Ma Yingyan, Xu Kai, Wang Shumin, Han Yaling
Department of Cardiology, Northern Hospital, Shenyang 110840, China.
Department of Thoracic Surgery, Northern Hospital, Shenyang 110840, China.
J Chromatogr Sci. 2014 Sep;52(8):793-8. doi: 10.1093/chromsci/bmt114. Epub 2013 Jul 25.
A rapid, sensitive and selective liquid chromatography-tandem mass spectrometry was developed to determine two epimeric furofuran lignans (sesamin and asarinin) simultaneously from Asarum heterotropoides extract in rat plasma. Simple protein precipitation with acetonitrile was performed to extract analytes by using alantolactone as an internal standard. Chromatographic separation was achieved using a DIKMA Diamonsil C18 analytical column (4.6 mm × 150 mm, i.d., 5 µm) by isocratically eluting with a mobile phase consisting of methanol/5 mM ammonium acetate/formic acid (75:25:0.1, v/v/v) at a flow rate of 0.8 mL/min. Tandem mass spectrometric detection with an electrospray ionization interface was performed by multiple reaction monitoring in positive ionization mode. This method was validated according to specificity, sensitivity, linearity, intra- and inter-day precision (<10.7%) and accuracy (<2.3%) and recovery and stability in a concentration range of 25.0-15 000 ng/mL for sesamin and 5.00-3 000 ng/mL for asarinin. This method has been successfully applied in a pharmacokinetic study of A. heterotropoides extract containing sesamin and asarinin after this extract was orally administrated in rats.
建立了一种快速、灵敏且选择性高的液相色谱-串联质谱法，用于同时测定大鼠血浆中细辛提取物中的两种差向异构呋喃呋喃木脂素（芝麻素和细辛脂素）。采用乙腈进行简单的蛋白沉淀，以土木香内酯为内标物提取分析物。使用迪马钻石C18分析柱（4.6 mm×150 mm，内径，5 µm），以甲醇/5 mM醋酸铵/甲酸（75:25:0.1，v/v/v）组成的流动相在0.8 mL/min的流速下等度洗脱，实现色谱分离。采用电喷雾电离接口进行串联质谱检测，在正离子模式下通过多反应监测进行。该方法在特异性、灵敏度、线性、日内和日间精密度（<10.7%）和准确度（<2.3%）以及回收率和稳定性方面得到验证，芝麻素的浓度范围为25.0 - 15000 ng/mL，细辛脂素的浓度范围为5.00 - 3000 ng/mL。该方法已成功应用于大鼠口服含芝麻素和细辛脂素的细辛提取物后的药代动力学研究。
