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
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[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...
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[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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