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A method for measuring the content of l-prolinamide synthesis process impurities or its structural analogue reference substance

A technology of impurity reference substance and synthesis process, which is applied in the field of analysis and determination, can solve the problems that the sample volume cannot meet the requirements and the consumption of the reference substance is huge, and achieves the effect of a reliable quantitative method and low sample consumption.

Active Publication Date: 2022-05-17
南京江北新区生物医药公共服务平台有限公司
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Problems solved by technology

Hereinafter referred to as impurity A, if the traditional mass balance method is used for quantification, the consumption of the reference substance is huge, and the sample volume cannot meet the requirements

Method used

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  • A method for measuring the content of l-prolinamide synthesis process impurities or its structural analogue reference substance
  • A method for measuring the content of l-prolinamide synthesis process impurities or its structural analogue reference substance
  • A method for measuring the content of l-prolinamide synthesis process impurities or its structural analogue reference substance

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Experimental program
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Effect test

Embodiment 1

[0031] 1) Experimental equipment: Bruker Avance III HD 400M nuclear magnetic resonance spectrometer, Mettler XP 6 analytical balance.

[0032] 2) Drugs: Octahydro-4H-dipyrrolo[1,2-b:2',1'-g][1,2,5]triazepine-4,6(5H)-dione is self-made The impurity produced in the synthesis process of L-prolinamide, the specific structure is Hereinafter referred to as impurity A; Dimethyl sulfoxide-d6 (solvent), maleic acid reference substance (internal standard);

[0033] 3) Test method:

[0034] (1) First set the parameters of the NMR spectrometer: pulse sequence: zg30, spectral width: 5000Hz, center frequency: 2100Hz, number of sampling points: 64K, relaxation delay time: 20s, sampling times: 32 times, empty sweep times: 4 times;

[0035] Accurately weigh 43.720mg of maleic acid as an internal standard, put it in a 10mL volumetric flask, use dimethyl sulfoxide-d6 to make up the volume, shake well, and use it as the internal standard solution;

[0036] Accurately weigh 8.00mg of impurity...

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Abstract

The invention discloses a method for measuring the content of L-proline amide synthesis process impurities or its structural analog reference substance. Firstly, a solvent, an internal standard, and a quantitative peak are selected; optimized spectrometer parameters for nuclear magnetic resonance analysis are set, Under these parameters, octahydro-4H-dipyrrolo[1,2-b:2',1'-g][1,2,5]triazepine-4,6(5H)-dione or The integral area of ​​each quantitative target peak in its structural analogue sample and internal standard thereby calculates content; Assay method of the present invention is a kind of effective method that assigns value under the situation that reference substance amount is relatively few; And for It is feasible for the measurement object without ready-made standard products, and compared with the traditional mass balance method, except that the sample consumption is as low as 4 mg, it is simpler and faster; the measurement method of the present invention is octahydro-4H-two Pyrrolo[1,2‑b:2',1'‑g][1,2,5]triazepine‑4,6(5H)‑dione and its structural analogues provide a simple and reliable quantitative method.

Description

technical field [0001] The invention relates to the technical field of analysis and determination, in particular to a method for determining the content of an L-prolinamide synthesis process impurity or a structural analog reference substance thereof. Background technique [0002] L-prolineamide is an important intermediate in the synthesis of peptides and chiral drugs, and is also used as a chiral ligand for asymmetric catalyzed synthesis reactions, used in Robinson illusion reactions and Aldol reactions, etc., and is also a raw material for health products. L-prolineamide is the raw material for the synthesis of vitagliptin for the treatment of type 2 diabetes and the anticancer drug Leuprolide A cetate; the research on its industrial synthesis is of great significance, but in the synthesis process of L-prolineamide, the reaction time is long, The whole reaction will produce too many by-products, that is, impurities, and impurity control is one of the core contents of drug...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N24/08G01N1/28
Inventor 项伟程润
Owner 南京江北新区生物医药公共服务平台有限公司
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