超高效液相色谱-四极杆飞行时间质谱法测定大鼠血浆中的N~6-羟苄腺苷

发布时间：2018-01-22 07:02

本文关键词： 超高效液相色谱-四极杆飞行时间质谱 N-羟苄腺苷药代动力学大鼠血浆　出处：《色谱》2015年07期 　论文类型：期刊论文

【摘要】：建立了测定大鼠血浆中N6-羟苄腺苷的超高效液相色谱-四极杆飞行时间质谱(UPLC-QTOF-MS)分析方法,并应用于N6-羟苄腺苷药代动力学研究。采用Agilent ZORBAX SB-C18色谱柱(150 mm×3 mm,1.8μm)对目标物分离,以0.2%(v/v)甲酸水溶液和乙腈为流动相进行梯度洗脱;以6-苄氨基嘌呤作为内标,在电喷雾离子源正离子模式下进行定量分析。结果表明:N6-羟苄腺苷在0.625~160 ng/mL的范围内线性关系良好(r0.99);方法的回收率在88.41%~108.26%之间;检出限达到0.1 ng/mL;日内和日间准确度(以RE计,RE=(测定浓度-加标浓度)/加标浓度×100%)均在±15%之内,精密度(以RSD计)均小于6%。该方法选择性好,灵敏度高,重现性好,结果准确,可用于N6-羟苄腺苷的血药浓度监测及药代动力学研究。
[Abstract]:A high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS) method for the determination of N6-hydroxybenzyl adenosine in rat plasma was established. The pharmacokinetics of N6-hydroxybenzyl adenosine was studied with Agilent ZORBAX SB-C18 column (150mm 脳 3mm). 1.8 渭 m) the target was separated and gradient elution was carried out with 0.2% v / v) formic acid aqueous solution and acetonitrile as mobile phase. 6-benzyl aminopurine was used as internal standard. The quantitative analysis was carried out under the positive ion mode of electrospray ion source. The results showed that the linear range of the concentration of 1: N6-hydroxybenzyl adenosine was 0.625 ~ (160) ng/mL, and the linear relationship was good in the range of 0.625 ~ (160) ng/mL. The recovery of the method was between 88.41% and 108.26%. The detection limit was 0.1 ng / mL; Both intraday and inter-day accuracy (measured by RE) were within 卤15%. The precision (in terms of RSD) is less than 6. The method has good selectivity, high sensitivity, good reproducibility and accurate results. It can be used to monitor the blood concentration of N6-hydroxybenzyl adenosine and to study its pharmacokinetics.
【作者单位】：中国科学院大连化学物理研究所中国科学院分离分析化学重点实验室;中国科学院大学;
【基金】：国家自然科学基金项目(81001629) 重大新药创制专项课题(2014XZ09304-307)
【分类号】：R927.2;O657.63
【正文快照】： 天麻是一种名贵的中药,主治头痛眩晕、肢体麻木、癫痫抽搐等症[1]。现代药理证实天麻有明显的神经保护作用[2,3],且神经保护作用对于脑卒中、癫痫等多种脑血管疾病有治疗意义[4]。目前,从天麻中已经分离得到60多种化合物[5-7],但是对天麻神经保护物质基础的认识仍局限于已知活

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