Ultra-high performance liquid chromatography analysis method of semaglutide

An ultra-high performance liquid chromatography and chromatographic analysis technology, which can be used in analytical materials, material separation, measurement devices, etc., and can solve problems such as unclear toxicological data, patient medication risks, and impact on the quality of semaglutide products.

Active Publication Date: 2021-01-29
HUBEI JIANXIANG BIOLOGICAL PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] During the synthesis and storage of semaglutide, a series of process impurities and degradation impurities are inevitably produced, such as: D-Thr impurities, D-His impurities, the existence of impurities affects the product quality of semaglutide, and these The toxicological data of the impurity is not yet clear, and there must be potential risks for patients
At present, there are few analysis methods for semaglutide content in the market. In order to monitor the product quality of semaglutide and improve the stability of patients’ medication, it is urgent to develop a quality analysis method for semaglutide.

Method used

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  • Ultra-high performance liquid chromatography analysis method of semaglutide
  • Ultra-high performance liquid chromatography analysis method of semaglutide
  • Ultra-high performance liquid chromatography analysis method of semaglutide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Chromatographic conditions

[0068]Instrument: ACQUITY CLASS-H (Wterse)

[0069] Chromatographic column: Chromatographic column 1: C8 column and C4 column in series

[0070] Column 2: C4 column and C18 column connected in series

[0071] Column 3: C8 column and C18 column connected in series

[0072] Mobile phase A: a mixed aqueous solution of 10mmol / L sodium perchlorate and 1mmol / L potassium hexafluorophosphate, adjust the pH to 3.0 with perchloric acid;

[0073] Mobile Phase B: Acetonitrile

[0074] Flow rate: 0.3ml / min

[0075] Column temperature: 45°C

[0076] Injection volume: 0.2μL

[0077] Detection wavelength: 214nm

[0078] Elution gradient: time: 0-120min, mobile phase B: 35-45%

[0079] The test was carried out with three different chromatographic columns connected in series, and 0.2ul of the test solution was accurately measured and injected into the chromatograph, and the chromatogram was recorded. The test results are shown in Table 1.

[0080] Ta...

Embodiment 2

[0085] Chromatographic conditions

[0086] Instrument: ACQUITY CLASS-H (Wterse)

[0087] Chromatographic column: C8 column and C4 column connected in series

[0088] Mobile phase A1: a mixed aqueous solution of 10mmol / L sodium perchlorate and 1mmol / L potassium hexafluorophosphate, adjust the pH to 3.0 with perchloric acid;

[0089] Mobile phase A2: 10mmol / L sodium perchlorate, adjust the pH to 3.0 with perchloric acid;

[0090] Mobile phase A3: a mixed aqueous solution of 10mmol / L sodium perchlorate, 1mmol / L potassium hexafluorophosphate, and 1mmol / L sodium trifluoroacetate, adjust the pH to 3.0 with perchloric acid;

[0091] Mobile Phase B: Acetonitrile

[0092] Flow rate: 0.3ml / min;

[0093] Column temperature: 50°C

[0094] Injection volume: 0.2μL

[0095] Detection wavelength: 214nm

[0096] Elution gradient: time: 0-120min, mobile phase: B: 35-45%;

[0097] The mobile phase A of the following three different ion-pairing solvents was tested respectively, and 0.2ul ...

Embodiment 3

[0103] Chromatographic conditions

[0104] Instrument: ACQUITY CLASS-H (Wterse)

[0105] Chromatographic column: C8 column and C4 column connected in series;

[0106] Mobile phase A: a mixed aqueous solution of 10mmol / L sodium perchlorate and 1mmol / L potassium hexafluorophosphate;

[0107] Mobile phase pH1: adjust the pH to 3.0 with perchloric acid;

[0108] Mobile phase pH2: adjust the pH to 2.0 with perchloric acid;

[0109] Mobile phase pPH3: adjust the pH to 4.0 with perchloric acid;

[0110] Mobile phase B: acetonitrile;

[0111] Flow rate: 0.3ml / min;

[0112] Column temperature: 55°C

[0113] Injection volume: 0.2μL

[0114] Detection wavelength: 214nm

[0115] Elution gradient: time: 0-60min, mobile phase B: 35-45%;

[0116] The following 3 different pHs were tested respectively, and 0.2ul of the test solution was accurately measured and injected into the chromatograph, and the chromatogram was recorded. The test results are shown in Table 3.

[0117] table 3 ...

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Abstract

The invention discloses an ultra-high performance liquid chromatography analysis method of semaglutide. The method is characterized by comprising the following steps: in an ultra-high performance liquid chromatograph, respectively mixing a mobile phase A and a mobile phase B according to different proportions to obtain a mobile phase, and carrying out gradient elution on a semaglutide sample, wherein the mobile phase A is selected from a mixed aqueous solution of one or more of trifluoroacetate, perchlorate and hexafluorophosphate, and the pH value is adjusted to be 2-4, and the mobile phase Bis selected from methanol, isopropanol and acetonitrile. According to the method, chromatographic column series connection and multiple buffer salt mixed elution technologies are adopted, and the product quality of the semaglutide can be accurately and effectively detected under specific chromatographic conditions, so that the medication stability of a patient is improved.

Description

technical field [0001] This field relates to a field of polypeptides, in particular to an ultra-high performance liquid chromatography analysis method for semaglutide. Background technique [0002] Semaglutide, whose English name is Semaglutide, is a new type of long-acting glucagon-like peptide-1 (GLP-1) analog developed and produced by Novo Nordisk, Denmark, for the treatment of type II diabetes. Semaglutide has the effects of lowering blood sugar, losing weight and protecting cardiovascular system, and was recommended by the FDA for approval on October 18, 2017. After the Lys side chain of semaglutide is modified by PEG, Glu and octadecanedicarboxylic acid, the hydrophilicity is greatly improved, and the binding force with albumin is enhanced; at the same time, after the Ala at the second position of the N-terminus is mutated into Aib, the effective It avoids being inactivated by DPP-IV enzymatic hydrolysis, and its half-life reaches 40 hours. Patients only need to injec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/36G01N30/54G01N30/60
CPCG01N30/02G01N30/36G01N30/54G01N30/6039
Inventor 姚志勇付玉清张伯钱姚林江煌余
Owner HUBEI JIANXIANG BIOLOGICAL PHARM CO LTD
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