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A hplc method for the resolution of enantiomers of cinacalcet hydrochloride

A technology of cinacalcet hydrochloride and enantiomer, which is applied in the field of high performance liquid chromatography, can solve the problems of complicated operation, high cost, long analysis time, etc., achieve high-purity preparation, ensure stability, and improve symmetry sexual effect

Active Publication Date: 2020-09-22
JIANGSU CONSORT MEDICAL TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Zhang Feng et al. (West China Pharmaceutical Journal, 2014, 29 (1): 075-076) on the same chromatographic column, using n-hexane-ethanol-ethanolamine (95:5:0.1) as the mobile phase, the flow rate is 1.0ml / min, Analyze the content of enantiomers in the starting material R-1-(1-naphthyl)ethylamine of cinacalcet hydrochloride, but when used to analyze cinacalcet hydrochloride, the enantiomers cannot be effectively separated and have an impact on column efficiency
[0008] In conclusion, the above methods either take a long time to analyze, or cannot achieve baseline separation of cinacalcet hydrochloride enantiomers, and all of them have problems such as low sensitivity, cumbersome operation, or high cost.

Method used

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  • A hplc method for the resolution of enantiomers of cinacalcet hydrochloride
  • A hplc method for the resolution of enantiomers of cinacalcet hydrochloride
  • A hplc method for the resolution of enantiomers of cinacalcet hydrochloride

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Experimental program
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Effect test

Embodiment 1

[0044] Instruments and Conditions

[0045] Thermo Fisher U3000 High Performance Liquid Chromatograph;

[0046] Chromatographic column: OJ-H (250mm×4.6mm, 5μm) cellulose-tris(4-methylbenzoate) chiral column;

[0047] Mobile phase volume ratio: n-hexane: absolute ethanol: ethanolamine=70:30:0.1;

[0048] Detection wavelength: 222nm;

[0049] Column temperature: 25°C;

[0050] Flow rate: 0.5ml / min;

[0051] Injection volume: 20 μl.

[0052] Experimental procedure

[0053] R-cinacalcet hydrochloride: Accurately weigh an appropriate amount of R-cinacalcet hydrochloride reference substance, dissolve it with the mobile phase, dilute it with the mobile phase to a solution containing about 2 μg per 1 ml, accurately measure 20 μl and inject it into the chromatograph, record Chromatogram, the chromatogram of R-cinacalcet hydrochloride see figure 1 , the peak is around 9.9min.

[0054] S-cinacalcet hydrochloride solution: accurately weigh an appropriate amount of S-cinacalcet hydr...

Embodiment 2

[0057] Instruments and Conditions

[0058] Thermo Fisher U3000 High Performance Liquid Chromatograph;

[0059] Chromatographic column: OJ-H (250mm×4.6mm, 5μm) cellulose-tris(4-methylbenzoate) chiral column;

[0060] Mobile phase volume ratio: n-hexane: absolute ethanol: ethanolamine = 65: 35: 0.1;

[0061] Detection wavelength: 222nm;

[0062] Column temperature: 25°C;

[0063] Flow rate: 0.5ml / min;

[0064] Injection volume: 20 μl.

[0065] Experimental procedure

[0066] Take an appropriate amount of R-cinnacalcet hydrochloride sample and S-cinnacalcet hydrochloride (or racemate) respectively, dissolve and quantitatively dilute with mobile phase to make about R-cinnacalcet hydrochloride and S - Each 10 μg system suitability solution of cinacalcet hydrochloride, accurately measure 20 μl, inject liquid chromatograph, record the chromatogram, see the chromatogram of system suitability solution Figure 4 , the No. 1 peak in the figure is S-cinnacalcet hydrochloride, the p...

Embodiment 3

[0068] Instruments and Conditions

[0069] Thermo Fisher U3000 High Performance Liquid Chromatograph;

[0070] Chromatographic column: OJ-H (250mm×4.6mm, 5μm) cellulose-tris(4-methylbenzoate) chiral column;

[0071] Mobile phase volume ratio: n-hexane: absolute ethanol: ethanolamine=75:25:0.1;

[0072] Detection wavelength: 222nm;

[0073] Column temperature: 25°C;

[0074] Flow rate: 0.5ml / min;

[0075] Injection volume: 20 μl.

[0076] Experimental procedure

[0077] Take an appropriate amount of R-cinnacalcet hydrochloride sample and S-cinnacalcet hydrochloride (or racemate) respectively, dissolve and quantitatively dilute with mobile phase to make about R-cinnacalcet hydrochloride and S - Each 10 μg system suitability solution of cinacalcet hydrochloride, accurately measure 20 μl, inject liquid chromatograph, record the chromatogram, see the chromatogram of system suitability solution Figure 5 , peak No. 1 in the figure is S-cinnacalcet hydrochloride, which elutes ...

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Abstract

The invention discloses a separation and analysis determination method of a cinacalcet hydrochloride enantiomer. Cellulose-tri(4-methylbenzoate) coated silica gel is selected to be used as a chiral stationary phase; a certain proportion of n-hexane-absolute ethyl alcohol-ethanol amine mixed solvents are used as a flowing phase for separating and analyzing the cinacalcet hydrochloride enantiomer.

Description

technical field [0001] The invention relates to a high-performance liquid chromatography, in particular to a high-performance liquid chromatography for separating enantiomers of cinacalcet hydrochloride. Background technique [0002] Cinacalcet hydrochloride is a second-generation calcium receptor modulator, a new type of compound containing an alkylaniline skeleton in its chemical structure, which can act on calcium receptors of G-protein conjugated receptors. In parathyroid cells, calcium receptors respond to extracellular calcium (Ca 2 + ) is more sensitive to concentration and regulates the secretion of parathyroid hormone (PTH). Binding of cinacalcet hydrochloride to calcium receptors enhances extracellular Ca through allosteric effects 2+ The role of calcium ion receptor activation (calcium ion receptor isomeric agonist). Cinacalcet hydrochloride can also inhibit the secretion of PTH and the proliferation of parathyroid cells, and can reduce the concentration of se...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/047
Inventor 何达陈巍李锋涛孙健岳永力钟灵玉陈毓马甜
Owner JIANGSU CONSORT MEDICAL TECH CO LTD
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