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Content detection method of gamithromycin

A detection method and technology of gamiycin, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of low precision and poor separation effect, and achieve a large detection range, stable baseline, and good separation effect. Effect

Active Publication Date: 2015-04-22
TIANJIN ZHONGSHENG TIAOZHAN BIOTECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims at the technical defects of the prior art, and provides a method for detecting the content of gamithromycin, so as to solve the problem of low sensitivity and precision in the prior art when using high performance liquid chromatography to quantitatively detect gamithromycin and technical problems with poor separation

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  • Content detection method of gamithromycin
  • Content detection method of gamithromycin
  • Content detection method of gamithromycin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Chromatographic conditions

[0025] The octadecylsilane-bonded silica gel column was used as the chromatographic column, and an Agilent C18 column (4.6*150mm, 5μm) was used, and the mobile phase was 0.1mol / L ammonium acetate solution (pH 8.0)-acetonitrile (30:70, V / V), the flow rate was 0.8 ml / min, the column temperature was 35°C, the drift tube temperature of the evaporative light scattering detector was 60°C, and the gas flow rate was 20 psi. The autosampler injection volume was 20 μL.

[0026] (2) Drawing of standard curve

[0027] Precisely weigh 50mg of the reference substance, put it in a 50ml brown volumetric flask, dissolve it in chromatographic acetonitrile, and make up to the mark as a stock solution of the standard solution of gamitomycin. 20, 50, 100, 200, and 500 μg / ml of standard solutions were injected into 20 μl of the chromatographic column of the HPLC device set in step (1) and entered the working state, respectively, and the peak areas at the s...

Embodiment 2

[0041] (1) Implementation of testing

[0042] A method for detecting gamycin content, the method is high performance liquid chromatography, utilizes a C18 chromatographic column, and has the following chromatographic conditions: the mobile phase is composed of 0.1mol / L ammonium acetate solution and acetonitrile, wherein the acetonitrile accounts for the total amount of the mobile phase. 70% of the volume (v / v); the flow rate was 0.8 mL / min; the column temperature was 40°C.

[0043] On the basis of the above technical solutions:

[0044] The specifications of the C18 column are: length 150 mm, inner diameter 4.6 mm, and filler particle size 5 μm.

[0045] The method utilizes an evaporative light scattering detector for detection and has the following operating conditions: the temperature of the drift tube is 60° C., the gas flow rate is 20 psi, and the injection volume is 20 μL.

[0046] (2) Standard curve drawing

[0047]Precisely weigh an appropriate amount of the referenc...

Embodiment 3

[0054] A method for detecting the content of gamycin, the method is high performance liquid chromatography, utilizes a C18 chromatographic column, and has the following chromatographic conditions: the mobile phase is composed of 0.1mol / L ammonium acetate solution and acetonitrile, wherein the acetonitrile accounts for the total amount of the mobile phase. 60% (v / v) of the volume; the flow rate was 1 mL / min; the column temperature was 20°C.

[0055] On the basis of the above technical solutions:

[0056] The specifications of the C18 column are: length 250 mm, inner diameter 4.6 mm, and filler particle size 5 μm.

[0057] The method utilizes an evaporative light scattering detector for detection.

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Abstract

The invention provides a content detection method of gamithromycin. According to the technical scheme, the content of gamithromycin is detected by virtue of a HPLC method; an evaporative light-scattering detector is utilized, is high in sensitivity and is not sensitive to temperature variation, and a base line is relatively stable; the response of the evaporative light-scattering detector does not depend on the optical property of a sample, is not influenced by functional groups, is not interfered by a mobile phase and is in direct proportion to the quality of the sample, and specific chemical structures of detected main components are not required; the gamithromycin is relatively low in absorption wavelength and is absorbed at a tail end of an ultraviolet ray; therefore, compared with an ultraviolet detector, the evaporative light-scattering detector has great superiority in the detection of gamithromycin. Besides, selected chromatographic columns and chromatographic conditions are designed tightly around the characteristic of the evaporative light-scattering detector, a relatively good separation effect is integrally realized; after the method is verified by virtue of methods such as an accuracy experiment, a linear relation experiment and a sampling recycling experiment, results show that the accuracy is high, the detection range is wide, and the sensitivity is relatively good.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a method for detecting the content of gamycin. Background technique [0002] Gamithromycin, English name: Gamithromycin, CAS number is 145435-72-9, molecular formula is C 40 H 76 N 2 O 12 , molecular weight 777.04, white to beige crystals, soluble in methanol, acetonitrile, acetone and other organic solvents, insoluble in water. [0003] Gamycin is a semisynthetic macrolide veterinary antibiotic with only one stable configuration. Gamitomycin has bacteriostatic and bactericidal activities by inhibiting the synthesis of bacterial proteins. It is mainly used for the treatment of bovine infectious diseases caused by bacterial pathogens such as Pasteurella hemolytica, Pasteurella hemorrhagicus, and Histophilus . Gamiycin can be used in edible animals, and has the advantages of fast absorption, wide distribution in the body, low residual in the body, and high safety. No ad...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/60G01N30/74
Inventor 张立会姜淋洁王建程雪娇王勇余贵菊甄盼盼杨雪
Owner TIANJIN ZHONGSHENG TIAOZHAN BIOTECH
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