J AOAC Int. 2016 Apr 19. doi: 10.5740/jaoacint.15-0273.
A new chiral reversed-phase (RP)-HPLC method with UV detection was developed. Enantioselective resolution of ibuprofen (IBP) was achieved using (3R,4S)-4-(3,5-dinitrobenzamido)-3-(3-(trioxysilyl)- propyl)-1,2,3,4-tetrahydro-phenanthrene [(R,R)-Whelk-O2] chiral stationary phase (4.6 mm id × 250 mm, 10 μm) with a mobile phase composed of ethanol-water (30 + 70, v/v) containing 100 mM ammonium acetate at a flow rate of 1.3 mL/min using diode array detector at λ 220 nm. Calibration curves were linear over the concentration range of 20-180 μg/mL for both IBP enantiomers. Mean % recoveries ±SD of 99.74 ± 1.73 and 99.60 ± 0.93 were obtained for dexibuprofen (dex-IBP) and levoibuprofen (levo-IBP), respectively. Intra- and interday precision calculated as RSD, % were not more than 1.66% for dex-IBP and 1.93% for levo-IBP. The detection limits were 2.09 and 2.06 μg/mL for dex-IBP and levo-IBP, respectively. The method was successfully applied for the determination of dex-IBP in tablet dosage form.
开发了一种带有紫外检测的新型手性反相（RP）-高效液相色谱法。使用(3R,4S)-4-(3,5-二硝基苯甲酰胺基)-3-(3-(三氧基硅基)-丙基)-1,2,3,4-四氢菲[(R,R)-Whelk-O2]手性固定相（内径4.6 mm×250 mm，10μm），以乙醇-水（30 + 70，v/v）组成的流动相，其中含有100 mM乙酸铵，流速为1.3 mL/min，在220 nm波长下使用二极管阵列检测器，实现了布洛芬（IBP）的对映体拆分。两种IBP对映体在20 - 180μg/mL浓度范围内校准曲线呈线性。右布洛芬（dex-IBP）和左布洛芬（levo-IBP）的平均回收率±标准差分别为99.74±1.73和99.60±0.93。以相对标准偏差（RSD）计算的日内和日间精密度，dex-IBP不超过1.66%，levo-IBP不超过1.93%。dex-IBP和levo-IBP的检测限分别为2.09和2.06μg/mL。该方法成功应用于片剂剂型中dex-IBP的测定。
