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Purity determination method for gonadotropin

A gonadotropin and determination method technology, applied in measurement devices, instruments, scientific instruments, etc., can solve problems such as inability to separate effectively, the molecular weight difference is not very large, and the main peak and impurity peak cannot be effectively separated.

Inactive Publication Date: 2014-10-15
SHANGHAI TECHWELL BIOPHARMACEUTICALS CO LTD
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0013] It can be seen that the current liquid phase analysis method for the purity of gonadotropins for the treatment of infertility is not ideal. Cannot be separated very efficiently on existing molecular exclusion media
Secondly, since this type of glycoprotein contains multiple sugar chains, and each sugar chain has a large degree of diversity, the same glycoprotein also has a certain difference in molecular weight. Therefore, in molecular exclusion What is reflected in the liquid phase is peak broadening, which can easily cause the main peak and impurity peaks to be effectively separated
Thirdly, due to the diversity of glycoproteins in nature, and the nature of impurities is similar to that of the main active ingredient, it is impossible to conduct effective purity analysis by separation and analysis methods of other principles
[0014] People have also tried to increase the column length by connecting two gel chromatographic columns in series, and increase the number of theoretical plates, thereby improving the separation effect of impurities. The detection of impurities has been significantly improved, but the detection of small molecule impurities in high-purity follicle stimulating hormone has not improved significantly
[0015] In addition, in the preparation process of gonadotropin APIs and gonadotropin preparations, the quality of the raw materials used for the preparation, such as gonadotropin powder and gonadotropin APIs, is directly related to the quality of the final product. If the quality of the raw materials used does not meet the requirements, the prepared product will also not meet the pharmaceutical quality standards

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  • Purity determination method for gonadotropin
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  • Purity determination method for gonadotropin

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preparation example Construction

[0130] Preparation of Gonadotropin APIs

[0131] The inventor has also obtained a method for preparing gonadotropin bulk drugs, said method comprising the following steps:

[0132] A, with the method for measuring the purity as described in the first aspect of the present invention, measure the total impurity content in the former powder of gonadotropins;

[0133] B. If the measurement result of step (A) shows that the total impurity content in the raw powder is > 2%, then the raw powder is repurified until the measurement result shows that the total impurity content is ≤ 2%;

[0134] C. If the measurement result of step (A) shows that the total impurity content in the raw powder is ≤ 2%, then add a pharmaceutically acceptable amount of excipients to the raw powder of gonadotropins to prepare raw materials of gonadotropins medicine.

[0135] By using the determination method provided by the inventor, the purity of the gonadotropin raw powder is analyzed and determined, so as...

Embodiment 1

[0152] HPLC Purity Analysis of FSH API

[0153] Sample to be analyzed: FSH API (produced by Shanghai Tianwei Bio-Pharmaceutical Co., Ltd., batch number: 111201, biological potency in terms of FSH 256.8IU / mg)

[0154] Method 1: This method adopts the liquid chromatography method of the literature "Compositional Analyzes of a Human Menopausal Gonadotrophin Preparation Extracted from Urine (menotropin)" to carry out the HPLC purity analysis of FSH.

[0155] Mobile phase: Take 71.6g of disodium hydrogen phosphate, add 700ml of water to dissolve, adjust the pH value to 7.0 with phosphoric acid, add water to 800ml, add 200ml of acetonitrile, mix, filter, and ultrasonically degas.

[0156] Get FSH crude drug 28.90mg, dissolve with mobile phase and make the solution that contains 500 units in every 1ml calculated by the marked amount, as need testing solution. Measured according to high performance liquid chromatography (Appendix VD of Part Two of the Chinese Pharmacopoeia 2010 Editi...

Embodiment 2

[0171] HPLC Purity Analysis of FSH API

[0172] Sample to be analyzed: FSH raw material drug (provided by Shanghai Tianwei Biopharmaceutical Co., Ltd., batch number: 100401, biological potency is 289.5IU / mg in terms of FSH)

[0173]Method 1: In this method, a TSK G2000SWXL (7.8×300mm) chromatographic column and a Superdex75 10 / 300GL chromatographic column are used for liquid chromatography in series to analyze the HPLC purity of FSH.

[0174] Mobile phase: 50mM sodium dihydrogen phosphate, pH7.0-acetonitrile (80:20).

[0175] Get FSH crude drug 28.72mg, dissolve with mobile phase and make the solution that contains 3500 units in every 1ml calculated by labeling amount, as need testing solution. Determined with reference to high-performance liquid chromatography (Appendix VD of Part Two of the Chinese Pharmacopoeia 2010 Edition). TSK G2000SWXL (7.8×300mm) and Superdex75 10 / 300GL are connected in series as the analytical chromatographic column, the flow rate is 0.5ml per minut...

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Abstract

The invention discloses an HPLC purity determination method for gonadotropin. Specifically, the invention provides a high pressure liquid chromatography determination method for raw powder and / or bulk drugs by a molecular exclusion chromatography column filled by sephadex or cross-linked agarose or a mixed cross-linked material of the two, wherein the main peak USP theoretical plate number of the molecular exclusion chromatography column is not less than 1600. The method has good specificity, accuracy and repeatability.

Description

technical field [0001] The present invention relates to the purity analysis of gonadotropins. In particular, it relates to the purity analysis of human urinary follicle-stimulating hormone. Background technique [0002] Gonadotropins for the treatment of infertility are a class of glycoprotein substances with close structures, including chorionic gonadotropin (HCG), menopausal gonadotropin (HMG), follicle stimulating hormone (FSH), and luteinizing hormone (LH) , wherein the menopausal gonadotropin is a mixture containing follicle-stimulating hormone and luteinizing hormone in a certain ratio (2:1-1:2). [0003] HCG, FSH, and LH are all composed of two subunits of α chain and β chain in the form of non-covalent bonds, in which their α subunits are completely identical, with 92 amino acids, a molecular weight of about 14500D, and positions 52 and 78 The asparagine on is an amino acid that undergoes N-glycosylation. The β subunit of HCG has 145-147 amino acids and a molecula...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/60
Inventor 洪云海王科伟季晓铭
Owner SHANGHAI TECHWELL BIOPHARMACEUTICALS CO LTD
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