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
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
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在线 SPE-HPLC-DAD 测定大鼠血浆中 4-甲基哌嗪-1-硫代碳酸 3-氰基-3,3-二苯丙酯盐酸盐：在药代动力学研究中的应用
DOI：
10.1002/jssc.201100876
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发表时间：
2012-03-01
影响因子：
3.1
通讯作者：
Cui, Jingrong
中科院分区：
文献类型：
--
作者：
Zhang, Jianmei;Lin, Wensi;Cui, Jingrong
建立了固相萃取-高效液相色谱-二极管阵列检测器（SPE-HPLC-DAD）法测定大鼠血浆中4-甲基哌嗪-1-硫代甲酸3-氰基-3，3-二苯基丙酯盐酸盐（TM 208）含量的方法。在该方法中，取50 μ L血浆样品，用75 μ L甲醇进行蛋白质沉淀，然后进样50 μ L含有目标分析物的上清液，并在C18固相萃取（SPE）柱中自动浓缩。然后在C18 RP分析柱上分离样品，并通过DAD进行分析。每个样品的运行周期为6.0 min，标准曲线在0.03 ~ 25.00 μ g/mL范围内线性关系良好（r > 0.9998）。质量控制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0.03 μ g/mL。该方法已成功应用于TM 208在大鼠体内的药代动力学研究。
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-mu L plasma sample was taken to perform protein precipitation with 75 mu L methanol, and then 50 mu L 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 mu g/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 mu g/mL, respectively. Finally, this method was successfully applied to a pharmacokinetic study of TM208 in rats.