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Liquid chromatographic analysis method of L-prolinamide

A liquid chromatographic analysis, prolineamide technology, applied in the direction of analysis materials, material separation, measuring devices, etc., can solve the problems of weak ultraviolet absorption, difficult sample detection, etc., and achieve the effect of high separation degree

Inactive Publication Date: 2018-06-29
ZHEJIANG TIANYU PHARMA
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Problems solved by technology

[0004] The ultraviolet absorption of L-prolinamide and D-prolinamide is all weak, and conventional high-performance liquid chromatography (HPLC) with ultraviolet detector cannot detect the content of L-prolinamide and D-prolinamide sensitively , there is a problem that the sample is not easy to be detected

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  • Liquid chromatographic analysis method of L-prolinamide
  • Liquid chromatographic analysis method of L-prolinamide
  • Liquid chromatographic analysis method of L-prolinamide

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Experimental program
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Embodiment Construction

[0038] specific implementation plan

[0039] Testing equipment : High performance liquid chromatography equipped with UV detector

[0040] Chromatographic conditions :

[0041] Chromatographic column: DAICEL CHIRALPAK IC 4.6×250mm, 5um

[0042] Mobile phase: n-hexane-ethanol (40 / 60(v / v))

[0043] Detection wavelength: 262nm

[0044] Flow rate: 1.0ml / min

[0045] Column temperature: 30°C

[0046] Injection volume: 10μL

[0047] Sample tray temperature control: 15°C

[0048] Running time: 30min

[0049] Solution preparation :

[0050] Diluent: Accurately pipette 1.0ml of trifluoroacetic acid into 1000ml of ethanol and mix well.

[0051] Test solution: Accurately weigh 50mg of L-prolinamide sample in a 25ml volumetric flask, dissolve and dilute to the mark with diluent, and shake well.

[0052] FMOC-Cl solution: Accurately weigh 15 mg of FMOC-Cl sample, dissolve it in 5 ml of acetonitrile, and mix well. (sealed, stored at 4°C, ready to use).

[0053] 1% triethyl...

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Abstract

The invention provides a liquid chromatographic analysis method of L-prolinamide. The liquid chromatographic analysis method comprises the following steps: precisely measuring an L-prolinamide solution, a triethylamine ethanol solution and a derivatization reagent solution respectively, and uniformly mixing through vortex; reacting for a period of time; then adding a diethylamine ethanol solutionand uniformly mixing through the vortex; reacting for a period of time; then adding a trifluoroacetic acid ethanol solution and uniformly mixing through the vortex to obtain an L-prolinamide derivative solution; carrying out chromatographic analysis on the L-prolinamide derivative solution. The liquid chromatographic analysis method provided by the invention can be used for accurately and sensitively detecting the L-prolinamide and D-prolinamide.

Description

technical field [0001] The invention relates to the field of medicine, in particular to a liquid chromatography analysis method for L-prolineamide. Background technique [0002] L-prolinamide is an important chiral intermediate for the synthesis of vildagliptin (Vildagliptin), and its enantiomer D-prolinamide usually exists in commercially available L-prolinamide products, the structural formula of the two They are as follows: [0003] [0004] The ultraviolet absorption of L-prolinamide and D-prolinamide is all weak, and conventional high-performance liquid chromatography (HPLC) with ultraviolet detector cannot detect the content of L-prolinamide and D-prolinamide sensitively , there is a problem that the sample is not easy to be detected. Therefore, it is necessary to develop an analytical method that can accurately and sensitively detect the content of L-prolinamide and D-prolinamide, so as to effectively control the content of chiral isomers in the subsequent vildag...

Claims

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Application Information

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IPC IPC(8): G01N30/02C07D207/16
CPCC07D207/16G01N30/02
Inventor 包策应燕飞王臻朱国荣屠勇军
Owner ZHEJIANG TIANYU PHARMA
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