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A thin-layer chromatography detection method for amino acid impurities in l-2-amino-5-guanidinovaleric acid raw materials

A technique of arginine and thin-layer chromatography, applied in the field of food and drug analysis, can solve the problems of low sensitivity and poor separation effect, and achieve the effect of solving the problem of detection sensitivity

Active Publication Date: 2020-11-24
FUJIAN GUTIAN PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a thin-layer chromatographic analysis and detection method for other amino acid impurities in the L-2-amino-5-guanidinopentanoic acid raw material, to solve the problem of L-2-amino-5-guanidinopentane in the existing TLC method. The problem of poor separation effect and low sensitivity of acid and other amino acid impurities, through the establishment and implementation of this detection method, provides a basis for the formulation of quality standards for L-2-amino-5-guanidinovaleric acid raw materials, so as to better control the product Quality, ensuring food and medicinal safety

Method used

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  • A thin-layer chromatography detection method for amino acid impurities in l-2-amino-5-guanidinovaleric acid raw materials
  • A thin-layer chromatography detection method for amino acid impurities in l-2-amino-5-guanidinovaleric acid raw materials
  • A thin-layer chromatography detection method for amino acid impurities in l-2-amino-5-guanidinovaleric acid raw materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Example 1: L-2- amino-5-guanidino-pentanoic acid detection sensitivity of the detection

[0063] 1, the sample solution preparation: Weigh L-2- amino-5-guanidino valeric acid was dissolved 0.1g in 10mL water, diluted with 1mL of the solution was taken with water to 50mL stand. The solution 0.5,1.0,1.5,2.0 and 2.5 mL were collected, placed in a 10mL volumetric flask, add water to the mark, respectively, formulated as 0.1%, 0.2%, 0.3%, 0.4% and 0.5% of L-2- amino - 5-guanidino-pentanoic acid solution.

[0064]2, thin layer chromatography: neutral were prepared of a hard glass tube from step 1 different concentrations of L-2- amino-5-guanidino-pentanoic acid 5 L of solution, spotted on the same TLC plate of silica gel G; then, spotted TLC plate was placed in a chromatography tank, added isopropanol - concentrated ammonia solution developing solvent: rear (73), expand about 10cm at room temperature for 26 ℃ environment of 74% relative humidity and drying out; then the TLC plate...

Embodiment 2

[0066] Example 2: Location-amino-5-guanidino-pentanoic acid homologs impurity L-2-

[0067] 1, was prepared:

[0068] (1) homolog solution: Weigh L-2- amino-succinic acid, L-2,5- diamino pentanoic acid, ( S ) -2-amino-5-ureido pentanoic acid, ( S ) -2-acetylamino-5-amino-valeric acid, ( S ) -2-acetylamino-oxoglutarate 2mg each placed in a different flask, dissolved in water and dilute to 10mL ,, homologs obtained solution concentration were 0.2mg / mL of solution were referred to as A2, the solution B2, a solution of C2, the solution D2, solution E2.

[0069] (2) The system suitability solution: Weigh accurately L-2- amino-5-guanidino valeric acid, and two L-2,6- reference aminocaproic acid, diluted with water and made, respectively, each containing about l mL L- amino-5-guanidino-pentanoic acid solution, and 20 mg L-2,6- diamino-hexanoic acid 0.4mg, denoted solution F2.

[0070] 2, thin layer chromatography: neutral, respectively, of a hard glass tube of each step taking 5μL homo...

Embodiment 3

[0072] Example 3: homologs L-2- amino-succinic acid formulation and a method for determining the concentration of

[0073] 1, was prepared:

[0074] (1) L-2- amino-water formulation succinic acid solution: Weigh accurately L-2- amino-succinic acid 10mg, is dissolved with dilute phosphoric acid was added after the water volume to 10mL, as a solution; respectively weighed 1mL, 0.8mL , 0.6mL, 0.4mL, 0.2mL solution 1, was placed in different volumetric flask, dilute to volume with water to 10mL, obtained at a concentration of 0.10mg / mL, 0.08mg / mL, 0.06mg / mL, 0.04mg / mL, 0.02 mg / mL of L-2- amino-succinic acid solution, a solution denoted as A3, solution B3, solution C3, the solution D3, a solution of E3.

[0075] (2) Preparation of L-2- amino-succinic acid solution was diluted with: sodium hydroxide solution to adjust the pH to 10.0 to 12.0 for aqueous dilution. Accurately weighed L-2- amino-succinic acid 10mg, is dissolved with the diluent and set the volume to 10mL, as a sol...

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Abstract

The invention relates to a thin-layer chromatography detection method for amino acid impurities in L-2-amino-5-guanidinolic acid raw materials, comprising solution preparation, thin layer chromatography detection, and result determination. The thin layer chromatography detection comprises the thin layer chromatography detection of amino acid impurities. A silica gel G thin layer plate is used in the thin layer chromatography detection. A developing agent is a mixed solution of propanol and concentrated ammonia solution. The developing environment is at a temperature of 26 to 40 DEG C, and therelative humidity is 75% to 90%. The invention has the advantages of good separation, high sensitivity, short detection time, low detection cost, simple operation, simple equipment, easy color development, and intuitive and reliable result, which is suitable for industrial detection and quality control of other amino acid impurities in L-2-amino-5-mercaptopuric acid raw materials and provides a basis for the establishment of quality standards in order to better control and master the quality of products, and ensure the safety of clinical medication.

Description

Technical field [0001] The present invention belongs to the technical field of food and pharmaceutical analysis, particularly relates to a method of thin layer chromatography L-2- amino-5-guanidino-pentanoic acid impurities in the feed. Background technique [0002] L-2- amino-5-guanidino-pentanoic acid (CAS No. 74-79-3 login) belonging to the amino compounds, having important physiological functions, often as a nutritional supplement, is an important component of amino acid infusion and capsules. L-2- amino-5-guanidino-pentanoic acid can effectively enhance immunity, the immune system to promote the secretion of endogenous substances, and is conducive to prevention of viral infections against cancer cells; beneficial severe trauma, burns and other tissue repair requires a lot of patients the health care provider. Clinically, L-2- amino-5-guanidino valeric acid suitable for ammonia increased hepatic coma, especially in patients with alkalosis; for assisting determination of pitui...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/90
CPCG01N30/90
Inventor 陈程俊李绪全刘红方佳茂陈伟滨林晓群张松浩陈榕兴
Owner FUJIAN GUTIAN PHARMA
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