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Purification method of melanotan II

A technology of Melanotan and purification method, which is applied in the field of HPLC, can solve problems such as inability to meet production requirements, and achieve the effects of low production cost, high yield, and protection of chromatographic columns

Inactive Publication Date: 2015-11-11
南京肽业生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the published literature and patents, the purification process of Melanotan II is rarely involved. Due to the limitation of the synthesis process, new requirements have been put forward for the purification, and a single method has been unable to meet the production requirements.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1. Sample treatment: add a certain amount of acetic acid to the crude Melanotan II solution and stir it ultrasonically, filter it with a filter membrane with a pore size of 0.45 μm, and collect the filtrate for later use.

[0020] 2. Primary purification

[0021] Purification conditions: Chromatographic column: a polymer-based packed chromatographic column with a pore size of 10 μm, a column diameter and length of 5 cm×25 cm. Mobile phase: Phase A: 0.1% trifluoroacetic acid aqueous solution by volume; Phase B: Volume percentage concentration 0.1% trifluoroacetic acid acetonitrile solution. Flow rate: 80ml / min. Detection wavelength: 220nm. Gradient: B%: 20-60%, 60min. The injection volume is 5g.

[0022] Purification process: wash the chromatographic column with acetonitrile solution of 90% trifluoroacetic acid by volume, then equilibrate and load the sample, the sample volume is 5g. Gradient elution was performed for 60 minutes, and fractions with a purity greater ...

Embodiment 2

[0029] 1. Sample treatment: add a certain amount of acetic acid to the crude Melanotan II solution and stir it ultrasonically, filter it with a filter membrane with a pore size of 0.45 μm, and collect the filtrate for later use.

[0030] 2. Primary purification

[0031] Purification conditions: Chromatographic column: a polymer-based packed chromatographic column with a pore size of 20 μm, a column diameter and length of 5cm×25cm. Mobile phase: Phase A: 0.05% trifluoroacetic acid aqueous solution by volume; Phase B: Volume percentage concentration 0.05% trifluoroacetic acid acetonitrile solution. Flow rate: 80ml / min. Detection wavelength: 220nm. Gradient: B%: 20-60%, 60min. The injection volume was 6.5 g.

[0032] Purification process: wash the chromatographic column with acetonitrile solution of 90% trifluoroacetic acid by volume, then equilibrate and load the sample, the sample volume is 6.5g. Gradient elution was performed for 60 minutes, and fractions with a purity gr...

Embodiment 3

[0039] 1. Sample treatment: add a certain amount of acetic acid to the crude Melanotan II solution and stir it ultrasonically, filter it with a filter membrane with a pore size of 0.45 μm, and collect the filtrate for later use.

[0040] 2. Primary purification

[0041] Purification conditions: Chromatographic column: a polymer-based packed chromatographic column with a pore size of 10 μm, a diameter and length of the column: 10cm×25cm. Mobile phase: Phase A: 0.1% trifluoroacetic acid aqueous solution by volume; Phase B: Volume percentage concentration 0.1% trifluoroacetic acid acetonitrile solution. Flow rate: 200ml / min. Detection wavelength: 220nm. Gradient: B%: 20-60%, 90min. The injection volume is 25g.

[0042]Purification process: wash the chromatographic column with acetonitrile solution of 90% trifluoroacetic acid by volume, then equilibrate and load the sample, the sample volume is 25g. Gradient elution was performed for 90 minutes, and fractions with a purity gr...

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PUM

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Abstract

The invention discloses a purification method of melanotan II, which mainly solves technical problem of chromatographic column damage caused by strong alkalinity. The purification method comprises the following steps: 1) filtering a melanotan II crude product solution through a 0.45-mu m filter membrane, carrying out gradient elution purification by using a polymer-based filler chromatographic column, a mobile-phase trifluoroacetic acid water solution as a phase A, an acetonitrile trifluoroacetate solution as a phase B, and collecting a peptide solution of primary target peak; 2) carrying out gradient elution purification on the primarily collected peptide solution through a reversed phase silica gel column by using octadecyl bonded silica gel as a stationary phase, a mobile-phase trifluoroacetic acid water solution as a phase A and an acetonitrile trifluoroacetate solution as a phase B, and collecting the peptide solution of target peak; 3) exchanging into acetate by an HPLC (high performance liquid chromatography) salt conversion process; and 4) carrying out rotary evaporation concentration on the final high-purity peptide solution under reduced pressure, and carrying out freeze-drying to obtain the powdery finished peptide product. The purification method disclosed by the method has the advantages of high purity and high yield, sufficiently protects the chromatographic column, lowers the cost, and is convenient for industrialized implementation.

Description

technical field [0001] The invention belongs to the field of HPLC technology, in particular to a method for purifying melanotan II. Background technique [0002] Erectile dysfunction (erectiledysfunction, ED) is a common and frequently-occurring disease in men. According to the Massachusetts Male Aging Study (MMAS), the incidence rate is as high as 52% among men aged 40 to 70. Hundreds of millions of men worldwide suffer from different The degree of ED greatly affects the happiness of human family life. [0003] Melanotan II, a new analogue of melanocyte-stimulating hormone developed by the University of Arizona School of Medicine, has the sequence Ac-Nle-(Cyclo)Asp-His-D-Phe-Arg-Trp-Lys-NH2 , can regulate the central nervous system and induce erection without any stimulation, and the action time lasts up to 4 hours, and the effect of treating ED is obvious. Melanotan II is easy to use and can be taken orally or nasal spray. It is not only used by men, but also has the eff...

Claims

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Application Information

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IPC IPC(8): C07K1/34C07K1/20C07K1/14
Inventor 徐红岩秦敬国
Owner 南京肽业生物科技有限公司
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