrenone sample solution, heat in a water bath, and carry out thermal destruction reaction. Take a 1mg / ml menadione sample solution and expose it to light for several hours to carry out photodestruction reaction. The above reaction solution was analyzed using the HPLC analysis conditions in Experimental Example 1.

[0023] The purpose of this test is to investigate the sensitivity of the sample to acid, alkali, oxidation, heat, light and the content change of the cis-isomer, and then determine whether the chromatographic conditions used can accurately detect the content of the cis-isomer so as to fully control the product quality. The quality and test results are shown in Table 2. It can be seen from the results that the menatetrenone solution is ...

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Abstract

The invention provides a high efficiency liquid chromatography detection method for cis isomer in vitamin K2 medicines, which adopts a normal phase chromatography column stuffed by silica gel, and a flow phase formed by one low-polarity solvent selected from hexane, pentane, petroleum ether, cyclohexane, isooctane and heptane, and one high-polarity solvent selected from butyl ether, isopropanol, pentanol, n-pentanol, tetrahydrofuran, dichloromethane and ethanol. The high efficiency liquid chromatography detection method has high sensitivity and specialization, having simple operation, high repeatability, which is beneficial for controlling the quality of raw materials and agents in production.

Description

technical field [0001] The invention relates to a method for detecting impurities in vitamin K2 drugs, in particular to a method for detecting cis-isomers in vitamin K2 drugs. Background technique [0002] With the extension of human life span, population aging has brought new problems to human health. Osteoporosis and the fractures it causes rank seventh among the current common diseases, seriously threatening the health of middle-aged and elderly people. [0003] Studies have confirmed that vitamin K2 drugs have osteogenic effects, promote calcium metabolism, and at the same time inhibit bone resorption caused by osteoclasts, thereby increasing bone density and preventing osteoporosis. Menatetrenone, as a kind of vitamin K2 drugs, has a strong procoagulant effect (approved in 1972 as a procoagulant drug). Menatetrenone also has two effects of promoting osteogenesis and inhibiting bone resorption. It can not only activate osteoblasts and promote calcification, but also in...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 宋丽明邹美香蒋庆峰孙歆慧蔡振华吴疆夏锦辉金松子刘谨
Owner 天津康鸿医药科技发展有限公司
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