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Method for detecting related substances of dexmedetomidine hydrochloride raw material or preparation

A technology for dexmedetomidine hydrochloride and related substances, which is applied in the field of detection of related substances of dexmedetomidine hydrochloride raw materials or preparations, can solve the problems of low specificity, low sensitivity, and unsatisfactory, and achieve specificity Strong, high-sensitivity, time-shortened effect

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

AI Technical Summary

Problems solved by technology

But above-mentioned method specificity is not strong, and sensitivity is low, can't satisfy the various preparations of dexmedetomidine hydrochloride

Method used

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  • Method for detecting related substances of dexmedetomidine hydrochloride raw material or preparation
  • Method for detecting related substances of dexmedetomidine hydrochloride raw material or preparation
  • Method for detecting related substances of dexmedetomidine hydrochloride raw material or preparation

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Instruments and conditions: Agilent 1260 liquid chromatography system, DAD detector, chromatographic column: Waters C18 (250×4.6mm, 5μm); detection wavelength: 220nm; phosphate buffer as mobile phase A, acetonitrile as mobile phase B, Gradient elution was carried out according to Table 1.

[0022] Table 1 Concentration gradient of mobile phase

[0023]

[0024] experiment procedure:

[0025] 1. System suitability test: take about 10 mg of dexmedetomidine hydrochloride raw material, put it in a 10 ml measuring bottle, add 1 ml of 6% hydrogen peroxide, heat in an oven at 60° C. for 30 minutes, and use acetonitrile-phosphate buffer (1:1 ) diluted to the mark, shake well, as the system suitability test solution, accurately measure 10 μ l into the liquid chromatograph, record the chromatogram, see the attached HPLC figure 1 .

[0026] Depend on figure 1 It can be seen that the retention time of the main peak of dexmedetomidine hydrochloride is 8.5 minutes, and the s...

Embodiment 2

[0040] Instruments and conditions: Agilent 1260 liquid chromatography system, DAD detector, chromatographic column: Welch Materials C8 (150×4.6mm, 5μm); detection wavelength: 220nm; phosphate buffer as mobile phase A, acetonitrile as mobile phase B, Gradient elution was carried out according to Table 2.

[0041] Table 2 Concentration gradient of mobile phase

[0042]

[0043] Experimental procedure: get about 10mg of dexmedetomidine hydrochloride raw material, put in 10ml measuring bottle, add 6% dioxygen phosphate buffer 1ml, heat in 60 ℃ oven for 30 minutes, with acetonitrile-phosphate buffer (8: 2) Dilute to the mark, shake well, and as a system suitability test solution, accurately measure 10 μl and inject it into a liquid chromatograph, and measure according to the law.

[0044] From the test results, it can be seen that the detection method of the present invention can separate dexmedetomidine hydrochloride from its most difficult oxidative degradation product, while...

Embodiment 3

[0046] Instruments and conditions: Agilent 1260 liquid chromatography system, DAD detector, chromatographic column: N-lycopine M bonded silica gel column (250×4.6mm, 5μm); detection wavelength: 220nm; phosphate buffer as mobile phase A. Acetonitrile is the mobile phase B, and gradient elution is carried out according to Table 3.

[0047] Table 3 Concentration Gradient of Mobile Phase

[0048]

[0049] Experimental procedure: get about 10mg of dexmedetomidine hydrochloride raw material, put in 10ml measuring bottle, add 6% dioxygen phosphate buffer 1ml, heat in 60 ℃ oven for 30 minutes, with acetonitrile-phosphate buffer (9.5: 0.5) Dilute to the mark, shake well, and as a system suitability test solution, accurately measure 10 μl and inject it into a liquid chromatograph, and measure according to the law.

[0050] 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 t...

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Abstract

The invention belongs to the technical field of medicine detection, and in particular relates to a method for detecting related substances of a dexmedetomidine hydrochloride raw material or a preparation. The method specifically comprises the following steps: detecting by using a high performance liquid chromatography method, and performing gradient mobile phase elution, wherein the detection wavelength is 220nm; a 50-95% acetonitrile phosphate buffer solution is adopted as a sample solvent; octyl bonded silica gel, octadecyl bonded silica gel or N-oxidized lycopodine M bonded silica gel is adopted as a chromatographic column of packing; a phosphate buffer solution and acetonitrile are adopted as mobile phases; and the phosphate buffer solution is prepared by dissolving 2.64g of diammonium hydrogen phosphate with water, diluting to be 1000ml, and adjusting the pH value to be 7.3 by using phosphoric acid. Compared with the prior art, the detection method provided by the invention is capable of well separating dexmedetomidine hydrochloride from other inert matters, is capable of accurately testing the contents of other impurities, and has the characteristics of being accurate and reliable in result and good in specificity.

Description

technical field [0001] The invention belongs to the technical field of drug detection, and in particular relates to a method for detecting related substances of dexmedetomidine hydrochloride raw materials or preparations. 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 b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 范峰卢秀莲袁洪雨姜瑞玲张小龙
Owner CISEN PHARMA
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