Objective: To establish a principal component external standard method with HPLC and calibration factors for the determination of 11 impurities in flurbiprofen axetil injection, and to explore its detection results and limit values. Methods: The Thermo BDS Hypersil C18 (250×4.6 mm, 5 μm) was selected for gradient elution, with water-0.15% acetic acid and acetonitrile-0.15% acetic acid as the mobile phase at a flow rate of 1.0 mL · min-1.The column temperature was 40 ℃, the detection wavelength was 254 nm and the injection volume was 10 μL.Results: Flurbiprofen axetil and 11 impurities were well separated by the method. Good linearity was obtained with correlation coefficients of 1.000 for the 3-fluoro-4-phenylphenol (4-OHB), 1-acetoxyethyl-2-(2-fluoro-4-biphenylyl)-2-hydroxypropionate (2-OHP), 4-acetyl-2-fluorobiphenyl (4-ACB), flurbiprofen ethyl ester, allyl - (2-fluoro-4-biphenyl) propionate (ALE), ChP impurity Ⅰ, impurity B, impurity C and impurity E in the range of 0.10-20 μg · mL-1. The average recovery rates was from 96.6% to 103.7% and the relative standard deviations (RSDs) were lower than 1.4%. The correction factors of flurbiprofen axetil related substances 4-OHB, 2-OHP, 4-ACB, flurbiprofen, flurbiprofen ethyl ester, ALE, ChP impurity Ⅰ, impurity B, impurity C and impurity E were 0.55, 1.05, 1.01, 0.76, 0.95, 0.86, 0.55, 0.93, 0.76 and 0.81, respectively. Notablely, desfluoro fiurbiprofen axetil of detected was around the prescribed limit 0.1%. Conclusion: The method above is rapid, simple, accurate, and reliable, and can be applied for the determination and quality control of related substances in flurbiprofen axetil injection.
WANG Xue
,
ZHANG Xiao-han
,
LI Tie-jun
,
LI Wen-xin
,
LI Lin
,
YANG Shu-juan
,
ZHANG Lian-yi
,
DOU Yan-li
,
GUO Chang-chuan
,
XU Yu-wen
. Determination of 11 related substances in flurbiprofen axetil injection by HPLC*[J]. Chinese Journal of Pharmaceutical Analysis, 2025
, 45(2)
: 246
-253
.
DOI: 10.16155/j.0254-1793.2024-0489
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