Yu Jia, Zhu Bolin, Su Dan, Jiang Zhen
Department of Pharmaceutical Analysis, School of Pharmacy, Shenyang Pharmaceutical University 103 Wenhua Road Shenyang Liaoning Province PR China 110016
RSC Adv. 2018 Sep 10;8(55):31633-31645. doi: 10.1039/c8ra04084b. eCollection 2018 Sep 5.
A sensitive, specific and rapid ultra-performance liquid chromatography tandem mass spectrometry method (UPLC-MS/MS) was developed for simultaneous determination of three main alkaloids (daucicoline, daurisoline, dauricine) in rat plasma, urine and feces after oral administration of menispermi rhizoma capsules. The chromatographic separation was performed on a Waters ACQUITY UPLC® BEH C column (50 mm × 2.1 mm, id, 1.7 μm) with a column temperature of 30 °C and a linear gradient elution using a mobile phase consisting of 0.1% formic acid and acetonitrile. The flow rate was set at 0.3 mL min, and the total run time was 10 min. The detection was performed, without interference, using positive electrospray ionization with a multiple reaction monitoring mode. A comprehensive validation of the method was performed. The linearity of the analytical response was good over a wide concentration range with correlation coefficients greater than 0.9903 and the lower limits of quantification were 1.5-5.0 ng mL for all matrices. Both accuracy and precision of the assay were satisfactory. The mean extraction recoveries of analytes and internal standard from rat plasma, urine and feces were all more than 78.3%. The validated methods of the three types of substrates were successfully applied to a pharmacokinetic and excretion study of the three alkaloids in rats after oral administration of menispermi rhizoma capsule. The pharmacokinetics and excretion study of these active components in menispermi rhizoma capsule have not been reported. The results provided a meaningful basis for the clinical application of menispermi rhizoma capsule.
建立了一种灵敏、特异且快速的超高效液相色谱串联质谱法(UPLC-MS/MS),用于同时测定大鼠口服北豆根胶囊后血浆、尿液和粪便中三种主要生物碱(蝙蝠葛碱、蝙蝠葛苏林碱、蝙蝠葛碱)的含量。色谱分离采用Waters ACQUITY UPLC® BEH C18柱(50 mm×2.1 mm,内径,1.7μm),柱温30℃,流动相为0.1%甲酸和乙腈,采用线性梯度洗脱。流速设定为0.3 mL/min,总运行时间为10 min。采用正电喷雾电离和多反应监测模式进行检测,无干扰。对该方法进行了全面验证。在较宽的浓度范围内,分析响应的线性良好,相关系数大于0.9903,所有基质的定量下限为1.5 - 5.0 ng/mL。该测定方法的准确度和精密度均令人满意。大鼠血浆、尿液和粪便中分析物和内标的平均提取回收率均超过78.3%。经验证的三种类型基质的方法成功应用于大鼠口服北豆根胶囊后三种生物碱的药代动力学和排泄研究。北豆根胶囊中这些活性成分的药代动力学和排泄研究尚未见报道。该结果为北豆根胶囊的临床应用提供了有意义的依据。