First Teaching Hospital of Tianjin University of Traditional Chinese Medicine, Tianjin 300193, China.
Tianjin State Key Laboratory of Modern Chinese Medicine, Tianjin University of Traditional Chinese Medicine, Tianjin 301617, China.
Biomed Res Int. 2020 Aug 21;2020:8420409. doi: 10.1155/2020/8420409. eCollection 2020.
A rapid and reliable UPLC-MS/MS method was developed and validated for the simultaneous quantification of thirteen bioactive compounds (luteolin, cynaroside, luteolin 7-O-glucuronide, isochlorogenic acid C, chlorogenic acid, cryptochlorogenic acid, apigenin, apigenin 7-glucoside, acacetin, hyperoside, isoquercitrin, tilianin, and hesperidin) in rat plasma. The compounds were separated on an ACQUITY UPLC BEH C column (2.1 × 100 mm, 1.7 m) with a gradient mobile phase system of acetonitrile and 0.1% (/) formic acid aqueous solution at a flow rate of 0.3 mL/min. All compounds were quantitated using Agilent Jet Stream electrospray ionization (AJS ESI) in a negative ion mode. The lower limit of quantification (LLOQ) for all compounds was below 5 ng/mL. The intra- and interday accuracy ranged from -13.0% to 14.0%, and precisions were less than 12.2%. The extraction recoveries of the compounds were in the range of 56.9% to 95.0%, and the matrix effect ranged between 71.6% and 109.3%. Stability studies proved that the thirteen compounds were stable under tested conditions, with a relative standard deviation (RSD) of less than 11.4%. This developed method was successfully applied to the pharmacokinetic study of the 13 bioactive compounds after oral administration of extract in rat by UPLC-MS/MS. Pharmacokinetic parameters of 8 out of the 13 compounds investigated are presented in this paper.
建立并验证了一种快速可靠的 UPLC-MS/MS 法,用于同时定量测定大鼠血浆中 13 种生物活性化合物(木樨草素、山柰苷、木樨草素 7-O-葡萄糖苷、异绿原酸 C、绿原酸、隐绿原酸、芹菜素、芹菜素 7-葡萄糖苷、木犀草素、高圣草素、异槲皮苷、荭草苷、橙皮苷)。采用 ACQUITY UPLC BEH C 柱(2.1×100mm,1.7μm),以乙腈和 0.1%(/)甲酸水溶液为流动相系统,梯度洗脱,流速为 0.3mL/min。所有化合物均采用安捷伦喷气流电喷雾电离(AJS ESI)在负离子模式下定量。所有化合物的定量下限(LLOQ)均低于 5ng/mL。日内和日间准确度范围为-13.0%至 14.0%,精密度小于 12.2%。化合物的提取回收率在 56.9%至 95.0%之间,基质效应在 71.6%至 109.3%之间。稳定性研究证明,在测试条件下,13 种化合物稳定,相对标准偏差(RSD)小于 11.4%。该方法已成功应用于 UPLC-MS/MS 法测定大鼠灌胃 提取物后 13 种生物活性化合物的药代动力学研究。本文介绍了 8 种研究化合物的药代动力学参数。