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Method for purifying pirarubicin

A technology of pirarubicin and purification method, applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., can solve the problems of cumbersome operation steps, little reference for industrial scale-up production, serious environmental pollution, etc. Small corrosion damage, saving maintenance costs, and low environmental pollution

Inactive Publication Date: 2020-09-18
SEPAX TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the purification method provided by it adopts silica gel column chromatography, which is more serious to environmental pollution, and the purification method needs to adopt a two-step purification method, and its operation steps are cumbersome, which is of reference significance for the industrial scale-up production of pirarubicin purification not big

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  • Method for purifying pirarubicin
  • Method for purifying pirarubicin
  • Method for purifying pirarubicin

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preparation example Construction

[0044]The packing of the preparation column in step S2 of the present invention is a silica gel substrate, and octadecylsilane and divinylbenzene are bonded on the silica gel substrate; wherein, the mass percent of octadecylsilane and divinylbenzene is (1 ~10):1, preferably (2~8):1, more preferably (4~6):1.

[0045] The eluent in steps S2 and S3 of the present invention is organic acid: water: organic solvent: ethyl acetate = 0.5~2: 100~400: 600~900: 20~80; wherein the organic acid is preferably formic acid, tris One or two of fluoroacetic acid; one or more of methanol, ethanol and acetonitrile as the organic solvent.

[0046] In step S3 of the present invention, the combined standard of pure pirarubicin is that the purity of the sample is higher than 99.5%, and the purity of the sample is less than 0.1%.

[0047] 1. Instruments and materials:

[0048] Crude pirarubicin, HPLC (ultraviolet detector), Sepax preparative liquid chromatograph LC6000, one analysis column Sepax-SAP...

Embodiment 1

[0064] Eluent volume ratio: formic acid: water: methanol: ethyl acetate = 1:300:700:50; flow rate: 400ml / min; injection volume: 400ml; column temperature: room temperature; sample: 100mg / ml; pressure: 1.1 MPa;

[0065] Instrument: Sepax preparative chromatograph LC6000; pirarubicin preparative column (100mm×250mm, containing about 0.98kg of filler);

[0066] Detection wavelength: UV@254nm; isocratic elution 70%C;

[0067] The specific method is as follows:

[0068] T1 solvent preparation: prepare two parts of solvent A and B in proportion, the solvent volume ratio is formic acid: water: methanol = 1:300:700, prepare 400ml, two parts; prepare one part of eluent C in proportion, the volume of eluent The ratio is formic acid: water: methanol: ethyl acetate = 1:300:700:50, prepare 30L, one part;

[0069] T2 sample is weighed: take by weighing pirarubicin crude product 40g (content 65.87%, see Table 1 or figure 2 ), and put into the Erlenmeyer flask;

[0070] T3 sample dissol...

Embodiment 2

[0094] Adopt the preparative chromatograph identical with embodiment 1, preparative column and elution method, its difference is:

[0095]Get pirarubicin crude product 65g (loading 6.6%), content 70.15%, with solvent (formic acid: water: acetonitrile=1:350:650, volume ratio) 400ml, magnetic stirring makes fully dissolve; : water: acetonitrile: ethyl acetate = 1:350:650:30) After elution and equilibration, the pirarubicin preparation column (100mm×250mm, containing about 0.98kg of filler mass), the flow rate of the sample solution was 200ml / min, and the Elution with eluent after sample, eluent flow rate 400ml / min, elution 60min altogether, collect pirarubicin purification sample and use HPLC to detect and collect pirarubicin component solution, merge qualified components, after lyophilization 49.68 g of pure pirarubicin was obtained, the purity detected by HPLC was 99.71%, the single impurity was less than 0.1%, and the recovery rate was 76.43%.

[0096] See Table 4 for the de...

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Abstract

The invention provides a method for purifying pirarubicin. The method includes the steps: S1, preparing crude pirarubicin into a sample liquid; S2, injecting the sample liquid into a preparation column; and S3, performing elution for purification and separation so as to obtain a purified pirarubicin pure product, wherein solvents and eluents for purification and separation comprise acid, water andorganic phases, the packing of the preparation column is a silica gel matrix, and the silica gel matrix is bonded with octadecylsilane and divinylbenzene. According to the purification method, the silica gel matrix is adopted as the packing, the packing is special and characteristic filler with silica gel which is bonded with octadecylsilane and divinylbenzene, and pure pirarubicin is obtained after separation and purification are performed, wherein the purity of the pure pirarubicin can reach 99.5% or above, the content of one individual impurity is less than 0.1%, and the recovery rate is 76% or above; the method has convenient operation, time and effort can be saved, little pollution to the environment is caused; and the characteristic filler of the method has long life, and can be utilized repeatedly, and the purification method has been verified by scale-up production, and is suitable for industrial scale-up production.

Description

technical field [0001] The invention relates to the technical field of medicinal chemical purification, in particular to a purification method of pirarubicin. Background technique [0002] Pirarubicin is a red crystalline powder. It is a broad-spectrum anti-tumor antibiotic that has effects on a variety of tumors and belongs to periodic non-specific drugs. It is suitable for the treatment of breast cancer, and also has certain curative effects on malignant tumors such as ureteral cancer, bladder cancer, ovarian cancer, and cervical cancer. Its molecular formula is: C 32 h 37 NO 12 , the molecular weight is: 627.636, and the molecular structural formula is shown in Formula 1: [0003] [0004] Pirarubicin is an anthracycline antibiotic drug. The mechanism of action of this drug is: directly intercalating between DNA double-stranded nucleic acid base pairs, interfering with the transcription process of enzymes, preventing the synthesis of mRNA, and inhibiting DNA polym...

Claims

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Application Information

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IPC IPC(8): C07H1/06C07H17/04
CPCC07H1/06C07H17/04
Inventor 贺元康王艺
Owner SEPAX TECH
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