Succinic acid trelagliptin raw medicine and HPLC analysis method of preparation enantiomer thereof

A technology of troxagliptin succinate and enantiomers, which is applied in the field of HPLC analysis of the enantiomers of troxagliptin succinate raw materials and its preparations, can solve problems such as no clear reference significance, and achieve Good separation, high sensitivity, accurate and reliable results

Inactive Publication Date: 2017-03-29
JIANGSU CAREFREE PHARM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no clear reference significance between the HPLC detection conditions of different compounds

Method used

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  • Succinic acid trelagliptin raw medicine and HPLC analysis method of preparation enantiomer thereof
  • Succinic acid trelagliptin raw medicine and HPLC analysis method of preparation enantiomer thereof
  • Succinic acid trelagliptin raw medicine and HPLC analysis method of preparation enantiomer thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] 1. Instruments and conditions

[0054] Instrument: Agilent1260 DAD detector, electronic analytical balance

[0055] Chromatographic column: AD-H chiral chromatographic column 4.6×250mm, 5μm

[0056] Column temperature: 30°C

[0057] Mobile phase 1: ethanol-diethylamine (100:0.1), solvent: methanol

[0058] Flow rate: 0.4ml / min

[0059] 2. Experimental steps

[0060] Accurately weigh about 2.5 mg of S-Trexagliptin reference substance (batch number: 140527-4 source: Jiangsu Kefeiping Pharmaceutical Co., Ltd.) into a 5ml measuring bottle, add methanol to dissolve and dilute to the mark, shake well, and use as impurity 4 stock solution. Accurately weigh about 25mg of the reference substance of troxagliptin succinate (batch number: 140802, source: Jiangsu Kefeiping Pharmaceutical Co., Ltd.), weigh it accurately, put it in a 25ml measuring bottle, and precisely add the above S-trexagliptin stock solution 1ml, add methanol to dilute to the mark, shake well, as a system s...

Embodiment 2

[0063] 1. Instruments and conditions

[0064] Instruments: DIONEX Ultimate 3000, Chromeleon 6.8 workstation, electronic analytical balance

[0065] Chromatographic column: AD-H chiral chromatographic column 4.6×250mm, 5μm

[0066] UV detection wavelength: 278nm

[0067] Column temperature: 30°C

[0068] Flow rate: 0.4ml / min

[0069] Mobile phase 2: ethanol-n-propylamine (100:0.1), solvent: methanol

[0070] Mobile phase 3: ethanol-methanol-n-propylamine (95:5:0.1), solvent: methanol

[0071] Mobile phase 4: ethanol-ethanolamine (100:0.1), solvent: methanol

[0072] Mobile phase 5: ethanol-methanol-ethanolamine (95:5:0.1), solvent: methanol

[0073] 2. Experimental steps

[0074] For the system suitability solution, see the experimental procedure of Example 1 above, and for the chromatogram, see Figure 2-Figure 5 .

Embodiment 3

[0076] Determination of Enantiomers of Trexagliptin Succinate

[0077] 1. Instruments and conditions

[0078] Instruments: DIONEX Ultimate 3000, Chromeleon 6.8 workstation, electronic analytical balance

[0079] Chromatographic column: AD-H chiral chromatographic column 4.6×250mm, 5μm

[0080] UV detection wavelength: 278nm

[0081] Mobile phase: ethanol-ethanolamine (100:0.1), solvent: methanol

[0082] Column temperature: 30°C

[0083] 2. Experimental steps

[0084] Take about 10mg of troxagliptin succinate, put it in a 10ml measuring bottle, add methanol and dilute to the mark, shake well, as the test solution, accurately measure 1ml of the test solution, put it in a 200ml measuring bottle, add methanol to dilute to the mark as a control solution. Precisely measure 10 μl of the control solution and inject it into the liquid chromatograph, adjust the sensitivity of the detector so that the peak height of the main component chromatographic peak is 10% to 20% of the full...

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Abstract

The invention belongs to the technical field of medicine analysis and particularly relates to a succinic acid trelagliptin raw medicine and a testing method of a preparation enantiomer thereof. A chiral chromatographic column with the silica gel surface coated with ADMPC as filler is used, and the uccinic acid trelagliptin enantiomer is measured with a lower alcohol mixed solution and lower aliphatic amine or lower alcohol amine as mobile phases. The method is easy and quick to operate, good in reproducibility and high in sensitivity.

Description

technical field [0001] The invention belongs to the field of drug analysis and detection, and relates to an HPLC analysis method for trexagliptin succinate bulk drug and its preparation enantiomer. Background technique [0002] Trexagliptin succinate, chemical name: (R)-2-((6-(3-aminopiperidin-1-yl)-3-methyl-2,4-dioxo-3,4-di Hydropyrimidin-1(2H)-yl)methyl)-4-fluoro-benzonitrile succinate, molecular formula: C 18 h 20 FN 5 o 2 ・C 4 h 6 o 4 , its chemical structure is as follows: [0003] [0004] Trexagliptin succinate was developed by Takeda Corporation. On March 26, 2015, the Human Drug Committee of the Japanese Ministry of Labor, Health and Welfare (PMDA) recommended approval of the dipeptidyl peptidase 4 (DPP-4) inhibitor trexagliptin succinate ( Trelagliptin Succinate) is used to treat patients with type 2 diabetes, which has the advantage of long half-life and can be taken once a week. Therefore, trexagliptin succinate is becoming an important drug among DPP...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 秦引林
Owner JIANGSU CAREFREE PHARM CO LTD
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