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High performance liquid chromatography detection method for hydroxyiminobarbituric acid and related matters thereof

A technology of high performance liquid chromatography and related substances, applied in the field of drug analysis, can solve the problems of inability to detect, weak absorption of impurities, etc., and achieve the effects of low cost, high accuracy and precision, and good stability and reproducibility

Active Publication Date: 2018-08-17
XINHUA PHARM (SHOUGUANG) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] (2) Some impurities absorb very weakly under this condition and cannot be detected

Method used

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  • High performance liquid chromatography detection method for hydroxyiminobarbituric acid and related matters thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Experimental Equipment and Reagents

[0026] (1) Experimental equipment:

[0027] Instrument: Shimadzu 20A with UV detector

[0028] (2) Chromatographic conditions:

[0029] Chromatographic column: ZORBAX SB-Phenyl C18 column, 4.6×250mm, 5μm;

[0030] Flow rate: 1.0ml / min;

[0031] Detection wavelength: 205nm;

[0032] Column temperature: 30°C;

[0033] Injection volume: 20μl

[0034] Mobile phase: A: 0.2% (V / V) triethylamine aqueous solution, adjust pH=3.0 with phosphoric acid; B: acetonitrile; A:B=97:3(V / V)

[0035] (3) Experimental reagents:

[0036] Acetonitrile: Beijing Bailingwei Technology Co., Ltd., HPLC grade;

[0037] Triethylamine: Tianjin Fuchen Chemical Reagent, analytically pure

[0038] Phosphoric acid: Tianjin Damao Chemical Reagent, analytically pure

[0039] Implementation steps:

[0040] 1. Determination of detection wavelength: Take violin acid and various impurities, add mobile phase to dissolve and dilute to a solution of about 20ug / ml, ...

Embodiment 2

[0047] Experimental Equipment and Reagents

[0048] (1) Experimental equipment:

[0049] Instrument: Shimadzu 20A with UV detector

[0050] (2) Chromatographic conditions:

[0051] Chromatographic column: ZORBAX SB-Phenyl C18 column, 4.6×250mm, 5μm;

[0052] Flow rate: 0.9ml / min;

[0053] Detection wavelength: 205nm;

[0054] Column temperature: 30°C;

[0055] Injection volume: 20μl

[0056] Mobile phase: A: 0.2% (V / V) triethylamine aqueous solution, adjust pH=3.0 with phosphoric acid; B: acetonitrile; A:B=97:3(V / V)

[0057] (3) Experimental reagents:

[0058] Acetonitrile: Beijing Bailingwei Technology Co., Ltd., HPLC grade;

[0059] Triethylamine: Tianjin Fuchen Chemical Reagent, analytically pure

[0060] Phosphoric acid: Tianjin Damao Chemical Reagent, analytically pure

[0061] Implementation steps:

[0062] Mix violuric acid and impurities in an appropriate amount, add mobile phase to dissolve, shake well, and use it as a resolution test solution (system suita...

Embodiment 3

[0064] Experimental Equipment and Reagents

[0065] (1) Experimental equipment:

[0066] Instrument: Shimadzu 20A with UV detector

[0067] (2) Chromatographic conditions:

[0068] Chromatographic column: ZORBAX SB-Phenyl C18 column, 4.6×250mm, 5μm;

[0069] Flow rate: 1.1ml / min;

[0070] Detection wavelength: 205nm;

[0071] Column temperature: 30°C;

[0072]Injection volume: 20μl

[0073] Mobile phase: A: 0.2% (V / V) triethylamine aqueous solution, adjust pH=3.0 with phosphoric acid; B: acetonitrile; A:B=97:3(V / V)

[0074] (3) Experimental reagents:

[0075] Acetonitrile: Beijing Bailingwei Technology Co., Ltd., HPLC grade;

[0076] Triethylamine: Tianjin Fuchen Chemical Reagent, analytically pure

[0077] Phosphoric acid: Tianjin Damao Chemical Reagent, analytically pure

[0078] Implementation steps:

[0079] Mix violuric acid and impurities in an appropriate amount, add mobile phase to dissolve, shake well, and use it as a resolution test solution (system suitab...

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Abstract

The invention provides a method for determining contents of hydroxyiminobarbituric acid and related impurities of cyanoacetic acid, dimethylurea, dimethylacetamide and dimethyl 4AU(dihydrogen-6-imino-1,3-dimethylurea pyrimidine). A reverse high performance liquid chromatography peak area normalizing type quantitative analysis method is utilized, and adopts the chromatography conditions that a chromatography column is Phenyl C19 column; the length of the column is 150 to 250mm, the inner diameter of the column is 4.0 to 4.6mm, and the particle size of filler is 3.5 to 5mu m; the flow rate is 0.9 to 1.1ml / min; the detection wavelength is 205nm; the temperature of the column is 27 to 33 DEG C; the sample feeding amount is 20mul; the flowing phase comprises a 0.2% (V / V) triethylamine water solution A and acetonitrile B, the pH (potential of hydrogen) value of the 0.2% (V / V) triethylamine water solution A is adjusted to 2.8 to 3.2 by phosphoric acid, and the ratio of A to B is (96 to 98):(2to 4)(V / V). The method has the advantages that the product quality is conveniently controlled in the production and quality control process; the cost is low, the operation is simple, the implementingis easy, the accuracy and precision are high, and the stability and reproducibility are good.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and in particular relates to a high-performance liquid chromatography analysis and detection method for violuric acid-related substances. Background technique [0002] Violuric acid (VIOLURIC ACID), its chemical name is 1,3-dimethyl-4-imino-5-isonitrosourazine, molecular formula: C 4 h 3 N 3 o 4 , molecular weight: 157.08. [0003] Its structural formula is: [0004] Violuric acid is an important intermediate in the caffeine preparation process and a key link in the quality control of caffeine. Accurate detection of violuric acid can provide quality assurance for subsequent reactions. Combined with the violuric acid process route, the possible process impurities, degradation products and other impurities were comprehensively analyzed. As a reaction intermediate, cyanoacetic acid is considered to have residues in the quality control of intermediates in combination with the analysis ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 丰宇胜郑忠辉徐豪杰张富强王志萍
Owner XINHUA PHARM (SHOUGUANG) CO LTD
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