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A method for detecting 4-(1-(2,5-dimethylphenyl)ethyl)-1h-imidazole or/and its hydrochloride

A dimethyl phenyl, detection method technology, applied in the detection field, to achieve the effect of meeting the requirements of impurity control, good durability and high sensitivity

Active Publication Date: 2021-03-23
CHENGDU BRILLIANT PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The main difficulty is that the structure of dexmedetomidine hydrochloride contains a "dimethylphenyl" group. Due to the substitution of the benzene ring, there are multiple reaction sites, so it may contain the methyl isomer impurity 4- (1-(2,5-Dimethylphenyl)ethyl)-1H-imidazole (Formula I), its hydrochloride is similar to dexmedetomidine hydrochloride in structure, in USP dexmedetomidine hydrochloride Under the related substance analysis method, this compound and dexmedetomidine (formula II) peak overlap completely

Method used

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  • A method for detecting 4-(1-(2,5-dimethylphenyl)ethyl)-1h-imidazole or/and its hydrochloride
  • A method for detecting 4-(1-(2,5-dimethylphenyl)ethyl)-1h-imidazole or/and its hydrochloride
  • A method for detecting 4-(1-(2,5-dimethylphenyl)ethyl)-1h-imidazole or/and its hydrochloride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Blank solvent (the following is used as diluent): phosphate buffer-methanol (60:40, v / v), water or acetonitrile-water (3:7, v / v).

[0068] Get the finished product of dexmedetomidine, add corresponding diluent to dissolve and make a solution containing about 0.5mg of dexmedetomidine in every 1ml, as need testing solution; precision measures appropriate amount of need testing solution, dilute with corresponding The solution was diluted to make a solution containing about 1 μg of dexmedetomidine per 1 ml, as a control solution. Accurately weigh appropriate amounts of dexmedetomidine hydrochloride and YM-Z6 reference substance, dissolve with corresponding diluents and make solutions containing about 0.5 mg of dexmedetomidine and about 0.5 μg of YM-Z6 in each 1 ml, as System Suitability Solution.

[0069] Measured according to high-performance liquid chromatography (Chinese Pharmacopoeia 2015 Edition Four General Rules 0512), accurately measure 20 μl of the system suitabil...

Embodiment 2

[0070] Embodiment 2 Screening of detection wavelength

[0071] The ultraviolet absorption spectrum of impurity YM-Z6 is shown in figure 1 , the UV absorption spectrum of the main peak dexmedetomidine is shown in figure 2 .

[0072] It can be seen from the scanning spectrum that the ultraviolet absorption of the main component and impurity YM-Z6 is terminal absorption, and the detection wavelength is set at 220nm with reference to the detection wavelength of the USP related substance method.

Embodiment 3

[0073] The screening of embodiment 3 chromatographic conditions

[0074] (1) Refer to the chromatographic conditions of the related substance method of dexmedetomidine hydrochloride USP standard (USP40s1):

[0075] Mobile phase: phosphate buffer (weigh 0.71 g of disodium hydrogen phosphate and dissolve in 1 L of water, adjust the pH value to 7.0 with 16 g / L sodium dihydrogen phosphate dihydrate)-methanol (40:60);

[0076] Chromatographic column: Agilent InfinityLabPoroshell 120EC-C18, 4.6×150mm, 4μm;

[0077] Flow rate: 1ml / min, detection wavelength: 220nm;

[0078] Column temperature: 25°C, injection volume: 100μl;

[0079] Diluent: Phosphate Buffer-Methanol (60:40).

[0080] Depend on image 3 It can be seen that YM-Z6 overlaps with the main peak under this method, indicating that YM-Z6 and dexmedetomidine cannot be separated under this method.

[0081] (2) Referring to the related substance method of dexmedetomidine hydrochloride USP standard (USP40s1), replace differe...

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Abstract

The invention discloses a method for detecting 4-(1-(2,5-dimethyl phenyl)ethyl)-1H-imidazole or / and a hydrochloride thereof from medetomidine or dexmedetomidine hydroch; HPLC (High Performance LiquidChromatography) method is used for qualitative or / and quantitative detection of the 4-(1-(2,5-dimethyl phenyl)ethyl)-1H-imidazole or / and the hydrochloride thereof, and detection conditions of LC (Liquid Chromatogram) include: chromatographic column: C18 chromatographic column, mobile phase includes an aqueous phase and an organic phase, wherein the aqueous phase is a phosphate buffer; the organicphase is a methanol or / and acetonitrile solution, and the organic phase is selected from methanol or / and acetonitrile; the mobile phase is eluted by isocratic elution method; the method of the invention can effectively detect 4-(1-(2,5-dimethyl phenyl)ethyl)-1H-imidazole or / and the hydrochloride thereof in the bulk pharmaceutical chemical, capable of indicating specificity and stability.

Description

technical field [0001] The invention relates to the field of detection methods, in particular to a method for detecting impurities in medicines. Background technique [0002] Dexmedetomidine hydrochloride is an α2-adrenergic receptor agonist with anti-sympathetic, sedative and analgesic effects. It is used for sedation during tracheal intubation and mechanical ventilation in patients undergoing general anesthesia. [0003] More than 5 years of clinical experience in the United States have shown that dexmedetomidine hydrochloride can produce stable sedative and awakening effects, and has a unique synergistic effect on the physical and psychological needs of critically ill patients, which can significantly reduce the time required for induction of anesthesia. The amount of anesthesia; giving this product before surgery can reduce the amount of opioid or non-opioid analgesics before and after surgery, which is of great significance for anesthesia and intensive care; it can also...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/54
CPCG01N30/02G01N30/06G01N30/54G01N2030/027G01N2030/062
Inventor 李耀成宜娟罗鸣李英富苏忠海
Owner CHENGDU BRILLIANT PHARMA CO LTD
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