A method for detecting enantiomers in vildagliptin intermediates

A technology of enantiomers and intermediates, applied in the field of high-efficiency liquid phase detection of enantiomers in -1--2-pyrrolidinecarbonitrile, can solve the problem of no detection method and peak shape symmetry Not good, can not be improved and other problems, to achieve good effect, strong practicability, easy to adjust the effect

Inactive Publication Date: 2018-10-12
海南欣莱医药科技股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Using this method to test, there are problems such as poor peak shape symmetry, tailing, poor column efficiency, etc., and no detailed detection method is given
Fine-tuning this detection method will not improve the above problems

Method used

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  • A method for detecting enantiomers in vildagliptin intermediates
  • A method for detecting enantiomers in vildagliptin intermediates
  • A method for detecting enantiomers in vildagliptin intermediates

Examples

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preparation example Construction

[0044] S3, the preparation of mixed solution:

[0045] Weigh (2S)-1-(2-chloroacetyl)-2-pyrrolidinecarbonitrile into a volumetric flask, and accurately measure (2R)-1-(2-chloroacetyl)-2- Add the pyrrolidinecarbonitrile reference substance solution into a volumetric flask and dilute to the mark with mobile phase, mix and shake well, and use it as a mixed solution for later use. According to the mass volume ratio (g / L), the ratio of (2S)-1-(2-chloroacetyl)-2-pyrrolidinecarbonitrile:mobile phase is 0.1~5:1, and the optimal ratio is 1:1; According to the mass volume ratio (g / L), the ratio of (2R)-1-(2-chloroacetyl)-2-pyrrolidinecarbonitrile:mobile phase is 0.001~0.1:1, and the optimal ratio is 0.01:1;

[0046] S4, draw equal amount of reference substance solution, need testing solution and mixed solution respectively, inject in the high-efficiency chromatograph and measure, and the determination condition of described high-efficiency liquid chromatography comprises:

[0047] Insp...

Embodiment 1

[0057] Choose the (2S)-1-(2-chloroacetyl group)-2-pyrrolidine carbonitrile sample that is 160104 batch number, its (2R)-1-(2-chloroacetyl group)-2-pyrrolidine carbonitrile content is detected, including the following steps:

[0058] S1. Preparation of (2S)-1-(2-chloroacetyl)-2-pyrrolidinecarbonitrile test solution:

[0059] Weigh 25mg of (2S)-1-(2-chloroacetyl)-2-pyrrolidinecarbonitrile sample and add 25mL of mobile phase, after mixing evenly, it is formulated into a solution containing 1.0mg of vildagliptin per 1mL as the test solution Product solution, ready to use.

[0060] S2. Preparation of (2R)-1-(2-chloroacetyl)-2-pyrrolidinecarbonitrile reference substance solution:

[0061] Weigh an appropriate amount of (2R)-1-(2-chloroacetyl)-2-pyrrolidinecarbonitrile reference substance, weigh it accurately, dissolve the mobile phase and quantitatively dilute it to make a solution containing about 100 μg per 1 mL, as (2R )-1-(2-chloroacetyl)-2-pyrrolidinecarbonitrile reference s...

Embodiment 2

[0073] Choose the (2S)-1-(2-chloroacetyl)-2-pyrrolidine carbonitrile sample of the same batch as in Example 1, to (2R)-1-(2-chloroacetyl)-2-pyrrole The content of alkanecarbonitrile is detected, the difference between this embodiment and embodiment 1 is only: the parameter of flow velocity in the chromatographic condition is different, and other detection conditions are consistent with embodiment 1. In this embodiment, the assay conditions of high performance liquid chromatography include:

[0074] Chromatographic column: CHIRALPAK IC (model: length 250mm, inner diameter 4.6mm, cellulose surface covalently bonded silica filler, filler particle size 5μm);

[0075] Detector: UV detector;

[0076] Detection wavelength: 210nm;

[0077] Column temperature: 30°C;

[0078] Flow rate: 0.8mL / min;

[0079] Mobile phase: Calculated by volume ratio, n-butanol:ethanol:diethylamine=60:40:0.05.

[0080] It can be seen through detection that the content of (2R)-1-(2-chloroacetyl)-2-pyrro...

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Abstract

The invention discloses a method for detecting enantiomer in a vildagliptin midbody. The chromatographic conditions of the method are that a CHIRALPAK IC chromatographic column is adopted, the column temperature is 25-40 DEG C, the detection wavelength is 210nm, the mobile phase is a mixture of n-butyl alcohol, ethanol and diethylamine, and the flow velocity is 0.8-1.2mL / min. By adopting the method disclosed by the invention, quantitative analysis on the enantiomer (2R)-1-(2-chloracetyl)-2-pyrrolidine formonitrile in (2S)-1-(2-chloracetyl)-2-pyrrolidine formonitrile can be implemented, the enantiomer can be effectively separated and detected, peak patterns are in symmetry without trailing, aspects such as the separation degree, the specificity, the limit of quantitation, the detection limit, the linearity, the precision degree, the accuracy degree, the solution stability and the durability need to be specifically verified, various verification results meet requirements of related rules and guidance principles, and a good detection effect can be achieved.

Description

technical field [0001] The invention belongs to the technical field of medicine and relates to a method for detecting enantiomers in vildagliptin intermediates, in particular to (2S)-1-(2-chloroacetyl)-2-pyrrolidinecarbonitrile A high-performance liquid phase detection method for enantiomers. Background technique [0002] Vildagliptin, the chemical name is (S)-1-[2-(3-hydroxy-1-adamantan-1-ylamino]acetyl]pyrrolidine-2-carbonitrile. Vildagliptin By combining with DPP-4 to form a DPP-4 complex to inhibit the activity of this enzyme, while increasing the concentration of GLP-1 and promoting the production of insulin by pancreatic B cells, it also reduces the concentration of glucagon, thereby reducing blood sugar, and has no effect on body weight. Obvious impact. The chemical structural formula of vildagliptin is: [0003] [0004] Pharmacokinetic studies in healthy humans show that oral vildagliptin is rapidly absorbed with a bioavailability of about 85%. The peak time i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/027
Inventor 邝少轶陈年根张鹏威杨雪峰白秉信
Owner 海南欣莱医药科技股份有限公司
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