Li Chao, Yang Chunjuan, Peng Xuling, Xiong Zhili, Li Famei
Department of Analytical Chemistry, Shenyang Pharmaceutical University, Shenyang, 110016, PR China.
J Chromatogr Sci. 2010 May-Jun;48(5):342-7. doi: 10.1093/chromsci/48.5.342.
A sensitive, specific method has been developed for simultaneous determination of neoeriocitrin and naringin in rat plasma using liquid chromatography-tandem mass spectrometry. With hesperidin as the internal standard, plasma samples were prepared by protein precipitation with methanol. Analysis was carried out on an ACQUITY UPLC BEH C(18) column using acetonitrile-water (20:80, v/v) as the mobile phase. Detection was performed by means of electrospray ionization mass spectrometry in negative ion mode with multiple reaction monitoring. Linear calibration curves of neoeriocitrin and naringin were obtained over the concentration ranges of 15.0-960 ng/mL and 12.0-1200 ng/mL, respectively. The intra- and inter-day precisions were within 9.7% and 7.6% for neoeriocitrin and 7.8% and 12.9% for naringin. The accuracy was from -4.3% to 0.43% for neoeriocitrin and from -3.8% to 3.0% for naringin. The validated method was successfully applied to the pharmacokinetic study of neoeriocitrin and naringin in rats after oral administration of a Chinese compound formulation, gushudan.
已开发出一种灵敏、特异的方法，采用液相色谱 - 串联质谱法同时测定大鼠血浆中的新橙皮苷和柚皮苷。以橙皮苷为内标，血浆样品通过甲醇蛋白沉淀法制备。分析在ACQUITY UPLC BEH C(18)柱上进行，以乙腈 - 水（20:80，v/v）作为流动相。采用电喷雾电离质谱在负离子模式下进行多反应监测检测。新橙皮苷和柚皮苷的线性校准曲线分别在15.0 - 960 ng/mL和12.0 - 1200 ng/mL的浓度范围内获得。新橙皮苷的日内和日间精密度分别在9.7%和7.6%以内，柚皮苷的日内和日间精密度分别在7.8%和12.9%以内。新橙皮苷的准确度在 - 4.3%至0.43%之间，柚皮苷的准确度在 - 3.8%至3.0%之间。该验证方法成功应用于大鼠口服中药复方制剂骨疏丹后新橙皮苷和柚皮苷的药代动力学研究。
