| abstract |
The invention discloses a quantitative determination method for genotoxic impurities in calcium dobesilate. The invention firstly uses an acidic acetonitrile solution to prepare a derivatization reagent, which can ensure that calcium dobesilate, 2-sulfonic acid group-1,4 ‑Benzoquinone, hydroquinone and 1,4‑benzoquinone can exist stably, while ensuring that benzoquinone impurities can react completely with the derivatization reagent, and then use acetonitrile aqueous solution to fully dissolve the sample and impurities. For the derivatized sample solution, a chromatographic column with end-capped octadecylsilane-bonded silica gel as a filler, and a mixed solution of buffer solution-acetonitrile with pH 4.5±0.5 as the mobile phase HPLC conditions, To achieve the separation and quantification of p-benzoquinone impurities. The method is easy to operate, has good specificity for the detection of benzoquinone impurities in the sample, high sensitivity, good precision and reproducibility, and can accurately quantitatively analyze two benzoquinone impurities in calcium p-dobesilate, ensuring that hydroxybenzene Safety and quality controllability of calcium benzenesulfonate raw materials and preparations. |