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A method for analyzing Zhongshengmycin content

An analysis method, the technology of bacteriocin, applied in the field of analysis and testing, can solve the problems of interference in the determination of active ingredients, cumbersome steps, and inability to effectively separate impurities.

Active Publication Date: 2016-04-06
SHENZHEN NOPOSION AGROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] As a type of biological pesticide, Zhongshengmycin also faces the problems of other pesticides: whether the content of the active ingredients of the pesticide is up to the standard; how to use the pesticide rationally; its drug residues may cause serious harm to human health
Because the biopotency method cannot separate some effective impurities, it cannot objectively reflect the content of active ingredients, and it is time-consuming, and its reproducibility and accuracy are far inferior to those of instrumental analysis.
Fluorescence detection after pre-column derivatization requires pre-column derivatization, cumbersome steps, and high solvent toxicity; in addition, since Zhongshengmycin original drug and its preparations contain other substances besides Zhongshengmycin, the derivatized Analytical method Derivative reagents and impurities will cause serious interference to the determination of active ingredients, and the content of Zhongshengmycin cannot be accurately determined

Method used

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  • A method for analyzing Zhongshengmycin content
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  • A method for analyzing Zhongshengmycin content

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 1. Chromatographic conditions

[0039]Octadecylsilane-bonded silica gel is used as filler, the particle size is 5 microns, the chromatographic column length is 250 mm, the inner diameter is 4.6 mm stainless steel column, the temperature of the column chamber is room temperature, the number of theoretical plates is 4000, and 0.02% heptanesulfonic acid is used The ion-pair aqueous solution composed of sodium and 0.10% volume fraction of phosphoric acid: the mixed solution of acetonitrile volume ratio = 81:19 is the mobile phase, the flow rate is 1.0mL / min, the detection wavelength is 210nm, and the injection volume is 10 microliters.

[0040] 2. Standard sample preparation

[0041] Accurately weigh 0.0532 grams of Zhongshengmycin standard sample (provided by the National Pesticide Testing Center, the content is 100%) in a 100mL volumetric flask, dissolve in water to volume, shake well (this standard solution is A solution), and then pipette Accurately draw 5.00mL of the ...

Embodiment 2

[0049] 1. Chromatographic conditions

[0050] Use octadecylsilane bonded silica gel as filler, particle size 4 microns, chromatographic column length 200 mm, stainless steel column inner diameter 4.6 mm, column chamber temperature is room temperature, theoretical plate number 5000, using 0.02% heptanesulfonic acid The ion-pair aqueous solution composed of sodium and 0.10% volume fraction of phosphoric acid: the mixed solution of acetonitrile volume ratio = 83:17 is the mobile phase, the flow rate is 1.0mL / min, the detection wavelength is 200nm, and the injection volume is 10 microliters.

[0051] 2. Sample preparation

[0052] Accurately measure 10, 5, 2.5, 0.5, 0.25, 0.125, and 0 mL of the standard solution A in the above-mentioned Example 1, place them in seven 25 mL volumetric flasks, dilute with water to the mark, and shake well for testing.

[0053] 3. Testing and data processing

[0054] Measure at 200nm according to the law, draw a standard curve with the sample mass ...

Embodiment 3

[0058] 1. Chromatographic conditions

[0059] Octadecylsilane-bonded silica gel is used as filler, the particle size is 3 microns, the chromatographic column length is 150 mm, the inner diameter is 4.6 mm stainless steel column, the temperature of the column chamber is room temperature, the number of theoretical plates is 3500, and 0.02% heptanesulfonic acid is used The ion-pair aqueous solution composed of sodium and 0.10% volume fraction of phosphoric acid: the mixed solution of acetonitrile volume ratio = 87:13 is the mobile phase, the flow rate is 1.0mL / min, the detection wavelength is 205nm, and the injection volume is 10 microliters.

[0060] 2. Sample preparation

[0061] Accurately weigh 0.5189g of 10% Zhongshengmycin original powder and place it in a 100mL volumetric flask, add water to make it up to the mark, dissolve it by ultrasonic oscillation, cool to room temperature, and then use a pipette to accurately draw 5.00mL of the solution into a 50mL volumetric flask ...

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Abstract

The invention relates to an analysis method of Zhongshengmycin content. A liquid chromatogram ultraviolet detection method is adopted for determination, pure water is taken as a solvent, a reversed phase C18 chromatographic column is used, a mixed system of an ion pair water solution and pure acetonitrile is taken as mobile phases, and the ion pair water solution mainly comprises sodium heptanesulfonate with the mass fraction of 0.01%-0.05% and acid buffer solution with the pH of 1.7-3.0. In the analysis method of the Zhongshengmycin content, the ion pair water solution and the pure acetonitrile are taken as the mobile phases, and the reversed phase C18 chromatographic column is adopted, so that an excellent peak shape can be obtained; the chromatographic column is relatively convenient to regenerate, so that the service life of the chromatographic column is prolonged, most of the used mobile phases is water, and thus the detection cost is reduced; the analysis method is suitable for real-time monitoring on the Zhongshengmycin content, and the obtained results are relatively accurate.

Description

technical field [0001] The invention relates to the technical field of analysis and testing, in particular to an analysis method for Zhongshengmycin content. Background technique [0002] Zhongshengmycin is a new type of agricultural antibiotic successfully developed by my country independently. It is produced by fermentation of Streptomyces lilacaceae Hainan variety B-7. L-lysine-2 deoxygulusamine, the molecule is composed of three parts, gulosamine, streptolidin and β-lysine. The structural formula is as follows: [0003] [0004] In the formula: the main active ingredients are n=1,2,3, and the minor ingredients are n=4,5. [0005] Zhongshengmycin is a protective fungicide with a wide bactericidal spectrum, which can resist Gram-positive and negative bacteria, mycobacteria, yeast and filamentous fungi; it has contact and penetration effects. Because of its broad-spectrum and high-efficiency bactericidal function, it has considerable development prospects and great mar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/60
Inventor 成妙金李欧燕孔建王芳戴兰芳文琴
Owner SHENZHEN NOPOSION AGROCHEM