Chen Yuanyuan, Zhang Shuangshuang, Chen Dahui, Zhou Mi, Zheng Jing, Xiang Zheng
School of Pharmaceutical Sciences, Wenzhou Medical University/, Wenzhou 325035, China.
School of Pharmaceutical Sciences, Wenzhou Medical University/, Wenzhou 325035, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2015 Mar 15;985:1-5. doi: 10.1016/j.jchromb.2015.01.017. Epub 2015 Jan 23.
Solasonine, a known glycoalkaloid, is a potential anti-cancer agent. In this work, a simple, sensitive and fast ultra performance liquid chromatography with tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for the quantitative determination of solasonine in rat plasma. Plasma samples were processed with a protein precipitation. The separation was achieved by an ACQUITY HSS T3 (100×2.1mm, 1.8μm) column with a gradient mobile phase consisting of 0.1% formic acid and acetonitrile. Detection was carried out using positive-ion electrospray tandem mass spectrometry via multiple reaction monitoring (MRM). The validated method had an excellent linearity in the range of 0.1-500ng/mL (R(2)>0.994) with a low limit of detection (0.1ng/mL) and lower limit of quantification (0.5ng/mL). The extraction recovery was in the range of 92.4-94.9% for solasonine and 91.9% for dendrobine (internal standard, IS). The intra- and inter-day precision was below 9.8% and accuracy was from 86.0% to 94.3%. No notable matrix effect and astaticism was observed for solasonine. The method has been successfully applied to a pharmacokinetic and bioavailability study of solasonine in rats for the first time, which provides the basis for the further development and application of solasonine.
茄解碱是一种已知的糖生物碱，是一种潜在的抗癌剂。在本研究中，开发并验证了一种简单、灵敏且快速的超高效液相色谱-串联质谱法（UPLC-MS/MS），用于定量测定大鼠血浆中的茄解碱。血浆样品采用蛋白沉淀法处理。采用ACQUITY HSS T3（100×2.1mm，1.8μm）色谱柱，以0.1%甲酸和乙腈组成的梯度流动相进行分离。采用正离子电喷雾串联质谱通过多反应监测（MRM）进行检测。验证后的方法在0.1-500ng/mL范围内具有良好的线性（R(2)>0.994），检测限低（0.1ng/mL），定量下限低（0.5ng/mL）。茄解碱的提取回收率在92.4-94.9%之间，石斛碱（内标，IS）的提取回收率为91.9%。日内和日间精密度低于9.8%，准确度在86.0%-94.3%之间。未观察到茄解碱有明显的基质效应和稳定性问题。该方法首次成功应用于大鼠茄解碱的药代动力学和生物利用度研究，为茄解碱的进一步开发和应用提供了依据。
