摘要
目的综合运用多维联用技术,建立日本救心丹HPLC-UV/ELSD和HPLC-UV/MS3指纹图谱研究方法,初步阐明其化学物质基础。方法A ltim a C18色谱柱(250 mm×4.6 mm ID,5μm);流动相为乙腈-0.2%甲酸水体系;梯度洗脱;流速1.0 mL.m in-1;检测波长286 nm。ELSD条件为漂移管温度110℃,N2流速2.5 L.m in-1。采用电喷雾离子阱质谱分析,正、负离子三级扫描。结果建立了日本救心丹HPLC-UV/ELSD多维指纹图谱,同时通过MS定性鉴别出21种成分,并推测可能存在去氧苷胆酸及其异构体。方法稳定且重现性好。结论该研究为分析汉方中药复杂体系提供了一种有效、可靠的模式。
Aim To develop HPLC-UV/ELSD and HPLC-UV/MS3 fingerprints of Japan Jiuxin pill using multi-dimensional hyphenated methods and study on its chemical base. Methods Separation was performed on Altima C18 analytical column （250 mm × 4.6 mm ID, 5 μm）. The mobile phases consisted of water containing 0.2% formic acid and acetonitrile was used as gradient elute. The flow rate was 1.0 mL·min^-1. An electrospray ion trap mass spectrometer was utilized for qualitative analysis and both positive and negative secondary ion scan mode were applied. Results HPLC-UV/ELSD and HPLC-UV/ MS3 fingerprints of Japan Jiuxin pill with well separation and reproducibility were obtained. Totally 21 components in the complex formula were identified and the chemical structural information of glycocholic acid and its isomer were suggested. Conclusion The research is propitious to offer an effective and reliable pattern for analyzing Japanese Kampo Medicines as well as its quality control.
出处
《药学学报》
CAS
CSCD
北大核心
2006年第12期1161-1165,共5页
Acta Pharmaceutica Sinica
基金
国家科技攻关计划资助项目(2004BA721A13).
