Wei Fen, Gou Xilan, Xu Xiao, Wang Sicen, Bao Tao
School of Pharmacy, Health Science Center, Xi'an Jiaotong University, Xi'an 710061, China.
Shaanxi Engineering Research Center of Cardiovascular Drugs Screening & Analysis, Xi'an 710061, China.
J Anal Methods Chem. 2021 Feb 26;2021:6629579. doi: 10.1155/2021/6629579. eCollection 2021.
Liensinine, an important alkaloid in lotus seed, exhibits multiple functions such as anti-AIDS, anticancer, antidepressant, and antihypertensive properties. In this study, a highly sensitive HPLC-MS/MS method was developed and validated for the quantification of liensinine in microvolume rat plasma as low as 45 L. Chromatographic separation was carried out using a reverse-phase Gemini-C18 column (100 mm × 3 mm i.d. × 5 m), and mass selective detection using multiple reaction monitoring was attained using an electrospray ionization source, which operated in the positive mode. Dauricine was used as the internal standard. The precursor-to-product ion transition m/z 611.15 > 206.10 was selected for the detection of liensinine; m/z 625.25 > 206.10 was used for the detection of dauricine. The developed method is linear over the concentration range of 0.05-1000 ng/mL with an excellent coefficient of determination ( = 0.991). The recoveries ranged from 92.57% to 95.88% at three quality control levels. Intraday and interday precision and accuracy are less than 12.2% and 6.59%, respectively. The lower limit of quantification (LLOQ) is 0.05 ng/mL. The matrix effect was insignificant and acceptable. The validated method was successfully applied to the pharmacokinetic study of liensinine in rats. This method can be used for studies as well as quality control of traditional Chinese medicines and herbal tea containing liensinine alkaloid.
莲心碱是莲子中的一种重要生物碱，具有多种功能，如抗艾滋病、抗癌、抗抑郁和降血压等特性。在本研究中，开发并验证了一种高灵敏度的HPLC-MS/MS方法，用于定量测定微体积大鼠血浆中低至45μL的莲心碱。采用反相Gemini-C18柱（100mm×3mm内径×5μm）进行色谱分离，使用电喷雾电离源以正模式运行，通过多反应监测实现质量选择性检测。以蝙蝠葛碱作为内标。选择母离子到子离子的跃迁m/z 611.15＞206.10用于检测莲心碱；m/z 625.25＞206.10用于检测蝙蝠葛碱。所开发的方法在0.05-1000ng/mL的浓度范围内呈线性，具有出色的决定系数（R² = 0.991）。在三个质量控制水平下，回收率在92.57%至95.88%之间。日内和日间精密度及准确度分别小于12.2%和6.59%。定量下限（LLOQ）为0.05ng/mL。基质效应不显著且可接受。经过验证的方法成功应用于大鼠体内莲心碱的药代动力学研究。该方法可用于含莲心碱生物碱的中药和凉茶的研究以及质量控制。
