在线 SPE-HPLC-DAD 法测定大鼠血浆中 4-甲基哌嗪-1-碳二硫代酸 3-氰基-3,3-二苯基丙酯盐酸盐：在药代动力学研究中的应用。
Determination of 4-methylpiperaine-1-carbodithioc acid 3-cyano-3,3-diphenylpropyl ester hydrochloride in rats' plasma by online-SPE-HPLC-DAD: application to a pharmacokinetic study.
机构信息
Department of Pharmaceutical Analysis, School of Pharmaceutical Sciences, Peking University, Beijing, China.
出版信息
J Sep Sci. 2012 Mar;35(5-6):721-5. doi: 10.1002/jssc.201100876.
A specific, simple, and fast online-solid-phase extraction-high performance liquid chromatography-diode array detector (SPE-HPLC-DAD) method was developed and validated to quantify 4-methylpiperaine-1-carbodithioc acid 3-cyano-3,3-diphenylpropyl ester hydrochloride (TM208) in small volume samples of rats' plasma for the first time. In this method, the 50-μL plasma sample was taken to perform protein precipitation with 75 μL methanol, and then 50 μL supernatant containing the target analytes was injected and concentrated automatically in a C18 solid-phase extraction (SPE) cartridge. After that the sample was separated on a C18 RP analytical column and analyzed by DAD. The run cycle time is 6.0 min for each sample, and the calibration curve over the range of 0.03 to 25.00 μg/mL has a good linear relationship (r > 0.9998). The recoveries of the quality control samples were all greater than 90%. The limit of detection and the lowest limit of quantification were 0.01 and 0.03 μg/mL, respectively. Finally, this method was successfully applied to a pharmacokinetic study of TM208 in rats.
建立并验证了一种特定、简单、快速的在线固相萃取-高效液相色谱-二极管阵列检测（SPE-HPLC-DAD）方法，用于首次定量检测大鼠血浆中少量样品中的 4-甲基哌啶-1-碳二硫代酸 3-氰基-3,3-二苯基丙酯盐酸盐（TM208）。在该方法中，取 50μL 血浆样品，用 75μL 甲醇进行蛋白沉淀，然后将含有目标分析物的 50μL 上清液自动注入并在 C18 固相萃取（SPE）小柱中浓缩。然后将样品在 C18 RP 分析柱上分离，并通过 DAD 进行分析。每个样品的运行周期时间为 6.0 分钟，在 0.03 至 25.00μg/mL 的范围内，校准曲线具有良好的线性关系（r>0.9998）。质控样品的回收率均大于 90%。检测限和最低定量限分别为 0.01 和 0.03μg/mL。最后，该方法成功应用于大鼠 TM208 的药代动力学研究。
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