Key Laboratory of Basic Pharmacology of Ministry of Education and Joint International Research Laboratory of Ethnomedicine of Ministry of Education, Zunyi Medical University, Zunyi, P. R. China.
Department of Pharmaceutical Analysis, Key Laboratory of Drug Quality control and Pharmacovigilance of Ministry of Education, China Pharmaceutical University, Nanjing, P. R. China.
J Sep Sci. 2018 Oct;41(20):3830-3839. doi: 10.1002/jssc.201800585. Epub 2018 Aug 26.
A selective and accurate HPLC-MS/MS method was established to simultaneously quantify luteolin and its active metabolites (diosmetin, chryseriol, and luteolin-7-O-glucuronide) in rat plasma. The analytes were separated on a C column with a mobile phase of water containing 0.5% formic acid and acetonitrile under gradient elution to shorten the total chromatographic run time and increase the resolution of diosmetin and chryseriol. A triple quadruple mass spectrometer coupled with an electrospray ionization source in the negative ion mode was used to detect the analytes. The multiple reaction monitoring transitions were of m/z 284.9→132.9 for luteolin, m/z 298.9→283.9 for diosmetin and chryseriol, m/z 461.1→284.9 for luteolin-7-O-glucuronide, and m/z 300.9→150.9 for the internal standard. The method was linear within the concentration ranges of 0.06-90 μg/mL for luteolin, 0.03-12 μg/mL for diosmetin, 0.015-4.8 μg/mL for chryseriol, and 0.06-60 μg/mL for luteolin-7-O-glucuronide. The intra- and interday precisions were all within 6.0%. Accuracy ranged from -3.2 to 6.4%. The matrix effect and instability were not observed during bioanalysis. This method was used to study the pharmacokinetic characteristics of luteolin and its metabolites in rats after treatment with luteolin.
建立了一种选择性和准确的 HPLC-MS/MS 方法，用于同时定量测定大鼠血浆中的木樨草素及其活性代谢物（芹菜素、橙皮素和木樨草素-7-O-葡萄糖苷）。分析物在 C 柱上分离，流动相为含 0.5%甲酸的水和乙腈，采用梯度洗脱，以缩短总色谱运行时间并提高芹菜素和橙皮素的分辨率。三重四极杆质谱仪与电喷雾源在负离子模式下联用，用于检测分析物。多重反应监测转换为 m/z 284.9→132.9 用于木樨草素，m/z 298.9→283.9 用于芹菜素和橙皮素，m/z 461.1→284.9 用于木樨草素-7-O-葡萄糖苷，m/z 300.9→150.9 用于内标。该方法在木樨草素的浓度范围为 0.06-90 μg/mL、芹菜素的浓度范围为 0.03-12 μg/mL、橙皮素的浓度范围为 0.015-4.8 μg/mL、木樨草素-7-O-葡萄糖苷的浓度范围为 0.06-60 μg/mL 时呈线性。日内和日间精密度均在 6.0%以内。准确度范围为-3.2%至 6.4%。在生物分析过程中未观察到基质效应和不稳定性。该方法用于研究木樨草素及其代谢物在大鼠体内经木樨草素处理后的药代动力学特征。
