Li Bing, Zhou Xu-Zheng, Li Jian-Yong, Yang Ya-Jun, Niu Jian-Rong, Wei Xiao-Juan, Liu Xi-Wang, Li Jin-Shan, Zhang Ji-Yu
Key Laboratory of Veterinary Pharmaceutical Development, Ministry of Agriculture, Lanzhou, China; Key Laboratory of New Animal Drug Project of Gansu Province, Lanzhou, China; Lanzhou Institute of Husbandry and Pharmaceutical Science of CAAS, Lanzhou 730050, China.
Key Laboratory of Veterinary Pharmaceutical Development, Ministry of Agriculture, Lanzhou, China; Key Laboratory of New Animal Drug Project of Gansu Province, Lanzhou, China; Lanzhou Institute of Husbandry and Pharmaceutical Science of CAAS, Lanzhou 730050, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Oct 15;969:12-8. doi: 10.1016/j.jchromb.2014.07.043. Epub 2014 Aug 8.
A rapid and sensitive high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the determination of arecoline concentration in dog plasma. Plasma sample was prepared by protein precipitation using n-hexane (containing 1% isoamyl alcohol) with β-pinene as an internal standard. Chromatographic separation was achieved on an Agilent C18 column (4.6×75mm, 3.5μm) using methanol: 5mM ammonium acetate as the mobile phase with isocratic elution. Mass detection was carried out using positive electrospray ionization in multiple reaction monitoring mode. The calibration curve for arecoline was linear over a concentration range of 2-500ng/mL. The intra-day and inter-day accuracy and precision were within the acceptable limits of ±10% at all concentrations. In summary, the LC-MS/MS method described herein was fully validated and successfully applied to the pharmacokinetic study of arecoline hydrobromide tablets in dogs after oral administration.
建立了一种快速、灵敏的高效液相色谱-串联质谱(LC-MS/MS)方法并进行了验证,用于测定犬血浆中槟榔碱的浓度。血浆样品采用正己烷(含1%异戊醇)与β-蒎烯作为内标进行蛋白沉淀制备。在安捷伦C18柱(4.6×75mm,3.5μm)上,以甲醇:5mM醋酸铵为流动相进行等度洗脱实现色谱分离。采用正电喷雾电离在多反应监测模式下进行质谱检测。槟榔碱的校准曲线在2-500ng/mL的浓度范围内呈线性。日内和日间的准确度和精密度在所有浓度下均在±10%的可接受范围内。总之,本文所述的LC-MS/MS方法经过充分验证,并成功应用于犬口服氢溴酸槟榔碱片后的药代动力学研究。