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Method for detecting enantiomer in pramipexole dihydrochloride and method for separating enantiomer from pramipexole dihydrochloride

A technology of pramipexole hydrochloride and enantiomers, which is applied in the detection of enantiomers in pramipexole hydrochloride and the separation of the two, can solve the problems of poor resolution and unsatisfactory separation effect, etc. To achieve the effect of ensuring quality control

Active Publication Date: 2014-04-02
SICHUAN KELUN PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The European Pharmacopoeia (EP6.8 version) uses normal phase silica gel (CHIRALCELOD-H) modified by cellulose derivatives as the chiral stationary phase to determine the enantiomeric impurities in pramipexole hydrochloride, and the resolution is poor. The separation effect is not ideal

Method used

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  • Method for detecting enantiomer in pramipexole dihydrochloride and method for separating enantiomer from pramipexole dihydrochloride
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  • Method for detecting enantiomer in pramipexole dihydrochloride and method for separating enantiomer from pramipexole dihydrochloride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1 Analysis and detection of pramipexole hydrochloride and its enantiomers

[0032] Instrument and chromatographic conditions:

[0033] High performance liquid chromatograph Agilent 1260 (including VWD detector, Agilent chromatographic workstation);

[0034] Chromatographic column: Chiralpak AY-H (Daicel, 250mm×4.6mm, 5μm);

[0035] Mobile phase: n-hexane - isopropanol - diethylamine (85:15:0.1);

[0036] Flow rate: 1.0ml / min;

[0037] Detection wavelength: 254nm;

[0038] Column temperature: 35°C;

[0039] Injection volume: 75 μL.

[0040] Experimental steps:

[0041] Take 6 mg of pramipexole hydrochloride racemate (containing pramipexole hydrochloride and its enantiomers) sample, put it in a 20mL volumetric flask, add 5mL of absolute ethanol to dissolve the sample by ultrasonic, use the mobile phase to make the volume up to the mark, Become a racemate sample solution. Take another 6 mg of pramipexole hydrochloride (S-configuration) sample, put it in a 2...

Embodiment 2

[0045] Embodiment 2 The influence of mobile phase ratio on separation effect

[0046] Instrument and chromatographic conditions:

[0047] High performance liquid chromatograph Agilent 1260 (including VWD detector, Agilent chromatographic workstation);

[0048] Chromatographic column: Chiralpak AY-H (Daicel, 250mm×4.6mm, 5μm);

[0049] Flow rate: 1.0ml / min;

[0050] Detection wavelength: 254nm;

[0051] Column temperature: 35°C;

[0052] Injection volume: 75 μL.

[0053] Experimental steps:

[0054] Take 6mg of pramipexole hydrochloride racemate sample, place it in a 20mL volumetric flask, add 5mL of absolute ethanol to dissolve the sample ultrasonically, and dilute to the mark with mobile phase to become a racemate sample solution. According to the above chromatographic conditions, adjust the ratio of n-hexane containing 0.1% diethylamine to isopropanol to be 90:10, 85:15, and 80:20 respectively, carry out HPLC analysis on the racemate sample solution, and investigate th...

Embodiment 3

[0059] The influence of embodiment 3 flow velocity on separation effect

[0060] Instrument and chromatographic conditions:

[0061] High performance liquid chromatograph Agilent 1260 (including VWD detector, Agilent chromatographic workstation);

[0062] Chromatographic column: Chiralpak AY-H (Daicel, 250mm×4.6mm, 5μm);

[0063] Mobile phase: n-hexane - isopropanol - diethylamine (85:15:0.1);

[0064] Detection wavelength: 254nm;

[0065] Column temperature: 35°C;

[0066] Injection volume: 75 μL.

[0067] Experimental steps:

[0068] Take 6 mg of pramipexole hydrochloride racemate sample, place it in a 20mL volumetric flask, add 5mL of absolute ethanol to dissolve the sample ultrasonically, and dilute to the mark with mobile phase to become a racemate sample solution. According to the above-mentioned chromatographic conditions, the flow rate is adjusted to be 0.8ml / min, 1.0ml / min and 1.2ml / min, and the racemate sample solution is analyzed by high performance liquid chrom...

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Abstract

The invention provides a method for detecting an enantiomer in pramipexole dihydrochloride. The method adopts a normal-phase high performance liquid chromatography method for detecting the enantiomer, and comprises the following steps: (1) preparing a test sample solution from a pramipexole dihydrochloride sample to be detected; (2) injecting the test sample solution into a high performance liquid chromatographic instrument, and analyzing, wherein chromatographic conditions are as follows: the ratio of a chromatographic column to an amylose derivative chiral column to a flowing phase to normal hexane to isopropanol to an amine solvent is (80-90) to (10-20) to (0.05-0.5), and the detection wavelength is 254+ / -2 nm. A study discovers that pramipexole dihydrochloride can be effectively separated from the enantiomer in pramipexole dihydrochloride by taking the amylose derivative chiral column as a stationary phase and adding a specific proportion of the flowing phase; the durability is good; the content of enantiomer impurities in pramipexole dihydrochloride can be quickly, accurately and sensitively separated and analyzed, so that the mass of pramipexole dihydrochloride and pramipexole dihydrochloride tablets can be effectively controlled.

Description

technical field [0001] The invention relates to a method for detecting enantiomers in pramipexole hydrochloride and a method for separating them. Background technique [0002] Pramipexole hydrochloride, chemical name (S)-2-Amino-4,5,6,7-tetrahydro-6-propylaminobenzothiazole dihydrochloride monohydrate, molecular formula C 10 h 17 N 3 S 2HCl H 2 O, its structural formula is: [0003] [0004] Pramipexole hydrochloride is a non-ergot highly selective dopamine receptor agonist, which can highly selectively act on DA-2 receptors, and its specificity is much higher than that of ergot alkaloid dopamine receptor agonists such as bromocriptine , Pergolet. Improve the clinical symptoms of Parkinson's disease patients by stimulating DA-2 receptors. In the early stage, it can be used alone to treat Parkinson's disease, and in the late stage, it can be used in combination with dopamine to treat Parkinson's disease. [0005] The molecular structure contains one chiral carbon at...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 赵同华吴松童元峰杨庆云邓愉凤王朝阳葛建华姜晓艳赵栋胡思玉王利春王晶翼程志鹏刘革新刘思川
Owner SICHUAN KELUN PHARMA CO LTD
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