摘要
目的:采用液质联用技术,分析四逆散水煎液体外化学成分及血中移行成分,对其体内外物质基础进行研究。方法:采用ACQUITY UPLCTMBEH C18柱(2.1 mm×100 mm,1.7μm),以乙腈-2 mmol.L-1醋酸铵水溶液为流动相进行梯度洗脱,流速0.2 mL.min-1,柱温35℃;质谱采用ESI源,正负离子同时检测,在m/z 100~1 000进行扫描,并对特征离子进行2次裂解,获得二级质谱数据。结果:在四逆散水煎液中,检测到芍药苷、甘草酸、柴胡皂苷a及柚皮苷等20种化学成分。在体内样品中,发现芍药苷、柚皮苷、橙皮苷等8种成分以原型入血;同时还检测到6种代谢物,包括葡萄糖醛酸结合物、硫酸酯结合物及葡萄糖醛酸硫酸酯结合物等。结论:采用UPLC-PDA-MS/MS技术分析四逆散水煎液的体内外化学成分,能比较全面、快速地反映四逆散水煎液的体内外物质基础,为进一步研究四逆散的药效物质基础提供依据。
Objective: To analyze chemical constituents of Sini San its migrating components in rat plasma and study its in vitro and in vivo material base using ultra-performance liquid chromatography coupled with photo-diode-array detector and tandem mass spetrometry (UPLC-PDA-MS/MS). Method: ACQUITT UPLC^TM BEH C18 column (2. 1 mm×100 mm, 1.7 μm) was adopted, with gradient elution system of water containing 2 mmol·L^ -1 ammonium acetate and acetonitrile at flow rate of 0. 2 mL·min^-1. The col- umn temperature was maintained at 35 ℃. The mass spectra were obtained by electrospray ionization source operating in both positive and negative ion mode. Ions were scanned from the m/z 100 to 1 000, and the characteristic ions were sehizolysised twice to obtain the secondary MS data. Result: Twenty chemical constituents were detected, including paeoniflorin, glyeyrrhizic acid, saikosaponins a and naringin. In vivo, there were 8 ingredients directly absorbed into blood after the administration of Sini San decoction, such as pae- oniflorin, naringin and hesperidin. Besides, 6 metabolites were also detected, involving glucuronides, sulfate and sulfoglueuronides. Conclusion: In vitro and in vivo chemical materials of Sini San decoction is analyzed by UPLC-PDA-MS/MS to reflect in vitro and in vivo material base of Sini San decoction in a comprehensive and rapid manner and provide basis for further study on efficacious material basis of Sini San decoction.
出处
《中国中药杂志》
CAS
CSCD
北大核心
2012年第11期1672-1676,共5页
China Journal of Chinese Materia Medica
基金
国家自然科学青年科学基金项目(81102786)