Method for detecting enantiomer in vildagliptin midbody

A technology of enantiomers and intermediates, which is applied in the field of high-performance 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: 2017-01-18
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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  • Method for detecting enantiomer in vildagliptin midbody
  • Method for detecting enantiomer in vildagliptin midbody
  • Method for detecting enantiomer in vildagliptin midbody

Examples

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preparation example Construction

[0044] S3. Preparation of mixed solution:

[0045] Weigh (2S)-1-(2-chloroacetyl)-2-pyrrolidinecarbonitrile into the volumetric flask, accurately measure (2R)-1-(2-chloroacetyl)-2- Pyrrolidinecarbonitrile reference substance solution was added to the volumetric flask and diluted to the mark with mobile phase, mixed, shaken, and used 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 optimized 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 optimized ratio is 0.01:1;

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

[0047] Inspection met...

Embodiment 1

[0057] The (2S)-1-(2-chloroacetyl)-2-pyrrolidinecarbonitrile sample with batch number 160104 was selected for its (2R)-1-(2-chloroacetyl)-2-pyrrolidinecarbonitrile Content detection, including the following steps:

[0058] S1, prepare (2S)-1-(2-chloroacetyl)-2-pyrrolidinecarbonitrile test solution:

[0059] Weigh 25mg (2S)-1-(2-chloroacetyl)-2-pyrrolidinecarbonitrile sample into 25mL mobile phase, mix well, and prepare a solution containing 1.0mg of vildagliptin per 1mL, as the test product solution, ready to use.

[0060] S2, prepare (2R)-1-(2-chloroacetyl)-2-pyrrolidinecarbonitrile reference substance solution:

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

[0062] S3. Preparation of mixed solution:

[0063] W...

Embodiment 2

[0073] Select (2S)-1-(2-chloroacetyl)-2-pyrrolidinecarbonitrile samples with the same batch number as in Example 1, for (2R)-1-(2-chloroacetyl)-2-pyrrole The content of alkanecarbonitrile is detected. The difference between this example and Example 1 is only that the parameters of the flow rate in the chromatographic conditions are different, and other detection conditions are consistent with Example 1. In this embodiment, the determination 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℃;

[0078] Flow rate: 0.8mL / min;

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

[0080] After testing, the content of (2R)-1-(2-chloroacetyl)-2-pyrrolidinecarbon...

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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 an intermediate of vildagliptin, in particular to (2S)-1-(2-chloroacetyl)-2-pyrrolidinecarbonitrile A high-performance liquid-phase method for the detection of enantiomers in China. Background technique [0002] Vildagliptin, chemical name (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, it can increase the concentration of GLP-1, promote the production of insulin by islet B cells, and reduce the concentration of glucagon, thereby reducing blood sugar, and has no effect on body weight. Significant effect. The chemical structural formula of vildagliptin is: [0003] [0004] Pharmacokinetic studies in healthy humans have shown that oral vildagliptin is rapidly absorbed and has a bioavailability of approximately 8...

Claims

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Application Information

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Patent Type & Authority Applications(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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