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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  • 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 pol

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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Example Embodiment

[0048] Example 1,

[0049] Such as Figure 1-7 , Dexmedetomidine hydrochloride reference solution, each dexmedetomidine hydrochloride impurity positioning solution (C, D, E, F, G) and the solution after mixing dexmedetomidine hydrochloride with each impurity are tested separately, The dexmedetomidine hydrochloride to be tested was allowed to stand for 30 minutes in a storage bottle filled with nitrogen at a temperature of 36°C, and then tested by high performance liquid chromatography, all using the same liquid chromatography conditions: Octaalkylsilane-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 mobile phase B, detection wavelength is 220nm, column temperature is 35°C, flow rate is 1ml / min, packed column inner diameter is 3.9mm, column length is 20cm, and a trapping column is installed before the injector. The said trapping c...

Example Embodiment

[0055] Example 2,

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

[0057] See the chromatogram result Figure 8 . It can be clearly seen in the figure that the main peak (10.568min) and the adjacent impurity peak (11.465min) in the test product on the abscissa are not separated, and there is an obvious phenomenon of inclusion of impurities, and the resoluti...

Example Embodiment

[0062] Example 3.

[0063] Such as Picture 11 As shown, the literature method is used to detect dexmedetomidine hydrochloride raw materials or related substances in preparations, using high performance liquid chromatography, liquid chromatography conditions: octadecyl silane-bonded silica gel is used as filler, with 0.03 mol / L Phosphate buffer (weigh 4.08g of potassium dihydrogen phosphate, add 1000ml of water to dissolve, add 2ml of triethylamine): acetonitrile (80:20) as mobile phase A, phosphate buffer: acetonitrile (20:80) ) Is mobile phase B, detection wavelength is 220nm, column temperature is 35°C, flow rate is 1.0ml / min. Perform gradient elution (V / V) according to the following table:

[0064]

[0065] See the chromatogram result Picture 11 . The sample detected by this method is a sample that has been destroyed, so there are many impurity peaks in the chromatographic column. Picture 11 It can be seen that the impurity peak resolution is not as good as the present inv...

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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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