Hefnawy Mohammed M, Al-Shehri Mona M, Abounassif Mohammed A, Mostafa Gamal A E
King Saud University, College of Pharmacy, Pharmaceutical Chemistry Department, PO Box 2457, Riyadh 11451, Saudi Arabia.
J AOAC Int. 2013 Sep-Oct;96(5):976-80. doi: 10.5740/jaoacint.11-191.
Enantiomeric resolution of atenolol was achieved on the HPLC vancomycin macrocyclic antibiotic chiral stationary phase Chirobiotic V. The polar ionic mobile phase consisted of methanol-glacial acetic acidtriethylamine (100 + 0.025 + 0.75, v/v/v) at a flow rate of 0.8 mL/min. Fluorescence detection at 2751305 nm for excitation and emission, respectively, was used. Plasma samples were purified using SPE on Oasis HLB cartridges. The calibration curves in plasma were linear over the range of 5-400 ng/mL (r = 0.999) for each enantiomer with an LOD of 1.0 ng/mL. The proposed method was validated in compliance with International Conference of Harmonization guidelines in terms of linearity, accuracy, precision, LOD, LOQ, and selectivity. The overall recoveries for S-(-)- and R-(+)-atenolol enantiomers from plasma were 95.0-99.5%; RSD ranged from 2.5 to 3.3%. The developed method was applied for the trace analysis of atenolol enantiomers in plasma and for the pharmacokinetic investigation of atenolol enantiomers in mouse plasma.
在高效液相色谱法中，使用万古霉素大环抗生素手性固定相Chirobiotic V实现了阿替洛尔的对映体拆分。极性离子流动相由甲醇 - 冰醋酸 - 三乙胺（100 + 0.025 + 0.75，v/v/v）组成，流速为0.8 mL/min。分别在激发波长275 nm和发射波长305 nm处进行荧光检测。血浆样品通过在Oasis HLB柱上的固相萃取进行纯化。每种对映体在血浆中的校准曲线在5 - 400 ng/mL范围内呈线性（r = 0.999），检测限为1.0 ng/mL。所提出的方法在线性、准确度、精密度、检测限、定量限和选择性方面按照国际协调会议指南进行了验证。血浆中S - (-)-和R - (+)-阿替洛尔对映体的总回收率为95.0 - 99.5%；相对标准偏差范围为2. / 5至3.3%。所开发的方法用于血浆中阿替洛尔对映体的痕量分析以及小鼠血浆中阿替洛尔对映体的药代动力学研究。
