Xiu Fen, Ying Zheming, Ying Xixiang, Yang Guanlin
School of Pharmacy, Liaoning University of Traditional Chinese Medicine, Dalian, China.
School of The First Clinic, Liaoning University of Traditional Chinese Medicine, Shenyang, Liaoning, China.
Biomed Chromatogr. 2019 Feb;33(2):e4399. doi: 10.1002/bmc.4399. Epub 2018 Oct 24.
Soyalkaloid A was isolated from Portulaca oleracea L. for the first time in our laboratory and then a rapid and sensitive ultra-high-performance liquid chromatography electrospray ionization quadrupole-time of flight mass spectrometry (UHPLC-ESI-Q-TOF/MS) method with hesperidin as internal standard (IS) was developed and validated to investigate the pharmacokinetics of soyalkaloid A in rats after oral and intravenous administrations. The analysis was achieved on an Agilent Zorbax Eclipse Plus C Column (2.1 × 50 mm, 1.8 μm) by elution with acetonitrile and water (containing 0.1% formic acid), at a flow rate of 0.3 mL/min. The MS analysis was performed in the positive ion mode with monitored ion m/z 227.0814 [M + H] and 611.1971 [M + H] for soyalkaloid A and IS, respectively. The linear range was established over the concentration range 7.5-6000 ng/mL (r = 0.9951). The intra- and inter-assay accuracy and precision were between -4.86-4.49 and 1.93-9.66, respectively. The lower limits of detection and quantitation observed were 2.1 and 7.4 ng/mL, respectively. The rapid, sensitive and specific UHPLC-ESI-Q-TOF/MS method was successfully applied to a pharmacokinetic study of soyalkaloid A. Moreover, its antioxidant was studied via a 1,1-diphenyl-2-picryl-hydrazyl radical scavenging assay, the IC value being 20.73 ± 0.51 μM.
大豆生物碱A首次在我们实验室从马齿苋中分离得到,随后建立并验证了一种以橙皮苷为内标(IS)的快速灵敏的超高效液相色谱-电喷雾电离四极杆-飞行时间质谱(UHPLC-ESI-Q-TOF/MS)方法,用于研究大鼠口服和静脉给药后大豆生物碱A的药代动力学。分析在安捷伦Zorbax Eclipse Plus C柱(2.1×50 mm,1.8μm)上进行,以乙腈和水(含0.1%甲酸)洗脱,流速为0.3 mL/min。质谱分析在正离子模式下进行,分别监测大豆生物碱A和内标的离子m/z 227.0814 [M + H]和611.1971 [M + H]。线性范围在7.5 - 6000 ng/mL浓度范围内建立(r = 0.9951)。批内和批间准确度和精密度分别在-4.86 - 4.49和1.93 - 9.66之间。观察到的检测限和定量下限分别为2.1和7.4 ng/mL。该快速、灵敏且特异的UHPLC-ESI-Q-TOF/MS方法成功应用于大豆生物碱A的药代动力学研究。此外,通过1,1-二苯基-2-苦基肼自由基清除试验研究了其抗氧化活性,IC值为20.73±0.51 μM。