Tang Chunlan, Wang Li, Cheng Mengchun, Liu Xinxin, Xiao Hongbin
Se Pu. 2015 Jul;33(7):699-703. doi: 10.3724/sp.j.1123.2015.03017.
An ultra performance liquid chromatography-quadrupole time of flight mass spectrometry (UPLC-QTOF-MS) method was developed and validated for the determination of N6-(4-hydroxybenzyl) adenine riboside and its pharmacokinetics in rat plasma. The chromatographic conditions were optimized. The separation was performed on an Agilent ZORBAX SB-C18 column(150 mm x 3 mm, 1.8 μm) with a gradient elution of 0.2% (v/v) formic acid aqueous solution and acetonitrile as the mobile phases at a flow rate of 0.35 mL/min. The detection was accomplished in positive mode with electrospray ionization (ESI) by UPLC-QTOF-MS, and 6-benzylamino purine was used as the internal standard (IS). The results showed that the linear range of calibration curve was 0.625-160 ng/mL for N6-(4-hydroxybenzyl) adenine riboside in rat plasma with the correlation coefficient more than 0.99. The recoveries were 88.41%-108.26%. The limit of detection was 0.1 ng/mL. The intra-day and inter-day precisions (RSDs) were less than 6%, and intra-day and inter-day accuracies (REs, RE = (measured concentration-spiked concentration)/spiked concentration x 100%) were less than ±15%. The method is rapid, sensitive and accurate for the quantitation of N6-(4-hydroxybenzyl) adenine riboside, which can be used for the study of pharmacokinetics of N6-(4-hydroxybenzyl) adenine riboside.
建立了一种超高效液相色谱-四极杆飞行时间质谱(UPLC-QTOF-MS)法,用于测定大鼠血浆中N6-(4-羟基苄基)腺嘌呤核苷及其药代动力学。优化了色谱条件。采用Agilent ZORBAX SB-C18柱(150 mm×3 mm,1.8μm),以0.2%(v/v)甲酸水溶液和乙腈为流动相进行梯度洗脱,流速为0.35 mL/min。通过UPLC-QTOF-MS在正离子模式下采用电喷雾电离(ESI)进行检测,以6-苄氨基嘌呤作为内标(IS)。结果表明,大鼠血浆中N6-(4-羟基苄基)腺嘌呤核苷校准曲线的线性范围为0.625160 ng/mL,相关系数大于0.99。回收率为88.41%108.26%。检测限为0.1 ng/mL。日内和日间精密度(RSD)均小于6%,日内和日间准确度(RE,RE =(测定浓度-加标浓度)/加标浓度×100%)均小于±15%。该方法快速、灵敏、准确,可用于N6-(4-羟基苄基)腺嘌呤核苷的定量分析,适用于N6-(4-羟基苄基)腺嘌呤核苷药代动力学研究。