Detection method used for measuring doxercalciferol and impurities contained by doxercalciferol

Abstract

The invention provides a detection method used for measuring doxercalciferol and impurities contained by doxercalciferol. According to the detection method, high performance liquid chromatography is adopted, and chromatographic conditions are determined as following: globular protein bonded with hydrophilic silicone or octadecyl silane is taken as the stationary phase, a mixed solution composed of an acid solution and an organic solvent is taken as the mobile phase, flow velocity is controlled to be 1.5 to 2.0ml / min, detection wavelength is controlled to be 210nm, column temperature is controlled to be room temperature, sample size is controlled to be 5 to 10<mu>L, sample concentration is controlled to be 3 to 5mg / ml, and the volume ratio of the acid solution to the organic solvent solution in the mixed solution is reduced in a gradient manner with elution progress of high performance liquid chromatography. In the gradient elution process of high performance liquid chromatography, the volume ratio of the acid solution to the organic solvent solution in the mixed solution is reduced in a gradient manner with elution progress of high performance liquid chromatography, so that synchronous separation and detection of doxercalciferol and three impurities contained by doxercalciferol are realized, separation and detection efficiency is increased, and detection time and relative retention time of main peaks are shortened.

Description

technical field [0001] The invention relates to the technical field of chemical detection, in particular to a detection method for measuring calciferol and impurities contained therein. Background technique [0002] Doxercalciferol, also known as 1-A hydroxyvitamin D2, is a vitamin D2 analog that mainly acts on the parathyroid gland, can effectively inhibit the secretion of the whole parathyroid hormone, and increase blood calcium and blood levels to a small extent. Phosphorus concentration, new drugs such as SHPT approved by FDA for patients with osteoporosis, grade 3 to 4 chronic kidney disease. The molecular formula of docecalcidol is: C 28 h 44 o 2 , and its chemical structure is as follows: [0003] [0004] During the synthesis of doxercalciferol, some related impurity substances such as by-products or intermediates or degradation products produced during the production process will be produced. These impurities may affect the purity and quality of the drug due...

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Problems solved by technology

But the detection time of this method is longer, and the relative retention time of main peak is longer, and the impurity response value at 274nm wavelength place is lower, makes the impurity content of measuring than actual low, is unfavorable for the impurity in the docecalcidol raw material control, thus ultimately affecting the clinical therapeutic effect of doxercalciferol preparations

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