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Method for detecting rasagiline and enantiomer thereof

A technology of enantiomers and ultraviolet detectors, applied in measuring devices, instruments, scientific instruments, etc., can solve problems such as the inability to separate and detect rasagiline mesylate, and achieve good separation

Pending Publication Date: 2020-11-24
CHONGQING PHARSCIN PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method cannot effectively separate and detect rasagiline mesylate and its enantiomers

Method used

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  • Method for detecting rasagiline and enantiomer thereof
  • Method for detecting rasagiline and enantiomer thereof
  • Method for detecting rasagiline and enantiomer thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Use Agilent 1260 high performance liquid chromatograph, ultraviolet detector, chromatographic column (CHIRALCEL OD) with 3,5-dimethyl benzoate derivatized cellulose bonded silica gel as filler, detection wavelength is 272nm, column temperature is 30°C, the mobile phase is n-hexane-isopropanol-diethylamine (90:10:0, the volume ratio, the same below), the flow rate is 1.0ml / min, and the injection volume is 20μl. Get each 10mg of rasagiline mesylate reference substance and rasagiline enantiomer reference substance, weigh accurately, place in 100ml measuring bottle, add n-hexane-isopropanol (90:10, be volume Ratio, the same below) dissolved and diluted to the mark, shaken up, as the test solution. The test solution is injected into the chromatographic column, and the results are shown in figure 1 .

[0027] It can be seen from Figure 1 that, figure 1 The first peak from left to right in the middle is the enantiomer of rasagiline, and the second peak is rasagiline. The tw...

Embodiment 2

[0029] Use Agilent 1260 high performance liquid chromatography, UV detector, chromatographic column (CHIRALCEL AD) with 3,5-dimethylbenzoate derivatized amylose-bonded silica gel as filler, detection wavelength is 272nm, column temperature The temperature is 30°C, the mobile phase is n-hexane-isopropanol-diethylamine (90:10:0), the flow rate is 1.0ml / min, and the injection volume is 20μl. Get each 10mg of rasagiline mesylate reference substance and rasagiline enantiomer reference substance, accurately weighed, place in 100ml measuring bottle, add n-hexane-isopropanol (90:10) to dissolve and Dilute to the mark and shake well as the reference solution. Inject the reference substance solution into the chromatographic column, see the results figure 2 .

[0030] Depend on figure 2 It can be seen that the two peaks have been clearly separated. Although the separation degree of the two peaks is greater than 3.0, the peak tails and the asymmetry is greater than 1.2.

Embodiment 3

[0032] Use Agilent 1260 high performance liquid chromatograph, ultraviolet detector, the chromatographic column (CHIRALCELAD) with 3,5-dimethyl benzoate derivatized amylose-bonded silica gel as filler, the detection wavelength is 272nm, and the column temperature is 30°C, the mobile phase is n-hexane-isopropanol-diethylamine (90:10:0.1), the flow rate is 1.0ml / min, and the injection volume is 20μl. Get each 10mg of rasagiline mesylate reference substance and rasagiline enantiomer reference substance, accurately weighed, place in 100ml measuring bottle, add n-hexane-isopropanol-diethylamine (90: 10:0.1) was dissolved and diluted to the mark, shaken well, as the reference substance solution. Inject the reference substance solution into the chromatographic column, see the results image 3 .

[0033] Depend on image 3 It can be seen that after adding 0.1% diethylamine in the mobile phase, the peak shape is obviously improved, and the separation degree of the two peaks is great...

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Abstract

The invention discloses a method for separating and detecting rasagiline and an enantiomer thereof. 3, 5-dimethyl benzoate derivatized amylose bonded silica gel is used as a chromatographic column ofa filler; hPLC ultraviolet detection is carried out, the detection wavelength is 272 nm, the column temperature is 30 DEG C, the mobile phase is n-hexane-isopropanol-diethylamine (85-95: 15-5: 0-0.1),the flow velocity is 1.0 ml / min, and the sample size is 20 [mu] l. Rasagiline and the chiral isomer thereof can be well separated, and the peak pattern is good.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular to a method for detecting rasagiline and its enantiomers. Background technique [0002] Rasagiline mesylate is an irreversible and selective inhibitor of monoamine oxidase. Monoamine oxidase is an enzyme involved in the metabolic degradation of dopamine in the brain. After the enzyme is inhibited, the signal transmission of dopamine is enhanced, which is beneficial to Parkinson's disease and also It can enhance the effect of levodopa, so the drug is used for the treatment of Parkinson's disease, and can also be used as an adjuvant drug for levodopa. [0003] From the chemical structure of rasagiline mesylate (compound of formula I below), it can be seen that the drug contains a chiral center, and enantiomeric impurities (compound of formula II below) may be introduced during the synthesis of the drug, Since the result of this impurity is highly similar to that of rasagiline m...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N3/06G01N30/74
CPCG01N30/02G01N3/06G01N30/74
Inventor 王涛莫小霞张婷婷刘森范林沈浩游洪涛刘小英游雪丹杜梅霞
Owner CHONGQING PHARSCIN PHARM CO LTD
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