摘要
目的建立高效液相色谱-紫外-串联质谱法同时测定痹祺胶囊(马钱子、川芎、甘草、丹参、白术、三七、党参等)中7个有效成分的方法。方法采用HPLC法,Zorbax-C18色谱柱(4.6 mm×100 mm,1.8μm);流动相乙腈-0.1%甲酸水溶液梯度洗脱;体积流量0.5 mL/min;进样5μL;DAD波长切换模式;柱温40℃。Finnigan电喷雾离子阱多级质谱仪,正/负离子检测模式;ESI喷雾电压±4.5 kV;鞘气(N2)压力为276 kPa;辅助气(N2)体积流量为3.3 L/min;毛细管温度350℃;毛细管电压±19 V;扫描范围m/z 100～850 amu。结果士的宁、马钱子碱、甘草苷、丹酚酸B、甘草酸、隐丹参酮和丹参酮IIA在相应的质量浓度范围内与峰面积呈良好的线性关系,相关系数均大于0.999 6;平均加样回收率(n=6)在90.25%～99.11%之间,RSD均小于2.91%。结论本方法简便快捷、精密度高、重复性好,适用于痹祺胶囊的质量控制。
AIM To establish a method for simultaneously determining seven active components in Biqi Capsules （Strychni Semen, Chuanxiong Rhizoma, Glycyrrhizae Radix et Rhizoma, Salviae miltiorrhizae Radix et Rhizoma, Atractylodis macrocephalae Rhizoma, Notoginseng Radix et Rhizoma, Codonopsis Radix, etc. ） by high performance liquid chromaography tandem mass spectrometer. METHODS The chromatographic separation was car- ried out on a Zorbax-C18 （4.6 mm × 100 mm, 1.8 um） column by using the mobile phase composed of acetonitrile and 0. 1% formic acid aqueous solution in a gradient elution. The switched wavelength of DAD was employed. The column temperature was set at 40℃. The flow rate was 0. 5 mL/min. The mass spectra were obtained by Finnigan LCQ Deca XPCUSion trap mass spectrometer. The positive and negative ion mode were converted to detect the seven compounds. Ion spray voltage was ＋ 4. 5 kV. Sheath gas （ N2） pressure was 276 kPa, and auxiliary gas （ N2） flow rate was 3.3 L/rain. Capillary temperature was maintained at 350℃. Capillary voltage was ＋ 19 V, and mass range recorded in m/z 100 to 850. RESULTS Strychnine, brucine, liquiritin, salvianolic acid B, gly- cyrrhizic acid, cryptotanshinone and tanshinone IIA showed good linearity in the tested ranges （r≥0. 999 6）. The average recoveries varied from 90. 25% to 99. 11% with RSDs ≤2. 91%. CONCLUSION This method is simple, expeditious, accurate and reproducible, and can be used for quality control of Biqi Capsules.
出处
《中成药》
CAS
CSCD
北大核心
2012年第8期1492-1496,共5页
Chinese Traditional Patent Medicine
基金
国家“重大新药创制”科技重大专项(2009ZX09301-008)
