Wang Zhibin, Wu Qiong, Meng Yonghai, Sun Yichun, Wang Qi, Yang Chunjuan, Wang Qiuhong, Yang Bingyou, Kuang Haixue
Key Laboratory of Chinese Materia Medica (Ministry of Education), Heilongjiang University of Chinese Medicine, 24 Heping Road, Xiangfang District, Harbin 150040, China; Department of Pharmaceutics, Ernest Mario School of Pharmacy, Rutgers, The State University of New Jersey, Piscataway, NJ 08854, USA.
Key Laboratory of Chinese Materia Medica (Ministry of Education), Heilongjiang University of Chinese Medicine, 24 Heping Road, Xiangfang District, Harbin 150040, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2015 Mar 15;985:164-71. doi: 10.1016/j.jchromb.2015.01.036. Epub 2015 Feb 3.
Aralia elata (Miq.) Seems (A. elata) grow in Northeast China and the total saponins of A. elata is used to auxiliary treatment for the acute hepatitis, chronic hepatitis and the transaminase on the high side. Aralia-saponinV and Aralia-saponinVI are the major bioactive saponins in A. elata leaves. A selective and sensitive UHPLC-MS/MS method was developed and validated for the determination and pharmacokinetic study of Aralia-saponinV and Aralia-saponinVI indwelling the extract in rat plasma in this article. The sample pretreatment involved a one-step extraction of 0.2mL plasma with methanol. Shengmaxinside C was used as internal standard (I.S.). The separation was carried out on an Agilent SB-C18 column (1.8μm, 50mm×2.1mm) at 30°C with a mobile phase of acetonitrile-5mM ammonium acetate (90:10, v/v) at a flow rate of 0.2mL/min. The detection was performed on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring (MRM) mode via electrospray ionization (ESI) source operating in the negative ionization mode. The optimized mass transition ion-pairs (m/z) monitored for Aralia-saponinV, Aralia-saponinVI and I.S. were 1103.2/941.2, 1119.2/957.0 and 707.0/647.1, respectively. The current UHPLC-MS/MS assay method was validated for linearity, intra-day and inter-day precisions, accuracy, extraction recovery and stability, and it was suitable for the pharmacokinetic studies of the two saponins after oral administration of extract of A. elata leaves. The lower limits of quantification were 5.70ng/mL for Aralia-saponinV and 6.15ng/mL for Aralia-saponinVI. Intra-day and inter-day precisions were less than 7.4% and the accuracy range was from 1.19% to 8.60%. The mean extraction recoveries of analytes and I.S. from rat plasma were all more than 89.5%. This paper described a simple, sensitive and validated UHPLC-MS/MS method for simultaneous determination of Aralia-saponinV and Aralia-saponinVI in rat plasma after oral administration of the extract of A. elata leaves, and investigated on their pharmacokinetic studies as well.
辽东楤木(Aralia elata (Miq.) Seems,即辽东楤木)生长于中国东北地区,其总皂苷用于辅助治疗急性肝炎、慢性肝炎以及转氨酶偏高的情况。楤木皂苷V和楤木皂苷VI是辽东楤木叶中的主要生物活性皂苷。本文建立并验证了一种选择性和灵敏的超高效液相色谱-串联质谱(UHPLC-MS/MS)方法,用于测定大鼠血浆中提取物中的楤木皂苷V和楤木皂苷VI及其药代动力学研究。样品预处理包括用甲醇一步提取0.2mL血浆。升麻素苷C用作内标(I.S.)。分离在安捷伦SB-C18柱(1.8μm,50mm×2.1mm)上于30℃进行,流动相为乙腈-5mM醋酸铵(90:10,v/v),流速为0.2mL/min。检测在三重四极杆串联质谱仪上通过多反应监测(MRM)模式进行,采用电喷雾电离(ESI)源,以负离子模式运行。监测楤木皂苷V、楤木皂苷VI和内标的优化质量转移离子对(m/z)分别为1103.2/941.2、1119.2/957.0和707.0/647.1。当前的UHPLC-MS/MS测定方法在线性、日内和日间精密度、准确度、提取回收率和稳定性方面得到了验证,适用于口服辽东楤木叶提取物后两种皂苷的药代动力学研究。楤木皂苷V的定量下限为5.70ng/mL,楤木皂苷VI的定量下限为6.15ng/mL。日内和日间精密度均小于7.4%,准确度范围为1.19%至8.60%。分析物和内标从大鼠血浆中的平均提取回收率均超过89.5%。本文描述了一种简单、灵敏且经过验证的UHPLC-MS/MS方法,用于同时测定口服辽东楤木叶提取物后大鼠血浆中的楤木皂苷V和楤木皂苷VI,并对其药代动力学进行了研究