Detection method for related substances in 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 in dexmedetomidine hydrochloride raw materials or preparations, can solve the problems of low sensitivity of detection results, incomplete dissolution, uneven mixing, etc., and achieve High sensitivity, good resolution, and improved accuracy

Inactive Publication Date: 2019-04-05
石药银湖制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Both of the above two patented technologies use a single mobile phase of organic phase and aqueous phase to mix directly. Due to the difference in polarity, the dissolution is not complete and the mixing is uneven, which makes the noise too large, resulting in low sensitivity of the detection results

Method used

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  • Detection method for related substances in dexmedetomidine hydrochloride raw material or preparation
  • Detection method for related substances in dexmedetomidine hydrochloride raw material or preparation
  • Detection method for related substances in dexmedetomidine hydrochloride raw material or preparation

Examples

Experimental program
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Effect test

Embodiment 1

[0049] Such as Figure 1-7 , the dexmedetomidine hydrochloride reference substance solution, the impurity positioning solution (C, D, E, F, G) of each dexmedetomidine hydrochloride and the mixed solution of dexmedetomidine hydrochloride and each impurity are detected respectively, The dexmedetomidine hydrochloride to be detected was left to stand in a storage bottle full of nitrogen at a temperature of 36°C for 30min, and then detected by high performance liquid chromatography, all using the same liquid chromatography conditions: using ten Octalkylsilane bonded silica gel is used as filler; acetonitrile-phosphate buffer (take 0.02mol / L potassium dihydrogen phosphate, adjust pH to 6.9 with triethylamine) as (20:80, V / V) flow Phase A, acetonitrile is the mobile phase B, the detection wavelength is 220nm, the column temperature is 35°C, the flow rate is 1ml / min, the inner diameter of the packed column is 3.9mm, and the column length is 20cm. A trapping column is installed in fron...

Embodiment 2

[0056] Such as Figure 8 As shown, the method of the United States Pharmacopoeia USP40 is used to detect the related substances of dexmedetomidine hydrochloride raw materials or preparations, and high performance liquid chromatography is adopted. The liquid chromatography conditions: use octadecylsilane bonded silica gel as filler, Use phosphate buffer (0.89g / L disodium hydrogen phosphate about 900ml, adjust pH to 7.0 with 16g / L sodium dihydrogen phosphate, dilute to 1000ml)-methanol=40:60 as mobile phase, detection wavelength 220nm, column temperature The temperature is 30°C, and the flow rate is 1.0ml / min. The inner diameter of the packed column is 4.6mm, and the column length is 10cm.

[0057] For the chromatogram results, see Figure 8 . As can be clearly seen in the figure, the main peak (10.568min) and the adjacent impurity peak (11.465min) are not separated in the test product on the abscissa, and there are obvious inclusions of impurities, and the resolution of this...

Embodiment 3

[0063] Such as Figure 11 As shown, adopt literature method to detect related substances of dexmedetomidine hydrochloride raw material or preparation, adopt high performance liquid chromatography, liquid chromatography condition: use octadecylsilane bonded silica gel as filler, with 0.03mol / L phosphate buffer (weigh 4.08g of potassium dihydrogen phosphate, add 1000ml of water to dissolve, add 2ml of triethylamine): acetonitrile (80:20) is mobile phase A, phosphate buffer: acetonitrile (20:80 ) is the mobile phase B, the detection wavelength is 220nm, the column temperature is 35°C, and the flow rate is 1.0ml / min. Carry out gradient elution (V / V) according to the following table:

[0064]

[0065] For the chromatogram results, see Figure 11 . This method detects that the sample is a destroyed sample, so there are many impurity peaks in the chromatographic column. Figure 11 It can be seen that the impurity peak resolution is not as good as the present invention. Moreo...

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Abstract

The invention relates to the technical field of drug detection and particularly relates to a detection method for related substances in a dexmedetomidine hydrochloride raw material or preparation. According to the method, dexmedetomidine hydrochloride and other inactive substances can be separated well and content of impurities can be accurately measured. According to the detection method providedby the invention, good propulsion effect for uniform establishment of quality control and standard of a product can be provided. According to the method, a high-performance liquid chromatography is employed; a detection wavelength is 215-220nm; a column temperature is 30-40 degrees centigrade; octadecyl silane bonded silica gel is taken as filler; acetonitrile-phosphate buffer is taken as mobilephase A; acetonitrile is taken as mobile phase B; trapping small columns are mounted between a gradient mixer and a sample injector; and gradient elution is carried out according to parameters set bythe method. According to the method, through adoption of the specific mobile phases and gradient elution parameters, the problem that the prior art is poor in separation degree and chromatographic column tolerance and high in cost is avoided.

Description

technical field [0001] The invention relates to the technical field of drug detection, in particular to a method for detecting related substances in dexmedetomidine hydrochloride raw materials or preparations. Background technique [0002] Dexmedetomidine hydrochloride is a highly selective alpha 2 Receptor agonist has sedative hypnotic and anti-anxiety effects, and also has analgesic and sympathetic block effects. It is an effective sedative, analgesic and anesthesia auxiliary drug. Provides a unique type of sedation, that is, "sedation with preserved consciousness", which can reduce the amount of anesthesia and analgesic drugs during the operation, effectively suppress the stress state during the perianesthesia period, improve the patient's hemodynamics, and have no obvious respiratory depression, It can also prevent postoperative nausea and vomiting and chills, and has potential benefits for neurological, cardiac and renal protection. Dexmedetomidine hydrochloride was f...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 蔡磊王振国狄彩霞郭良于春杨姚春虎高凯丽
Owner 石药银湖制药有限公司
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