Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of purification method of moxidectin

A technology of moxidectin and purification method, applied in the field of medicinal chemistry purification, can solve the problems of large amount of solvent, complicated operation process, complicated operation and the like

Active Publication Date: 2021-04-13
SEPAX TECH
View PDF6 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The Chinese patent with publication number CN101372492A provides a method for preparing high-purity moxictine, but the process is complex, multi-step chromatography is required, and the amount of solvent used is large and the operation is complicated
The Chinese patent with the publication number CN107216338A provides a method for separating and purifying moxidectin. It adopts a supercritical fluid chromatography system, uses silica gel matrix filler as a stationary phase, supercritical carbon dioxide as a mobile phase, and uses methanol as an entrainer. Can be separated and purified to obtain more than 96% pure product, but does not provide information such as yield, and requires special equipment
The Chinese patent with the publication number CN107686489A provides a method for the separation and purification of high-purity moxidectin. The purity of the final pure product that can be obtained is about 98%, and the yield is 74% to 83%. After chromatographic purification, mycocin needs to be purified by crystallization. The operation process is still somewhat complicated, and crystallization requires the use of a large amount of organic solvents, which is not suitable for industrial production.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of purification method of moxidectin
  • A kind of purification method of moxidectin
  • A kind of purification method of moxidectin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Chromatographic column: moxidectin preparative column (100mm×250mm) (the filler used is polystyrene / divinylbenzene (PS / DVB) with a cross-linking degree of 80% as the matrix, and the matrix contains phenyl functional groups)

[0034] mobile phase:

[0035] The first mobile phase: 0.1% formic acid aqueous solution; the second mobile phase (mobile phase B): methanol (containing 0.1% formic acid)

[0036] Flow rate: 400ml / min Injection volume: 400ml Column temperature: room temperature

[0037] Sample: 100mg / ml Pressure: 1.2MPa

[0038] Instrument: Sepax preparative chromatograph

[0039] Detection wavelength: UV@242nm

[0040] Isocratic elution: 75% B

[0041] The specific method is as follows:

[0042] 1. Sample weighing: weigh 40g of the crude moxidectin on an analytical balance;

[0043] 2. Solvent preparation: prepare 400ml of 75% methanol aqueous solution containing 0.1% formic acid: take 300ml of methanol, 100ml of purified water, and 400μl of formic acid with ...

Embodiment 2

[0056] Get 40g of moxidectin crude product, purity 80.09% (m / m), add 80% ethanol (V / V) 400ml containing 0.1% trifluoroacetic acid, stir to fully dissolve; The chromatographic column (100mm×250mm, containing about 0.71kg of filler mass) after % ethanol balance, the sample loading flow rate is 200 ml / min, and 80% mobile phase B is used after sample loading (mobile phase A is water, and mobile phase B is containing 0.1% ethanol of trifluoroacetic acid) was used as the eluent for elution, the elution flow rate was 400ml / min, and the total elution was 100min. The moxidectin component solution was collected by HPLC detection, and the qualified components were combined, and the moxicillin was obtained after lyophilization. The pure mycin was 29.87g, the HPLC detection purity was 99.02%, and the recovery rate was 74.68%.

Embodiment 3

[0058] Get moxidectin crude product 71g (10% of column packing weight), purity 94.86% (m / m), add 70% acetonitrile (V / V) 400ml of 0.1% trifluoroacetic acid, stir and make fully dissolving; Chromatographic column (100mm * 250mm, containing about 0.71 kg of filler quality) after the 70% acetonitrile equilibrium of % trifluoroacetic acid, the loading flow rate 200ml / min, use 70% acetonitrile mobile phase B after loading the sample (mobile phase A is Water, mobile phase B is the acetonitrile containing 0.1% trifluoroacetic acid) as eluent elution, elution flow rate 400ml / min, elution altogether 100min, HPLC detects and collects the moxidectin component solution, merges qualified components, After freeze-drying, 55.51 g of pure moxidectin was obtained. The HPLC detection purity was 99.09%, and the recovery rate was 78.18%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
cross-linking degreeaaaaaaaaaa
cross-linking degreeaaaaaaaaaa
recovery rateaaaaaaaaaa
Login to View More

Abstract

The invention provides a method for purifying moxidectin, comprising: S1) mixing and fully dissolving the crude moxidectin with a solvent to obtain a sample solution; S2) purifying the sample solution by column chromatography, The moxidectin is obtained; the chromatographic filler of the column chromatography is based on a highly cross-linked polystyrene / divinylbenzene copolymer. Compared with the prior art, the present invention adopts the method of column chromatography purification, which can increase the loading amount of the chromatographic process. The purification method is simple in process, and the amount of solvent used is small, and the recovery rate and purity of moxidectin in the whole process are All are relatively high, and the type of filler used, the type of solvent and the industrial scale-up process route of a large number of products are similar, which can be industrialized and passed the pilot test.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemical purification, and in particular relates to a method for purifying moxidectin. Background technique [0002] Moxidectin (MOX), also known as moxidectin, is an abamectin drug, a large single-structured drug that is chemically modified or derived from nemadectin produced by Streptomyces fermentation. Cyclic lactone antibiotics are a new type of antiparasitic drugs. Antiparasitic drugs are widely used in basic agriculture such as animal husbandry and aquaculture, and the international demand for antiparasitic drugs has continued to grow. Compared with other avermectins, moxidectin has a single ingredient, higher anthelmintic activity, long-term effect, safety and other characteristics, and has a broad market prospect. [0003] The Chinese patent with the publication number CN101372492A provides a method for preparing high-purity moxictine, but the process is complicated, multi-step chroma...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/22
CPCC07D493/22
Inventor 贺元康王艺
Owner SEPAX TECH