Objective: To develop a method for determination of 4-hydrazine benzoic acid content in deferasirox by acetone solution derivatization-HPLC. Methods: 4-hydrazine benzoic acid was derivatized by acetone solution [phosphoric acid-acetone-water(25∶100∶900)].The analysis was carried out on a Symmetry Shield C18(150 mm×4.6 mm,3.5 μm)column, mobile phase A: phosphoric acid-acetonitrile-water (2∶100∶900),mobile phase B: phosphoric acid-water-acetone (2∶100∶900). The flow rate was 1.0 mL·min-1 in a gradient mode. The detection wavelength was 316 nm. The column temperature was set at 40 ℃ and the injection volume was 25 μL. Results: The limit of quantitation was 15.5 ng·mL-1. The limit of detection was 7.7 ng·mL-1. The linear range was 15.7-785.7 ng·mL-1(r2=0.999 7). Average recoveries were 95.2%(RSD=4.8%, n=9). The RSD for repeatability of six samples was 4.8%.The RSD for intermediate precision of twelve samples was 4.4%. When the chromatographic conditions were changed slightly, The RSD of 4-hydrazine benzoic acid content was 3.8%. Conclusions: The established method has high accuracy and specificity. It can be used for quality control of deferasirox crude drug.
YU Xiao-yan, XIE Chun-wen, WU Xiao-dong, WANG Hong-jie, SHA Sha, LI Liang-Liang, CAO Huan-ying
. Determination of 4-hydrazine benzoic acid content in deferasirox by acetone solution derivatization-HPLC[J]. Chinese Journal of Pharmaceutical Analysis, 2021
, 41(12)
: 2102
-2106
.
DOI: 10.16155/j.0254-1793.2021.12.08
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