Rong Rong, Cui Mei-Yu, Zhang Qi-Li, Zhang Mei-Yan, Yu Yu-Ming, Zhou Xian-Ying, Yu Zhi-Guo, Zhao Yun-Li
Institute Department of Pharmaceutical Analysis, School of Pharmacy, Shenyang Pharmaceutical University, Shenyang, China.
J Sep Sci. 2016 Jul;39(14):2728-35. doi: 10.1002/jssc.201600295. Epub 2016 Jun 27.
A sensitive and selective ultra high performance liquid chromatography with tandem mass spectrometry method was established and validated for the simultaneous determination of hydroxy-α-sanshool, hydroxy-β-sanshool, and hydroxy-γ-sanshool in rat plasma after the subcutaneous and intravenous administration of an extract of the pericarp of Zanthoxylum bungeanum Maxim. Piperine was used as the internal standard. The analytes were extracted from rat plasma by liquid-liquid extraction with ethyl acetate and separated on a Thermo Hypersil GOLD C18 column (2.1 mm × 50 mm, 1.9 μm) with a gradient elution system at a flow rate of 0.4 mL/min. The mobile phase consisted of acetonitrile/0.05% formic acid in water and the total analysis time was 4 min. Positive electrospray ionization was performed using multiple reaction monitoring mode for the analytes. The calibration curves of the three analytes were linear over the tested concentration range. The intra- and interday precision was no more than 13.6%. Extraction recovery, matrix effect, and stability were satisfactory in rat plasma. The developed and validated method was suitable for the quantification of hydroxy-α-sanshool, hydroxy-β-sanshool, and hydroxy-γ-sanshool and successfully applied to a pharmacokinetic study of these analytes after subcutaneous and intravenous administration to rats.
建立并验证了一种灵敏且具选择性的超高效液相色谱-串联质谱法,用于同时测定大鼠皮下和静脉注射花椒(Zanthoxylum bungeanum Maxim)果皮提取物后血浆中羟基-α-山椒素、羟基-β-山椒素和羟基-γ-山椒素的含量。胡椒碱用作内标。通过乙酸乙酯液-液萃取从大鼠血浆中提取分析物,并在Thermo Hypersil GOLD C18柱(2.1 mm×50 mm,1.9μm)上进行分离,采用梯度洗脱系统,流速为0.4 mL/min。流动相由乙腈/0.05%甲酸水溶液组成,总分析时间为4分钟。对分析物采用正电喷雾电离,以多反应监测模式进行检测。三种分析物的校准曲线在测试浓度范围内呈线性。日内和日间精密度均不超过13.6%。大鼠血浆中的提取回收率、基质效应和稳定性均令人满意。所建立并验证的方法适用于羟基-α-山椒素、羟基-β-山椒素和羟基-γ-山椒素的定量分析,并成功应用于大鼠皮下和静脉注射后这些分析物的药代动力学研究。