Department of Traditional Chinese Medicine Resource and Bee Products, Bee Science College, Fujian Agriculture and Forestry University, Fuzhou 350002, China.
Department of Pharmaceutical Analysis, School of Pharmacy, Fujian Medical University, Fuzhou 350122, China.
Molecules. 2018 Dec 25;24(1):64. doi: 10.3390/molecules24010064.
This study has developed a reliable and precise high performance liquid chromatography-tandem mass spectrometry method for the simultaneous determination of five phenolic acids and four flavonoid glycosides in rat plasma after a single intravenous administration of Kudiezi injection (KI). Chromatographic separation was carried out on an UltimateXB-C column (4.6 × 100 mm, 3.5 μm) using a gradient elution program with a mobile phase consisting of water containing 0.5% acetic acid and acetonitrile at a flow rate of 0.6 mL/min. Detection was performed on a triple-quadrupole tandem mass spectrometry using multiple reaction monitoring in negative electrospray ionization mode. The calibration curves of all analytes showed good linearity (R² > 0.990). The results of selectivity, intra-day and inter-day precisions, extraction recoveries, matrix effects and stability were satisfactory. Pharmacokinetic parameters showed that luteolin-7--β-d-gentiobioside, luteolin-7--β-d-glucuronide, luteolin-7--β-d-glucoside and apigenin-7--β-d-glucuronide were eliminated quickly (0.07 h < < 0.66 h), whereas 5-caffeoylquinic acid, caftaric acid, chlorogenic acid, 4-caffeoylquinic acid and caffeic acid were eliminated relatively slowly (2.22 h < < 6.09 h) in rat blood. The pharmacokinetic results would be valuable to identify bioactive constituents, elucidate mechanisms of pharmacological actions or adverse drug reactions and guide the rational clinical use of KI.
本研究建立了一种可靠、精确的高效液相色谱-串联质谱法，用于单次静脉注射苦参注射液（KI）后大鼠血浆中 5 种酚酸和 4 种黄酮苷的同时测定。色谱分离在 UltimateXB-C 柱（4.6×100mm，3.5μm）上进行，采用梯度洗脱程序，流动相由含 0.5%乙酸的水和乙腈组成，流速为 0.6mL/min。检测采用三重四极杆串联质谱，在负离子电喷雾电离模式下采用多反应监测进行检测。所有分析物的校准曲线均呈良好的线性（R²＞0.990）。选择性、日内和日间精密度、提取回收率、基质效应和稳定性的结果令人满意。药代动力学参数表明，木犀草素-7--β-d-龙胆二糖苷、木犀草素-7--β-d-葡萄糖醛酸苷、木犀草素-7--β-d-葡萄糖苷和芹菜素-7--β-d-葡萄糖醛酸苷消除较快（0.07 h＜＜0.66 h），而 5-咖啡酰奎宁酸、咖啡酸、绿原酸、4-咖啡酰奎宁酸和咖啡酸消除较慢（2.22 h＜＜6.09 h）。这些药代动力学结果对于鉴定生物活性成分、阐明药理作用或不良反应的机制以及指导苦参注射液的合理临床应用具有重要意义。
