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High purity 4-hydroxyciclosporin and purification and preparation method thereof

A hydroxycyclosporine, high-purity technology, applied in the field of biopharmaceuticals, can solve the problem of high removal difficulty, and achieve the effects of shortening the process cycle, reducing the difficulty, and being difficult to recover and reuse.

Inactive Publication Date: 2016-06-08
SHIJIAZHUANG ZHONGTIAN BIOTECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The main impurities in the 4-OH cyclosporine fermentation products are unconverted cyclosporine and its homologues, which are difficult to remove. After searching, there is no way to remove these impurities to obtain high-purity 4-OH cyclosporine related literature

Method used

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  • High purity 4-hydroxyciclosporin and purification and preparation method thereof
  • High purity 4-hydroxyciclosporin and purification and preparation method thereof
  • High purity 4-hydroxyciclosporin and purification and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] 1) Take 30L of 4-OH cyclosporin fermentation broth, containing 10.2g of 4-OH cyclosporine, add 30L of isopropanol to soak for 5 hours, filter with plate and frame, collect 58L of extract, and the titer is 173 μg / ml.

[0059] 2) Use 1LD290 resin as the decolorization medium to decolorize the collected extraction solution at a flow rate of 2BV / h, and collect the decolorization solution, which is obviously shallower than before the column.

[0060] 3) Use a 1LHZ816 column to adsorb the collected decolorized solution, and the sample loading flow rate is 1BV / h. After the adsorption is completed, the titer of the column solution is detected to be 1 μg / ml, and discarded. The adsorbed resin is washed in one step, the detergent is 45% methanol, the flow rate is 1-1.5BV / h, and the washing column liquid has no unit after testing. Then analyze with 80% isopropanol at a flow rate of 1 BV / h, and collect the analysis solution in sections. When the outlet unit of the analysis solution...

Embodiment 2

[0064] 1) Take 25L of 4-OH cyclosporin fermentation broth, containing 8.2g of 4-OH cyclosporine, add 20L of ethanol to soak for 5 hours, filter with plate and frame, collect 41L of extract, and the titer is 189 μg / ml.

[0065] 2) Use 1LRX-01T resin as the decolorization medium to decolorize the collected extraction solution at a flow rate of 2BV / h, and collect the decolorization solution. The decolorization solution is obviously shallower than that before the column.

[0066] 3) Use a 1LHZ816 column to adsorb the collected decolorized solution, and the sample loading flow rate is 1BV / h. After the adsorption is completed, the titer of the column solution is detected to be 1 μg / ml, and discarded. The adsorbed resin is washed in two steps. The detergent 1 is 45% methanol-alkali (1g / LNaOH), and the detergent 2 is 45% methanol. The flow rate is 1-1.5BV / h. . Then analyze with 82% ethanol at a flow rate of 1 BV / h, and collect the analysis solution in sections. When the analysis exp...

Embodiment 3

[0070] 1) Take 28L of 4-OH cyclosporin fermentation broth, containing 9.8g of 4-OH cyclosporine, add 25L of methanol to soak for 5 hours, filter with plate and frame, collect 50L of extract, and the potency is 185 μg / ml.

[0071] 2) Use 1LRX-02T resin as the decolorization medium to decolorize the collected extraction solution at a flow rate of 2BV / h, and collect the decolorization solution, which is obviously shallower than before the column.

[0072] 3) Use a 1LHZ816 column to adsorb the collected decolorized solution, and the sample loading flow rate is 1BV / h. After the adsorption is completed, the titer of the column solution is detected to be 3 μg / ml, and discarded. The adsorbed resin is washed in two steps. The detergent 1 is 45% methanol-alkali (1g / LNaOH), and the detergent 2 is 45% methanol. . Then analyze with 80%-85% methanol, the flow rate is 1BV / h, and collect the analysis solution in sections. When the analysis export unit is less than 10 μg / ml, the analysis is ...

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Abstract

The invention discloses high purity 4-hydroxyciclosporin and a purification and preparation method thereof. The purification and preparation method comprises the following steps: extracting 4-hydroxyciclosporin, discoloring 4-hydroxyciclosporin extract by a discoloring medium, enriching by an adsorbing medium; carrying out high pressure chromatography preparation; and performing crystallization and purification. According to the purification and preparation method, an ion exchange resin discoloring technology, a macroporous adsorption resin enriching technology, and a high pressure chromatography purification technology are adopted; in each phase, a specific technology is chosen, technologies cooperate with each other, and a good technology effect is achieved.

Description

technical field [0001] The invention relates to the field of biopharmaceuticals, in particular to a method for extracting and preparing high-purity 4-hydroxycyclosporine from a 4-hydroxycyclosporin fermentation broth prepared by a biotransformation method. Background technique [0002] 4-Hydroxycyclosporine (abbreviated as 4-OH cyclosporine) is an important pharmaceutical intermediate of new anti-hepatitis C virus drugs, mainly for hepatitis C virus, referred to as hepatitis C, hepatitis C, is a hepatitis C Viral hepatitis caused by virus (HepatitisCvirus, HCV) infection. According to the statistics of the World Health Organization, the current global HCV infection rate is about 3%, it is estimated that about 180 million people are infected with HCV, and about 35,000 new cases of hepatitis C occur each year. Hepatitis C is a global epidemic, which can lead to chronic inflammation, necrosis and fibrosis of the liver, and some patients can develop liver cirrhosis and even cel...

Claims

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Application Information

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IPC IPC(8): C07K7/64C07K1/16
Inventor 魏增辉胡帅珂刘莹王乔波董国豪康志飞刘建明张志军
Owner SHIJIAZHUANG ZHONGTIAN BIOTECH
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