Method for detecting content of 5,6-dimethyl benzimidazole

A technology of dimethylbenzimidazole and detection method, applied in the field of chemical analysis, can solve the problems of human body burns, strong irritation, strong corrosion, etc., and achieve the effects of high sensitivity, accurate method and good repeatability

Inactive Publication Date: 2015-08-26
宁夏泰瑞制药股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In the prior art, the content determination of 5,6-dimethylbenzimidazole adopts the perchloric acid titration method, and reagents such as glacial acetic acid and perchloric acid are used in the detection process, which are highly corrosive and irritating. There will be burns to the human body, so developing a method that can safely and accurately determine the content of 5,6 dimethylbenzimidazole has always been a problem to be solved

Method used

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  • Method for detecting content of 5,6-dimethyl benzimidazole
  • Method for detecting content of 5,6-dimethyl benzimidazole
  • Method for detecting content of 5,6-dimethyl benzimidazole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 5,6-Dimethylbenzimidazole analysis sample preparation:

[0024] Preparation of standard solution: Weigh 50 mg of 5,6-dimethylbenzimidazole standard, accurately weigh it, put it in a 100ml volumetric flask, add mobile phase to dissolve and set the volume to the mark, and shake well. Take the solution with a 1ml syringe and filter it through a 0.45um organic filter head to obtain a standard solution.

[0025] Preparation of the test solution: Weigh 50mg of 5,6-dimethylbenzimidazole sample, weigh it accurately, place it in a 100ml volumetric flask, add an appropriate amount of mobile phase, dissolve it and set the volume to the mark, and shake well. Take the solution with a 1ml syringe and filter it through a 0.45um organic filter head to obtain the test solution.

[0026] Five copies of each of the standard solution and the test solution were prepared.

[0027] Chromatographic analysis conditions: Shimadzu LC-20A liquid chromatograph, Waters C18 chromatographic column (...

Embodiment 2

[0044] Samples and standard preparations are the same as in Example 1.

[0045] Chromatographic analysis conditions: Shimadzu LC-20A liquid chromatograph, Waters C8 chromatographic column (150*4.6, 3.5um); mobile phase: methanol: disodium hydrogen phosphate solution (10g / L) (pH3.0) = (20.0 :80.0); flow rate: 0.60ml / min; detection wavelength: 260nm; injection volume 10ul, detector: ultraviolet detector; column thermostat 30°C.

[0046] According to the above-mentioned chromatographic conditions, inject samples respectively to all standard substances and test substances, such as figure 1 As shown, the peak area obtained by injecting 5 samples of the standard solution respectively is 1558746, and the RSD is 0.25%; the average value of the peak area obtained by the 5 samples of the test solution is 1498754, and the RSD is 0.31%.

[0047] According to the formula:

[0048] Content of 5,6-dimethylbenzimidazole: a=A 样 m 标 / A 标 m 样 *100%.

[0049] Using the external standard me...

Embodiment 3

[0051] Samples and standard preparations are the same as in Example 1.

[0052] Chromatographic analysis conditions: Shimadzu LC-20A liquid chromatograph, Waters C8 chromatographic column (150*4.6, 3.5um); mobile phase: methanol: disodium hydrogen phosphate solution (10g / L) (pH3.5) = (30.0 :70.0); flow rate: 1.2ml / min; detection wavelength: 276nm; injection volume 10ul, detector: ultraviolet detector; column thermostat 40°C.

[0053] According to the above-mentioned chromatographic conditions, inject samples respectively to all standard substances and test substances, such as figure 1 As shown, the peak area obtained by injecting 5 samples of the standard solution was 1432451 respectively, and the RSD was 0.30%; the average value of the peak area obtained by the 5 samples of the test solution was 1455312, and the RSD was 0.12%.

[0054] According to the formula:

[0055] Content of 5,6-dimethylbenzimidazole: a=A样 m 标 / A 标 m 样 *100%.

[0056] Using the external standard m...

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Abstract

The invention relates to a method for detecting the content of 5,6-dimethyl benzimidazole. The method is characterized in that a high-performance liquid chromatography is adopted for detection. As the high-performance liquid chromatography is adopted for detecting the content of 5,6-dimethyl benzimidazole, no strongly-corrosive and strongly-irritant solvent used in a titration method exists, and the safety and reliability are achieved; the content of 5,6-dimethyl benzimidazole in a sample is quantified according to an external standard method, so that the method provided by the invention is accurate, simple, and high in repeatability and sensitivity; a relatively good linear relationship is formed when the 5,6-dimethyl benzimidazole is between 0.1-2.0 mg / ml, and the linear correlation coefficient is 0.9996.

Description

technical field [0001] The method of the invention belongs to the field of chemical analysis, and in particular relates to a method for determining the content of 5,6-dimethylbenzimidazole by a high-performance liquid phase method. Background technique [0002] 5,6-Dimethylbenzimidazole as vitamin B 12 Synthetic exogenous precursors, added to the fermentation medium, directly bound to VB through the biosynthesis process of microorganisms 12 In the molecular structure, its own structure has not changed much, but VB 12 The output of but because of adding 5,6-dimethylbenzimidazole has greatly improved. Therefore, the level of 5,6-dimethylbenzimidazole content directly affects the VB 12 output. [0003] The structure of 5,6-dimethylbenzimidazole is as follows: [0004] [0005] In the prior art, the content determination of 5,6-dimethylbenzimidazole adopts the perchloric acid titration method, and reagents such as glacial acetic acid and perchloric acid are used in the d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 陈红丽
Owner 宁夏泰瑞制药股份有限公司
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