Lv Song-Feng, Wang Xiang-hong, Li Hong-wei, Zhang Xiao-lei, Wang Bo
Luoyang Orthopedic Traumatological Hospital of Henan Province, Henan Province Hospital of orthopedics, Luoyang 471002, China.
Medical College of Henan University of Science and Technology, Luoyang 471003, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2015 Jun 15;992:43-6. doi: 10.1016/j.jchromb.2015.04.023. Epub 2015 Apr 20.
An ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was developed to determine liensinine in rat plasma using carbamazepine as the internal standard (IS). Sample preparation was accomplished through a protein precipitation procedure with acetonitrile to 0.1ml plasma sample. The analyte and IS were separated on an Acquity UPLC BEH C18 column (2.1mm×50mm, 1.7μm) with the mobile phase of acetonitrile and 0.1% formic acid in water with gradient elution at a flow rate of 0.40ml/min. The injection volume was 6μl. The detection was performed on a triple quadrupole tandem mass spectrometer equipped with electrospray ionization (ESI) by multiple reactions monitoring (MRM) of the transitions at m/z 611.6→206.2 for liensinine and m/z 237.1→194.2 for IS. The linearity of this method was found to be within the concentration range of 10-1000ng/ml with a lower limit of quantification of 10ng/ml. Only 3.0min was needed for an analytical run. The matrix effect was 93.8-107.4% for liensinine. The intra- and inter-day precision (RSD %) were less than 9.9% and accuracy (RE %) was within ±10.5%. The recovery ranged from 76.2 to 86.8%. Liensinine was sufficiently stable under all relevant analytical conditions. The method was also successfully applied to the pharmacokinetic study of liensinine in rats. The pharmacokinetic parameters were demonstrated as followed: t1/2 was 8.2±3.3h, Cmax was 668.4±156.9ng/ml, and AUC0→∞ was 1802.9±466.4ng/mlh.
建立了一种超高效液相色谱串联质谱（UPLC-MS/MS）法，以卡马西平为内标（IS）测定大鼠血浆中莲心碱的含量。通过用乙腈对0.1ml血浆样品进行蛋白沉淀程序来完成样品制备。分析物和内标在Acquity UPLC BEH C18柱（2.1mm×50mm，1.7μm）上分离，流动相为乙腈和0.1%甲酸水溶液，采用梯度洗脱，流速为0.40ml/min。进样量为6μl。采用配备电喷雾电离（ESI）的三重四极杆串联质谱仪，通过多反应监测（MRM）对莲心碱的m/z 611.6→206.2和内标的m/z 237.1→194.2进行检测。该方法的线性范围为10-1000ng/ml，定量下限为10ng/ml。一次分析运行仅需3.0分钟。莲心碱的基质效应为93.8-107.4%。日内和日间精密度（RSD%）小于9.9%，准确度（RE%）在±10.5%以内。回收率在76.2%至86.8%之间。莲心碱在所有相关分析条件下均足够稳定。该方法还成功应用于大鼠莲心碱的药代动力学研究。药代动力学参数如下：t1/2为8.2±3.3h，Cmax为668.4±156.9ng/ml，AUC0→∞为1802.9±466.4ng/mlh。
