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Method for separating and analyzing trelagliptin succinate and preparation related substances thereof

A technology for the separation and analysis of troxagliptin succinate, which is applied in the field of chemical analysis, can solve problems such as inaccurate integration, and achieve the effect of ensuring product quality and good elution and separation effects

Inactive Publication Date: 2017-01-04
WATERSTONE PHARMA WUHAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Members of our research team found in experiments that an unknown impurity often appeared after the main peak of trexagliptin, and this unknown impurity was easily produced under the condition of oxidative degradation of raw materials. Impurities, the unknown impurity is likely to be produced after mixing raw materials and related excipients, and the impurity is very close to the main peak, which is prone to inaccurate integration

Method used

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  • Method for separating and analyzing trelagliptin succinate and preparation related substances thereof
  • Method for separating and analyzing trelagliptin succinate and preparation related substances thereof
  • Method for separating and analyzing trelagliptin succinate and preparation related substances thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Instrument: Agilent 1100 HPLC, VWD detector

[0045] Chromatographic column: Octadecyl bonded silica gel as filler (4.6mm×250mm, 5μm)

[0046] Mobile phase A: 0.02mol / L potassium dihydrogen phosphate buffer solution (containing 0.3% by volume of triethylamine), adjust the pH to 3.0 with phosphoric acid

[0047] Mobile Phase B: Acetonitrile

[0048] The gradient elution is shown in Table 1 below:

[0049] Table 1

[0050]

[0051] Flow rate: 1.0mL / min

[0052] Wavelength: 224nm

[0053] Column temperature: 30°C

[0054] Injection volume: 10μL

[0055] Diluent: mobile phase A

[0056]Experimental procedure: take trexagliptin tablets (the ratio of trexagliptin raw material to microcrystalline cellulose is 1:5), grind it into fine powder with a mortar, weigh the fine powder, and prepare each mL of koji with mobile phase A Gliptin 500μg solution was then analyzed under the above-mentioned gradient elution conditions, and the obtained spectra were as follows figu...

Embodiment 2

[0059] Instrument: Agilent 1100 HPLC, VWD detector

[0060] Chromatographic column: Octadecyl bonded silica gel as filler (4.6mm×250mm, 5μm)

[0061] Mobile phase A: 0.02mol / L sodium dihydrogen phosphate buffer solution (containing 0.3% by volume of triethylamine), adjust pH to 3.0 with phosphoric acid

[0062] Mobile Phase B: Acetonitrile

[0063] The gradient elution is shown in Table 2 below:

[0064] Table 2

[0065]

[0066]

[0067] Flow rate: 1.0mL / min

[0068] Wavelength: 224nm

[0069] Column temperature: 30°C

[0070] Injection volume: 10μL

[0071] Diluent: mobile phase A

[0072] Experimental procedure: take trexagliptin tablets (the ratio of trexagliptin raw material to microcrystalline cellulose is 1:5), grind it into fine powder with a mortar, weigh the fine powder, and prepare each mL of koji with mobile phase A Gliptin 500μg solution was then analyzed under the above-mentioned gradient elution conditions, and the obtained spectra were as follows ...

Embodiment 3

[0075] Instrument: Agilent 1100 HPLC, VWD detector

[0076] Chromatographic column: Octadecyl bonded silica gel as filler (4.6mm×250mm, 5μm)

[0077] Mobile phase A: 0.02mol / L potassium dihydrogen phosphate buffer solution (containing 0.3% by volume of triethylamine), adjust the pH to 3.0 with phosphoric acid

[0078] Mobile Phase B: Acetonitrile

[0079] The gradient elution is shown in Table 3 below:

[0080] table 3

[0081]

[0082] Flow rate: 1.0mL / min

[0083] Wavelength: 224nm

[0084] Column temperature: 30°C

[0085] Injection volume: 10μL

[0086] Diluent: mobile phase A

[0087] Experimental procedure: take trexagliptin tablets (the ratio of trexagliptin raw material to microcrystalline cellulose is 1:5), grind it into fine powder with a mortar, weigh the fine powder, and prepare each mL of koji with mobile phase A Gliptin 500μg solution was then analyzed under the above-mentioned gradient elution conditions, and the obtained spectra were as follows ima...

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Abstract

The invention discloses a method for separating and analyzing trelagliptin succinate and preparation related substances thereof. According to the method, the chromatographic conditions comprise that an octadecyl bonded silica gel is adopted as a stationary phase, a buffer liquid is adopted as a mobile phase A and an organic solvent is adopted as a mobile phase B to carry out gradient elution, and the gradient elution conditions comprise that the mobile phase A is 85-50 (V%) and the mobile phase B is 15-50 (V%) at the time of 0-10 min, the mobile phase A is 50 (V%) and the mobile phase B is 50 (V%) at the time of 25-30 min, and the mobile phase A is 85-50 (V%) and the mobile phase B is 15-50 (V%) at the time of 31-35 min; the sample solution preparation comprises that the sample to be detected is prepared into the sample solution by using the mobile phase A; and separating and analyzing are performed, wherein the sample solution is injected into a high performance liquid chromatography so as to complete the detection of the trelagliptin succinate and the preparation related substances thereof. With the method of the present invention, the trelagliptin and the related substances can be rapidly and effectively separated under the same chromatographic conditions. The detection method of the present invention has advantages of high specificity, high precision, strong accuracy, convenient operation, and effective control of drug quality.

Description

technical field [0001] The invention relates to the field of chemical analysis, in particular to a method for separating and analyzing troxagliptin succinate and related substances of its preparation. Background technique [0002] Trelagliptin succinate (Trelagliptin succinate, the structure shown in formula 1) is a dipeptidyl peptidase IV (DPP-4) inhibitor originally developed by Japan's Takeda (Takeda) company. Sexual and persistent inhibition of DPP-4 to control blood sugar levels. DPP-4 is an enzyme that triggers the inactivation of incretins, glucagon-like peptide-1 (GLP-1) and glucose-dependent insulinotropic polypeptide (GIP), two incretins in Plays an important role in blood sugar regulation. Inhibition of DPP-4 can increase blood glucose level-dependent insulin secretion, thereby controlling blood glucose levels. In March 2015, Trexagliptin Tablets was approved by the Ministry of Health, Labor and Welfare of Japan. The original manufacturer’s Trexagliptin Tablets...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 祝小芬钱丽娜李天宇蔡兰熊丽刘大鹏崔健
Owner WATERSTONE PHARMA WUHAN
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