A rapid and sensitive LC-MS/MS method for the determination of linarin in small-volume rat plasma and tissue samples and its application to pharmacokinetic and tissue distribution study
A rapid and sensitive LC-MS/MS method for the determination of linarin in small-volume rat plasma and tissue samples and its application to pharmacokinetic and tissue distribution study
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一种快速、灵敏的 LC-MS/MS 方法，用于测定小体积大鼠血浆和组织样品中的里那林及其在药代动力学和组织分布研究中的应用。
DOI：
10.1002/bmc.3605
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发表时间：
2016-04-01
影响因子：
1.8
通讯作者：
Di, Xin
中科院分区：
文献类型：
--
作者：
Feng, Xinchi;Liu, Youping;Di, Xin
建立了一种快速、灵敏的LC-MS/MS测定小体积大鼠血浆和组织样品中蒙花苷的方法。通过蛋白质沉淀（PPT）和液-液萃取（LLE）的组合使用样品制备，以允许在5个数量级的浓度范围内进行测量。在Hypersil Gold柱（100 × 2.1 mm i.d.，5 µm）。使用配备有以正离子化模式操作的电喷雾电离接口的三重四极杆质谱仪实现质谱检测。采用选择性反应监测蒙花苷和黄芩苷（内标）在m/z 593 → 285和m/z 447 → 271处的吸收产物离子跃迁进行定量。每个样品的总运行时间仅为2.8分钟。PPT和LLE的校准曲线在0.4-200 µg/mL和0.001-1.0 µg/mL浓度范围内呈线性。仅使用20 μL血浆或组织匀浆即可达到1.0 ng/mL的定量下限。所有样品的日内和日间精密度均≤ 14.7%，而准确度在标称值的±5.2%范围内。该方法已成功应用于蒙花苷的药代动力学和组织分布研究。
A rapid and sensitive LC-MS/MS method was developed for the determination of linarin in small-volume rat plasma and tissue sample. Sample preparation was employed by the combination of protein precipitation (PPT) and liquid-liquid extraction (LLE) to allow measurement over a 5-order-of-magnitude concentration range. Fast chromatographic separation was achieved on a Hypersil Gold column (100 × 2.1 mm i.d., 5 µm). Mass spectrometric detection was achieved using a triple-quadrupole mass spectrometer equipped with an electrospray ionization interface operating in positive ionization mode. Quantification was performed using selected reaction monitoring of precursor-product ion transitions at m/z 593 → 285 for linarin and m/z 447 → 271 for baicalin (internal standard). The total run time was only 2.8 min per sample. The calibration curves were linear over the concentration range of 0.4-200 µg/mL for PPT and 0.001-1.0 µg/mL for LLE. A lower limit of quantification of 1.0 ng/mL was achieved using only 20 μL of plasma or tissue homogenate. The intra- and inter-day precisions in all samples were ≤14.7%, while the accuracy was within ±5.2% of nominal values. The validated method has been successfully applied to pharmacokinetic and tissue distribution study of linarin.