摘要
目的：建立UPLC-MS同时测定大鼠组织中黄连生物碱类成分的分析方法,研究黄连生物碱类成分在大鼠体内的组织分布特征。方法：以延胡索乙素为内标,组织样品经乙酸乙酯萃取后进行UPLC-MS分析。色谱柱为Waters BEHC18（2.1 mm×100 mm,1.7μm）,流动相为0.2%的甲酸水-乙腈,梯度洗脱,流速为0.2 m L/min。正离子检测模式,选择的检测离子质荷比分别为：降氧化北美次碱m/z 191.904/118.973,8-氧黄连碱m/z 335.877/308.072,盐酸巴马汀m/z 351.94/294.554,表小檗碱m/z 335.94/262.112,非洲防己碱m/z 337.94/322.422,黄连碱m/z 319.904/292.037,延胡索乙素m/z 355.977/192.036,盐酸小檗碱m/z 335.94/320.036,氧化小檗碱m/z351.94/321.995,药根碱m/z 337.94/322.949。结果：在大鼠不同组织中,9个生物碱成分在测定的线性范围内线性关系良好（r＆0.9901）;方法的精密度RSD小于15%,准确度和稳定性均在±15%以内,提取回收率在72.1%~82.9%之间,RSD≤15%。黄连碱、表小檗碱、小檗碱、药根碱、非洲防己碱、巴马汀成分在大鼠体内分布广泛,降氧化北美次碱、8-氧黄连碱、氧化小檗碱仅在肝及心/肾中检测到。结论：本实验建立的方法简便易行、准确可靠,应用于检测大鼠体内生物碱类成分的组织分布研究是可行的。
Objective： To develop an UPLC-MS method for simultaneous determination of alkaloids from Coptidis Rhizoma in rat tissues,and to study the tissue distribution of alkaloids from Coptidis Rhizoma in rats. Methods： The samples were extracted with ethyl acetate,and analyzed by UPLC-MS with acetonitrile-0. 2% formic acid solution in a gradient elution mobile phase,the flow rate was 0. 2m L/min. Tetrahydropalmatine was used as an internal standard. The mass spectrometer was operated in selected reaction monitoring（ SIM） mode with positive electrospray ionization,the transition were m/z 191. 904 /118. 973（ noroxyhydrastinine）,m/z 335. 877 /308. 072（ 8-ocoptisine）,m/z 351. 94 /294. 554（ palmatine chloride）,m/z 335. 94 /262. 112（ epiberberine）,m/z 337. 94 /322. 422（ columbamine）,m/z 319. 904 /292. 037（ coptisine）,m/z 355. 977 /192. 036（ tetrahydropalmatine）,m/z 335. 94 /320. 036（ berberine hydrochloride）,m/z 351. 94 /321. 995（ oxyberberin）,m/z 337. 94 /322. 949（ jatrorrhizine respectively）. Results： Excellent linearity was observed in all alkaloids in their linear range（ r 0. 9901）. The RSD of precision of the developed method was less than 15%,and the accuracy and stability were less than ± 15%,the extraction recovery was 72. 1% ~ 82. 9% with RSD less than 15%. Coptisine,epiberberine,berberine,jatrorrhizine,columbamine,palmatine were widely distributed in rat tissues. Noroxyhydrastinine,8-ocoptisine,oxyberberin could only be determined in liver and heart or kidney. Conclusion： The established method is simple and accurate. Satisfactory results are obtained with applying this method to the tissue distribution study of alkaloids from Coptidis Rhizoma.
出处
《中药材》
CAS
CSCD
北大核心
2016年第8期1849-1853,共5页
Journal of Chinese Medicinal Materials
基金
国家自然科学基金(81403114)
江苏省高校优势学科建设工程资助项目(中药学优势学科资助)
2014年南京中医药大学大学生实践创新训练计划资助项目
2015江苏省大学生实践创新训练计划资助项目
