Ma Jianshe, Ding Xitao, Sun Chengxiang, Lin Chongliang, An Xinxin, Lin Guanyang, Yang Xuezhi, Wang Xianqin
Function Experiment Teaching Center of Wenzhou Medical University, Wenzhou 325035, China.
The First Affiliated Hospital of Wenzhou Medical University, Wenzhou 325000, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Jul 15;963:24-8. doi: 10.1016/j.jchromb.2014.05.031. Epub 2014 May 23.
Solasodine is a poisonous alkaloid chemical compound that occurs in plants of the Solanaceae family. A simple and selective liquid chromatography mass spectrometry method for determination of solasodine in rat plasma was developed and validated over the range of 3-1,000 ng/mL. Chromatographic separation was achieved on a C18 (2.1 mm×50 mm, 3.5 μm) column with acetonitrile-0.1% formic acid in water as mobile phase with gradient elution. The flow rate was set at 0.4 mL/min. After addition of midazolam as internal standard (IS), liquid-liquid extraction by ethyl acetate was used as sample preparation. An electrospray ionization source was applied and operated in positive ion mode; selective ion monitoring mode was used for quantification with target ions m/z 414 for solasodine and m/z 326 for IS. Mean recoveries of solasodine in rat plasma were in the range of 87.6-94.1%. Matrix effects for solasodine were between 94.9% and 102.3%. Coefficient of variation of intra-day and inter-day precision were both <13%. The accuracy of the method ranged from 94.4% to 105.3%. The method was successfully applied to a pharmacokinetic study of solasodine after oral administration of 20mg/kg in rats.
茄解定是一种存在于茄科植物中的有毒生物碱化合物。建立了一种简单且具有选择性的液相色谱 - 质谱法，用于测定大鼠血浆中茄解定的含量，该方法在3 - 1000 ng/mL范围内得到验证。采用C18（2.1 mm×50 mm，3.5 μm）色谱柱，以乙腈 - 0.1%甲酸水溶液为流动相进行梯度洗脱，实现色谱分离。流速设定为0.4 mL/min。加入咪达唑仑作为内标（IS）后，采用乙酸乙酯液 - 液萃取法进行样品制备。采用电喷雾电离源，以正离子模式运行；采用选择性离子监测模式进行定量分析，茄解定的目标离子为m/z 414，内标的目标离子为m/z 326。大鼠血浆中茄解定的平均回收率在87.6% - 94.1%范围内。茄解定的基质效应在94.9%至102.3%之间。日内和日间精密度的变异系数均<13%。该方法的准确度在94.4%至105.3%之间。该方法成功应用于大鼠口服20mg/kg茄解定后的药代动力学研究。
