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

A technology of dexmedetomidine hydrochloride and related substances, which is applied in the field of drug analysis, can solve problems such as long gradient elution time, complicated mobile phase preparation, poor chromatographic column tolerance, etc., and achieve excellent chromatograms, quality control and improvement Good and convenient comparison effect

Active Publication Date: 2021-05-14
广州艾格生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In summary, there are the following problems, such as complex mobile phase preparation, long gradient elution time, low efficiency, low sensitivity, or poor chromatographic column tolerance

Method used

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

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] Using the USP43 related substance detection method in the background technology, the 5 impurity positioning solutions listed in USP43 and the impurities and impurity mixed solutions that may be produced according to the synthesis process route were injected into samples for detection. Adopt Merck Lichrospher100RP-18 (4mm * 12.5cm, 5 μm) chromatographic column, with 0.89g / L disodium hydrogen phosphate dihydrate (dissolve disodium hydrogen phosphate dihydrate with 90% water of the preparation amount, use 16g / L disodium hydrogen phosphate Adjust the pH to 7.0 with sodium dihydrogen phosphate hydrate, and then dilute to the mark with water)-methanol (40:60) as the mobile phase; the wavelength is 220nm; the column temperature is 30°C, and the flow rate is 1.0ml per minute.

[0075] The test results are shown in Table 1, and the spectrum is attached figure 1 and figure 2 .

[0076] Table 1

[0077]

[0078] figure 1 It can be seen from Table 1 that among the five impu...

Embodiment 2

[0080] Using the detection method of the present invention, the 5 impurity positioning solutions listed in USP43 and the impurities and impurity mixed solutions that may be produced according to the synthesis process route are respectively injected for detection. Instrument and conditions: Shimadzu LC-20AT UV liquid chromatography system, chromatographic column: Agilent Eclipse plus C18 (4.6×150mm, 3.5μm); detection wavelength is 220nm; column temperature is 30°C; flow rate is 1.0ml / min; The disodium hydrogen phosphate dihydrate of 10mmol / L is the mobile phase A, and acetonitrile is the mobile phase B, and the gradient elution is carried out in the following table 2:

[0081] Table 2

[0082] time (min) Mobile phase A(%) Mobile phase B(%) 0 80 20 20 60 40 30 35 65 35 35 65 35.01 80 80 45 80 20

[0083] The results are shown in Table 3 and attached image 3 .

[0084] table 3

[0085]

[0086] From Table 3 and image...

Embodiment 3

[0088] Instrument and conditions: Shimadzu LC-20AT UV liquid chromatography system, chromatographic column: Agilent Eclipse plus C18 (4.6×150mm, 3.5μm); detection wavelength is 220nm; 10mmol / L disodium hydrogen phosphate dihydrate as mobile phase A, Acetonitrile is the mobile phase B, the column temperature is 30°C; the flow rate is 1.0ml / min, and the gradient elution is carried out in the following table 4:

[0089] Table 4

[0090] time (min) Mobile phase A(%) Mobile phase B(%) 0 80 20 20 60 40 30 35 65 35 35 65 35.01 80 80 45 80 20

[0091] Test sample: take an appropriate amount of raw material, add water to dissolve and dilute to make a solution containing dexmedetomidine 0.1mg / ml, as the raw material for the test solution; precisely measure 50ul of the solution and blank solvent, and inject into the liquid chromatograph. see results Figure 4 and Figure 5 .

[0092] Figure 4 and Figure 5 It can be seen that w...

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Abstract

The invention discloses a method for detecting related substances in a dexmedetomidine hydrochloride raw material or preparation; the method comprises the following steps: using high performance liquid chromatography for detection, a mobile phase being composed of a mobile phase A and a mobile phase B, the mobile phase A being a phosphate buffer solution with a pH value of 7.3-7.7, the mobile phase B being acetonitrile, and the concentration of phosphate in the phosphate buffer solution being 8 mmol / L to 12 mmol / L; and using gradient mobile phase elution. The mobile phase system is matched with proper gradient elution conditions, 13 related impurities in starting materials, intermediates, side reaction products and dexmedetomidine hydrochloride degradation products brought in the preparation process of dexmedetomidine hydrochloride raw materials or preparations can be detected, the impurities are better separated, and the accuracy of detection results is improved.

Description

technical field [0001] The invention relates to the technical field of drug analysis technology, in particular to a method for detecting related substances in dexmedetomidine hydrochloride raw materials or preparations. Background technique [0002] Dexmedetomidine hydrochloride is a new type of highly selective α2-adrenergic receptor agonist, which is the dextroisomer of medetomidine. Compared with medetomidine, this product has a greater effect on the central α2-adrenergic The selectivity of hormone receptor agonism is stronger, and the half-life is short, and the dosage is small. Dexmedetomidine has sedative and anti-anxiety effects, and is clinically suitable for sedation of intubated and ventilated patients during intensive care treatment. In addition, it also has analgesic effects and anti-sympathetic inhibition of perioperative stress responses. Reduce the dosage of anesthetic drugs and maintain the stability of hemodynamics. Dexmedetomidine Hydrochloride Injection ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/36G01N30/74G01N30/86
CPCG01N30/02G01N30/06G01N30/34G01N30/36G01N30/74G01N30/8679
Inventor 汤文星贺珊珊张现涛何盛江谭斌吴沛桃
Owner 广州艾格生物科技有限公司
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