Sun Yichun, Xue Juan, Li Baimei, Lin Xiaoting, Wang Zhibin, Jiang Hai, Zhang Hongwei, Wang Qiuhong, Kuang Haixue
Key Laboratory of Chinese Materia Medica (Ministry of Education), Heilongjiang University of Chinese Medicine, Harbin, China.
J Sep Sci. 2016 Nov;39(22):4360-4368. doi: 10.1002/jssc.201600801. Epub 2016 Oct 28.
A rapid, sensitive, and reliable analytical ultra performance liquid chromatography with tandem mass spectrometry method was developed for the simultaneous determination of Aralia-saponin IV, 3-O-β-d-glucopyranosyl-(1→3)-β-d-glucopyranosyl-(1→3)-β-d-glucopyranosyl oleanolic acid 28-O-β-d-glucopyranoside, Aralia-saponin A and Aralia-saponin B after the oral administration of total saponin of Aralia elata leaves in rat plasma. Plasma samples were pretreated by protein precipitation with methanol. The analysis was performed on an ACQUITY UPLC HSS T3 column. The detection was performed on a triple quadrupole tandem mass spectrometer in multiple reaction monitoring mode using an electrospray ionization source with negative ionization mode. Under the experimental conditions, the calibration curves of four analytes had good linearity values (r > 0.991). The intra- and inter-day precision values of the four analytes were ≤ 11.6%, and the accuracy was between -6.2 and 4.2%.The extraction recoveries of four triterpenoid saponins were in the range of 84.06-91.66% (RSD < 10.5%), and all values of the matrix effect were more than 90.30%. The developed analytical method was successfully applied to pharmacokinetic study on simultaneous determination of the four triterpenoid saponins in rat plasma after oral administration of total saponin of Aralia elata leaves, which helps guiding clinical usage of Aralia elata leaves.
建立了一种快速、灵敏、可靠的超高效液相色谱-串联质谱分析方法,用于同时测定大鼠血浆中刺老芽叶总皂苷口服给药后刺五加皂苷IV、3-O-β-D-吡喃葡萄糖基-(1→3)-β-D-吡喃葡萄糖基-(1→3)-β-D-吡喃葡萄糖基齐墩果酸28-O-β-D-吡喃葡萄糖苷、刺五加皂苷A和刺五加皂苷B的含量。血浆样品用甲醇沉淀蛋白进行预处理。分析在ACQUITY UPLC HSS T3柱上进行。采用电喷雾电离源负离子模式,在多反应监测模式下,用三重四极杆串联质谱仪进行检测。在实验条件下,4种分析物的校准曲线线性良好(r>0.991)。4种分析物的日内和日间精密度值≤11.6%,准确度在-6.2%至4.2%之间。4种三萜皂苷的提取回收率在84.06%-91.66%范围内(RSD<10.5%),基质效应值均大于90.30%。所建立的分析方法成功应用于刺老芽叶总皂苷口服给药后大鼠血浆中4种三萜皂苷同时测定的药代动力学研究,有助于指导刺老芽叶的临床应用。