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Purification method of fulvestrant by normal phase chromatography

A fulvestrant and purification method technology, applied in the directions of organic chemistry, steroids, etc., can solve problems such as low purification efficiency, achieve the effects of good purification efficiency, reduce repeated extraction and washing, and simplify the operation of purification

Active Publication Date: 2022-03-29
JIANGSU HANSOH PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be known from various published synthetic routes that the crude product of fulvestrant needs repeated recrystallization or column chromatography to obtain a qualified product, and the purification efficiency is generally low

Method used

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  • Purification method of fulvestrant by normal phase chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Prepare anhydrous ethanol and n-hexane in a volume ratio of 1:2 to form a mixed solution, ready for use. Dissolve the crude product of fulvestrant in the above solvent, and stir until it dissolves (concentration is about 100 mg / ml). The crude fulvestrant solution was filtered, and the pore size of the filter membrane was 0.45 μm. Collect the filtrate and keep it refrigerated.

Embodiment 2

[0034] Measure 1L of the filtered crude fulvestrant solution, and load it into a 200mm preparative column system (chromatographic column size 250×200mmID.) from the loading pump, with a sample loading flow rate of 1000ml / min and a sample loading pressure of ≤10mPa. After loading the sample, rinse the sample pump with 50ml of absolute ethanol / n-hexane (1:2) solution.

Embodiment 3

[0036] 50g fulvestrant crude product solution is loaded to spherical silica gel chromatographic column (particle diameter 20 μm, pore diameter 250×200mmID.), eluted with 13% methanol / n-hexane for 60 minutes, the detection wavelength is 225nm, and the flow rate is 1200ml / min. When the UV absorption peak rises to 300mAU, it starts to collect, and when the UV absorption peak reaches the highest, Continue to collect until reaching 90% of the maximum value of the UV absorption peak and stop collecting. Complete the elution according to the following purification process parameters. The fractions were collected, and the results of RP-HPLC analysis were as follows: the purity of the main peak was 95.40%, and the maximum single impurity was 0.61%.

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Abstract

The present invention relates to a fulvestrant normal-phase chromatography purification method, in particular to a normal-phase high-performance liquid chromatography purification method of fulvestrant, which can prepare fulvestrant with high purity, comprising the following steps: a. The crude product of the group is adsorbed on the chromatographic column filler; b. Gradient elution with the first mobile phase and the second mobile phase; c. Collecting the positive components to obtain the pure product of fulvestrant. The method improves the fulvestrant purification efficiency, reduces the production cost, and is suitable for large-scale production.

Description

technical field [0001] The invention relates to the field of medicinal chemistry, in particular to a fulvestrant normal phase chromatographic purification method. Background technique [0002] In 2002, fulvestrant was approved by the US FDA to be marketed by AstraZeneca. The product name is Faslodex, which is mainly used for the treatment of postmenopausal advanced breast cancer with estrogen receptor positive and ineffective anti-estrogen therapy. [0003] Fulvestrant (Fulvestrant), the chemical name is 7α-[9-(4,4,5,5,5-pentafluoropentanesulfinyl)nonyl]estro-1,3,5(10)-tri ene-3,17β-diol, molecular formula C 32 h 47 f 5 o 3 S. [0004] [0005] Fulvestrant molecule is composed of steroidal skeleton and 7-position long side chain, which is difficult to synthesize. It can be seen from various published synthetic routes that the crude product of fulvestrant requires repeated recrystallization or column chromatography to obtain a qualified product, and the purification ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J31/00
CPCC07J31/006
Inventor 朱后田吴文涛闫成玉王佩
Owner JIANGSU HANSOH PHARMA CO LTD