Department of Pharmaceutical Analysis and Analytical Chemistry, College of Pharmacy, Harbin Medical University, No. 157 Baojian Road, Nangang District, Harbin 150081, China.
School of Pharmaceutical Sciences, Sun Yat-sen University, Guangzhou 510006, China.
Molecules. 2018 Nov 15;23(11):2980. doi: 10.3390/molecules23112980.
A selective and sensitive ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed and validated for the determination of ziyuglycoside I (), 3β,19α-dihydroxyurs-12-en-28-oic-acid 28-β-d-glucopyranosyl ester (), 3β-[(α-l-arabinopyranosyl) oxy]-urs-12,18(19)-dien-28-oic acid β-d-glucopyranosyl ester (), rosamultin (), 1β-hydroxyeuscaphic acid () and alpinoside () in rats after oral administration of L. () extract. The 3β,19α-dihydroxyurs-12-en-28-oic-acid 28-β-d-glucopyranosyl ester, 3β-[(α-l-arabinopyranosyl) oxy]-urs-12,18(19)-dien-28-oic acid β-d-glucopyranosyl ester, rosamultin, 1β-hydroxyeuscaphic acid and alpinoside in rat plasma were the first report in the pharmacokinetics study in the present study. The analytes were quantified using the multiple reaction monitoring (MRM) mode with the electrospray ion source in positive electrospray ionization. Plasma was extracted with ethyl acetate via liquid⁻liquid extraction. Bifendate was used as internal standard (IS). The current method was validated for linearity, intra-day and inter-day precisions, accuracy, extraction recovery, matrix effect and stability. The lower limits of quantification of ziyuglycoside I, 3β,19α-dihydroxyurs-12-en-28-oic-acid 28-β-d-glucopyranosyl ester, 3β-[(α-l-arabinopyranosyl) oxy]-urs-12,18(19)-dien-28-oic acid β-d-glucopyranosyl ester, rosamultin, 1β-hydroxyeuscaphic acid and alpinoside were 6.1, 4.9, 1.3, 3.8, 1.5 and 5.7 ng/mL, respectively. Intra-day and inter-day precision and the accuracy of the assay were in range from -9.48 to 12.74%. The extraction recoveries of analytes and bifendate (IS) from rat plasma ranged from 77.17% to 92.48%. Six compounds could be rapidly absorbed into blood (, 0.58⁻1.58 h), and then eliminated relatively slowly (, 6.86⁻11.63 h). The pharmacokinetic results might contribute to further guide the clinical application of .
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,用于测定大鼠口服 L. ()提取物后血浆中的 Ziyuglycoside I ()、3β,19α-二羟基熊果酸 28-β-D-吡喃葡萄糖酯 ()、3β-[(α-L-阿拉伯吡喃糖基)氧基]-熊果酸 12,18(19)-二烯-28-羧酸 β-D-吡喃葡萄糖酯 ()、Rosamultin ()、1β-羟基桉脂素酸 ()和 Alpinoside ()。本研究中,3β,19α-二羟基熊果酸 28-β-D-吡喃葡萄糖酯、3β-[(α-L-阿拉伯吡喃糖基)氧基]-熊果酸 12,18(19)-二烯-28-羧酸 β-D-吡喃葡萄糖酯、Rosamultin、1β-羟基桉脂素酸和 Alpinoside 在大鼠的药代动力学研究中为首次报道。采用电喷雾源正离子模式下的多重反应监测(MRM)模式对分析物进行定量。采用液液萃取法用乙酸乙酯从血浆中提取。双飞仙作为内标(IS)。该方法经过线性、日内和日间精密度、准确度、提取回收率、基质效应和稳定性验证。Ziyuglycoside I、3β,19α-二羟基熊果酸 28-β-D-吡喃葡萄糖酯、3β-[(α-L-阿拉伯吡喃糖基)氧基]-熊果酸 12,18(19)-二烯-28-羧酸 β-D-吡喃葡萄糖酯、Rosamultin、1β-羟基桉脂素酸和 Alpinoside 的定量下限分别为 6.1、4.9、1.3、3.8、1.5 和 5.7 ng/mL。该测定的日内和日间精密度及准确度均在-9.48%至 12.74%范围内。分析物和双飞仙(IS)从大鼠血浆中的提取回收率为 77.17%至 92.48%。六种化合物可迅速被血液吸收(0.58-1.58 h),然后缓慢消除(6.86-11.63 h)。药代动力学结果可能有助于进一步指导 的临床应用。