ABSTRACT
AIM To establish an HPLC method for the content determination of six constituents in Shiyifang Vinum (Notoginseng Radix et Rhizoma,Dipsaci Radix,Carthami Flos,etc.).METHODS The content determination of notoginsenoside R1,ginsenoside Rg1,ginsenoside Rb1 and asperosaponin Ⅵ was performed on a 30℃ thermostatic Inertsil(R) ODS-3 C18column (4.6 mm ×250 mm,5 μm),with the mobile phase comprising of acetonitrile-0.1％ phosphoric acid flowing at 1.0 mL/min in a gradient manner,and the detection wavelength was set at 203 nm.The content determination of brucine and strychnine was conducted on a 30 ℃ thermostatic Geminni(R) C18 110(A) column (4.6 mm × 250 mm,5 μm),with the mobile phase comprising of acetonitrile-mixed solution of 0.01 mol/L sodium heptanesulfonate and 0.02 mol/L potassium dihydrogen phosphate flowing at 1.0 mL/min in an isocratic elution manner,and the detection wavelength was set at 260 nm.RESULTS Six constituents showed good linear relationships within their own ranges (r ＞ 0.999 0),whose average recoveries were 98.52％-99.96％ with the RSDs of 2.0％-2.3％.CONCLUSION This simple,accurate and reproducible method can be used for the quality control of Shiyifang Vinum.
ABSTRACT
Objective:To develop a determination method for strychnine and brucine in Shiyifang vinum by LC-MS/MS. Meth-ods:The samples were separated on an Agilent Zorbax SB-C18column(2.1 mm×100 mm,3.5 μm). The mobile phase was metha-nol-10 mmol·L-1ammonium formate solution (adjusting pH to 3.0 with methane acid)(25: 75), and the flow rate was 0.2 ml· min-1. The eletrospray ionization( ESI) with positive source of the mass spectrometer and multiple reaction monitor( MRM) mode were used to detect strychnine(m/z 395.2→243.8;m/z 395.2→212.8)and brucine(m/z 335.2→183.9;m/z 335.2→155.9). Re-sults:The linear range of strychnine was 0.242-7.733 μg·ml-1,and that of brucine was 0.302-9.661 μg·ml-1. The average re-covery was 100.1% (RSD=0.8%,n=6) and 99.4% (RSD=1.4%,n=6),respectively. Conclusion:The method is simple and accurate,which can be used to determine the contents of strychnine and brucine in Shiyifang vinum.