Validation and implementation of a method for determination of bryostatin 1 in human plasma by using liquid chromatography/tandem mass spectrometry.
Validation and implementation of a method for determination of bryostatin 1 in human plasma by using liquid chromatography/tandem mass spectrometry.
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使用液相色谱/串联质谱法测定人血浆中苔藓抑素 1 的方法的验证和实施。
DOI：
10.1016/j.ab.2004.10.030
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发表时间：
2005
期刊：
影响因子：
--
通讯作者：
Baker,SharynD
中科院分区：
文献类型：
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作者：
Zhao,Ming;Rudek,MichelleA;He,Ping;Smith,BDouglas;Baker,SharynD
建立了一种新的检测苔藓抑素1的液相色谱-串联质谱法。样品前处理包括用乙腈/正丁基氯（1/4，v/v）混合物进行双液-液萃取步骤。在沃茨X-Terra C18（50× 2.1 mm i.d.，3.5μm）分析柱，乙腈/水移动的流动相（80：20，v/v），含0.1%甲酸，等度流速为0.15 mL/min，持续13 min。感兴趣的分析物通过串联质谱与电喷雾正离子化进行监测。在50- 2000 pg/mL范围内生成线性校准曲线，决定系数值>0.99。日内和日间精密度和准确度均<15%。该方法用于表征剂量为20μg/m2的苔藓抑素1的血浆药代动力学，以优化该药剂的治疗。
A new sensitive and specific method using liquid chromatography/tandem mass spectrometry for determination of bryostatin 1 was developed and validated. Sample pretreatment involved a double liquid–liquid extraction step with a mixture of acetonitrile/n-butyl chloride (1/4, v/v). Separation of the compound of interest, including the internal standard paclitaxel, was achieved on a Waters X-Terra C18(50×2.1mm i.d., 3.5μm) analytical column with acetonitrile/water mobile phase (80:20, v/v) containing 0.1% formic acid using isocratic flow at 0.15mL/min for 13min. The analytes of interest were monitored by tandem mass spectrometry with electrospray positive ionization. The linear calibration curves were generated over the range of 50–2000pg/mL with values for the coefficient of determination of >0.99. The values for both within-day and between-day precision and accuracy were <15%. This method was used to characterize the plasma pharmacokinetics of bryostatin 1 at doses of 20μg/m2to optimize treatment with this agent.