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High-pressure liquid-phase preparation method for enramycin standard sample

A technology of enramycin and high-pressure liquid phase, which is applied in the field of high-pressure liquid phase preparation of enramycin standard products, can solve the problems that the preparation method of enramycin has not been found yet, and achieve simple and fast pretreatment and simple collection method , easy-to-operate effects

Active Publication Date: 2012-09-19
江西兴鼎科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, no report related to the preparation method of enramycin standard substance has been found

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1: After cleaning the fermented bacteria with deionized water, suspend in the ratio of 65ml / g in the extract mixed with acetone:hydrochloric acid solution:water=20:1:21, acetone is analytically pure concentration, hydrochloric acid The concentration of the solution is 2 mol / L, and the cells are broken with an ultrasonic breaker or an ultrasonic machine for 10 minutes, and the obtained mixture is shaken and extracted at 20°C and 180 rpm for 90 minutes to obtain an extract containing enramycin, and then heated at 10000r / m Centrifuge at a speed of 10 min for 10 min, collect the supernatant, and filter it with a 0.45 μm filter membrane as a sample solution for later use.

[0023] Inject the processed sample according to the following chromatographic conditions:

[0024] Injection volume: 100μl;

[0025] Chromatographic column: Phenomenex C18 column semi-preparative type, length 250mm, inner diameter 10mm, particle size 5μm;

[0026] Mobile phase: B: chromatographi...

Embodiment 2

[0032] Embodiment 2: select animal feed sample 400g according to the regulations of GB / T 14699.1, shrink to 100g with the quartering method, pulverize and pass through a 0.45mm aperture sieve, mix, and store in a grinding bottle for subsequent use, get the above-mentioned animal feed sample 5- Add 10g to 80ml of the extract solution mixed with acetone: hydrochloric acid solution: water = 20:1:21, the concentration of acetone is analytically pure, the concentration of hydrochloric acid solution is 2mol / L, shake at 20°C and 180rpm Extract for 90 minutes to obtain an extract containing enramycin, then centrifuge at a speed of 10,000r / min for 10 minutes, collect the supernatant, and filter it with a 0.45μm filter membrane as a sample solution for later use. The concentration of the sample solution should not exceed 2000μg / min. ml.

[0033] Inject the processed sample according to the following chromatographic conditions:

[0034] Injection volume: 100μl;

[0035] Chromatographic...

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Abstract

The invention discloses a high-pressure liquid-phase preparation method for an enramycin standard sample, and the method comprises preparation of a fermented thallus test sample solution and preparation of a animal feed test sample solution, wherein the preparation of the fermented thallus test sample solution comprises the following steps of: suspending fermented thallus in an extraction solution, which is formed by mixing acetone, hydrochloric acid solution and water in a ratio of 20:1:21, in a ratio of 30-90 ml / g, disrupting cells by an ultrasonic disruptor or an ultrasonic machine to obtain an extraction solution containing enramycin, collecting a supernatant, filtering the supernatant by a filter membrane, and using the supernatant as the test sample solution for the future use; and the preparation of the animal feed test sample solution comprises the following steps of: performing reverse-phase high-performance liquid chromatography in corresponding conditions, collecting according to the retention time of the constituents, and then removing a solvent according to a conventional rotary evaporation process, thus obtaining the standard sample of the enramycin constituent. The high-pressure liquid-phase preparation method of the enramycin standard sample disclosed by the invention has the following advantages: 1, the pre-treatment is simple, fast, and easy to operate; 2, the collection method is simple; and 3, the purity of the prepared standard sample is high and up to more than 90%.

Description

technical field [0001] The invention relates to a high-pressure liquid-phase preparation method of enramycin standard substance. Background technique [0002] Enramycin is a polypeptide antibiotic composed of 13 different kinds of 17 amino acid molecules and fatty acid molecules, wherein the amino acid molecules form a cyclic polypeptide structure, and the fatty acid is located at the end of the polypeptide structure. According to the different types of terminal fatty acids, it can be divided into Entrapsis A (C 107 h 138 C l2 N 26 o 31 ) and enramycin B (C 108 h 140 C l2 N 26 o 31 ), and enramycin is a mixture of these two components. Enramycin hydrochloride is a white crystalline powder with a molecular weight of about 2500 and a melting point of 238-245°C. It is easily soluble in dimethyl sulfoxide, soluble in methanol and aqueous ethanol, hardly soluble in acetone, and insoluble in benzene. , Chloroform. Enramycin hydrochloride has excellent stability to heat...

Claims

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Application Information

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IPC IPC(8): C07K7/08C07K1/16G01N33/68
Inventor 崔厚华冷董碧殷晓浦黄苓刘雅晶
Owner 江西兴鼎科技有限公司
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