Method for detecting isomers of dexmedetomidine hydrochloride crude product

A technology of dexmedetomidine hydrochloride and a detection method, applied in the field of detection of isomers in crude dexmedetomidine hydrochloride, can solve the problems of insufficient sensitivity, poor specificity, unsuitable isomer detection and the like, and achieves the The effect of good specificity and high accuracy

Inactive Publication Date: 2017-02-22
CISEN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the specificity of the above-mentioned assay method is poor, and the sensitivity is not high enough, so it is not suitable to detect the isomers in the crude product of dexmedetomidine hydrochloride

Method used

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  • Method for detecting isomers of dexmedetomidine hydrochloride crude product
  • Method for detecting isomers of dexmedetomidine hydrochloride crude product
  • Method for detecting isomers of dexmedetomidine hydrochloride crude product

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Experimental program
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Effect test

Embodiment 1

[0018] The determination of isomers in the crude product of dexmedetomidine hydrochloride is to adopt high performance liquid chromatography, and its chromatographic conditions are chromatographic column: N-oxide lycoperpine M bonded silica gel column; flow rate: 0.5ml / min detection wavelength: 210; Column temperature: 25°C; mobile phase: n-hexane-ethanol-trifluoroacetic acid-diethylamine (95:5:0.3:0.05).

[0019] The preparation steps of the N-lycopine M-bonded silica gel column are: 1) take 20g of activated silica gel in a 500mL three-necked flask, then measure 100mL of toluene and 40mL of γ-aminopropyltriethoxysilane, 120 ℃ in an oil bath, stirred and refluxed for 13 hours, after cooling, the product was washed with toluene and ethanol and filtered until no gel was present; dried at 60 ℃ for 24 hours, and cooled in a drying oven; 2) Added The product of step 1), then add 120mL 35wt% formaldehyde solution and 2mL acetic acid successively, stir and react at room temperature f...

Embodiment 2

[0034] The determination of isomers in the dexmedetomidine hydrochloride crude product adopts high performance liquid chromatography, and its chromatographic conditions are chromatographic column: AS-H type chiral column; Flow rate: 0.5ml / min Detection wavelength: 210; Column temperature: 25°C; mobile phase: n-hexane-ethanol-trifluoroacetic acid-diethylamine (95:5:0.3:0.05).

[0035] Diluent: ethanol (chromatographic grade). System suitability test: Take 20mg of medetomidine reference substance, put it in a 50ml measuring bottle, add ethanol and ultrasonically treat it to dissolve and dilute to the mark, shake well, take 2ml precisely, put it in a 10ml measuring bottle, add ethanol to dilute to the mark, Shake well as a pre-test solution. Take 20 μl of the pretest solution and inject it into the liquid chromatograph, and record the chromatogram. The main peaks are dexmedetomidine and levmedetomidine in sequence, and the separation degree of dexmedetomidine and levmedetomidine...

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Abstract

The invention belongs to the technical field of drug detection, and particularly relates to a method for detecting isomers in a dexmedetomidine hydrochloride crude product. The detection method includes the specific step of conducting detection by high performance liquid chromatography, wherein a chromatographic column refers to a chiral column chromatography column or an N-lycopodine oxide M bonded silica gel column, flow velocity is 0.2-2.0 ml / min, detection wavelength is 180-380nm, column temperature is 0-40 DEG C, and mobile phase is n-hexane-ethyl alcohol-organic acid and / or organic base. Compared with the prior art, the method for detecting the isomers in the dexmedetomidine hydrochloride crude product has good specificity and high accuracy, a main peak and the isomers can be effectively separated, the isomers in the dexmedetomidine hydrochloride crude product can thus be accurately detected, and quality control of the product and establishment of a unified standard are well promoted.

Description

technical field [0001] The invention belongs to the technical field of drug detection, and in particular relates to a method for detecting isomers in crude dexmedetomidine hydrochloride. Background technique [0002] Dexmedetomidine hydrochloride is a brand-new α2-adrenergic receptor agonist with a strong sedative effect, which is 8 times that of clonidine. It mainly acts on the adrenergic receptors of the pons, medulla oblongata, and blue spots of the brainstem. It has anti-sympathetic effects, a half-life of 2.3 hours, a strong sedative effect and other anesthesia auxiliary effects. It is mainly suitable for the sedation of patients who are initially intubated and using a ventilator during intensive care treatment. It can be used continuously before, during and after extubation in mechanically ventilated patients, and there is no need to stop the drug before extubation; it can also be used for non-intubation Administer patient sedation before and / or during surgery and oth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 张宇丽杜爽孙品张静袁洪雨
Owner CISEN PHARMA
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