Cloprostenol sodium pure product preparation method

A technology of sodium cloprostenol, pure product, applied in the field of preparation of pure product of sodium cloprostinol, can solve the problems of long time, low purity, small sample loading, etc., and achieve low cost, high product purity, and sample loading A large amount of effect

Inactive Publication Date: 2015-02-25
JIANGSU HANBON SCI & TECH CO
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for large-scale separation and preparation of cloprostenol sodium. Its technical idea is to utilize industrial preparation grade liquid chromatography separation and purification system to separate and prepare cloprostenol sodium on a large scale, so as to solve the current problem of purifying cloprostenol sodium Existing time in the process is long, the technical problem such as loading sample amount is little and purity is not high, simple operation, high product content, good reproducibility, can obtain cloprostenol sodium pure product rapidly in a short period of time, this method comprises the following steps :

Method used

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  • Cloprostenol sodium pure product preparation method

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Experimental program
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Effect test

Embodiment 1

[0018] 1. Weigh 1.25g of the synthesized sodium chloroprostol powder, dissolve it in 25ml of pure ethanol, treat it with ultrasound, and filter it through a 0.45μm filter membrane to obtain a sample solution;

[0019] 2. Equilibrate the two column volumes with a 92:8 mobile phase of n-hexane / ethanol (containing 0.1% acetic acid). Take the sample solution from step 1 and inject it into the industrial preparative liquid chromatography separation and purification system with a syringe. The column is eluted at equal degrees, the column packing size is Φ50×250mm, the packing is spherical silica gel, the particle size is 10um, the sample volume is 1.25g, the flow rate is 60ml / min, the detection wavelength of the UV-visible light detector is 220nm, and the collection retention time is 71~ For the 89min target fraction, continue to flush 1~2 column volumes with mobile phase solution to make all impurities flow out;

[0020] 3. Concentrate the collected fractions in a vacuum rotary evaporat...

Embodiment 2

[0022] 1. Weigh 20g of synthetic chloroprostol sodium powder, dissolve it in 25ml of pure ethanol, treat it with ultrasound, and filter it through a 0.45μm filter membrane to obtain a sample solution;

[0023] 2. Equilibrate the two column volumes with a 90:10 mobile phase of n-hexane / ethanol (containing 0.1% acetic acid), take the sample solution from step 1, and inject it into the industrial preparative liquid chromatography separation and purification system with a sample pump. Equivalent elution, the column packing size is Φ200×250mm, the packing is spherical silica gel, the particle size is 20um, the sample volume is 20g, the flow rate is 900ml / min, the detection wavelength of the UV-visible light detector is 220nm, and the collection retention time is 68~95min Continue to flush 1~2 column volumes with mobile phase solution to make all impurities flow out;

[0024] 3. The collected fractions were concentrated under reduced pressure in a vacuum rotary evaporator at 40°C to obta...

Embodiment 3

[0026] 1. Weigh 125g of synthetic chloroprostol sodium powder, dissolve it in 2.5Lml of pure ethanol, treat it with ultrasound, and filter through a 0.45μm filter membrane to obtain a sample solution;

[0027] 2. Equilibrate the two column volumes of the column with a 95:5 mobile phase of n-hexane / ethanol (containing 0.1% acetic acid), take the sample solution from step 1, and inject it into the industrial preparative liquid chromatography separation and purification system with a sample pump. Equivalent elution, the column packing size is Φ500×250mm, the packing is spherical silica gel, the particle size is 20um, the sample volume is 125g, the flow rate is 4L / min, the detection wavelength of the UV-visible light detector is 220nm, and the collection retention time is 75~110min Continue to flush 1~2 column volumes with mobile phase solution to make all impurities flow out;

[0028] 3. The collected fractions were concentrated under reduced pressure on a vacuum rotary evaporator at ...

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Abstract

The invention discloses a cloprostenol sodium pure product preparation method for preparation of cloprostenol sodium by an industrial preparative liquid chromatography separation purification system, and belongs to the technical field of separation and purification of biological products, the method is simple and high in yield, the prepared cloprostenol sodium is high in product purity, and the method is applicable to industrial mass production preparation of the cloprostenol sodium.

Description

Technical field [0001] The present invention is a method for preparing pure sodium chloroprostol, and particularly relates to a preparation technology of an industrial preparative liquid chromatography separation and purification system for pure sodium chloroprostol. Background technique [0002] Sodium cloprostol is an analog of PGF2α, and it has the highest activity among the commonly used PGF2α and its analogs. It is a synthetic hormone medicine, mainly used to control the estrus of cows at the same time and induce delivery by pregnant sows. Its pharmacological effect is to dissolve the corpus luteum and reduce the concentration of progesterone in the blood. In 2005, it was listed in the latest veterinary drugs approved by the Ministry of Agriculture. In recent years, it has been widely used in breeding techniques such as embryo transfer of livestock, especially for the long-lasting luteal infertility of female animals and is often used clinically. [0003] However, the purity...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C405/00
Inventor 张宇王缄张大兵
Owner JIANGSU HANBON SCI & TECH CO
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