Determination of Six Alkaloids in Tianma Capsule by UHPLC-MS/MS
OBJECTIVE To establish an UHPLC-MS/MS method for the determination of six alkaloids in Tianma capsule.METHODS Phenomenex Kinetex C18(2.1 mm × 100 mm,2.6 μm)column was used for separation.The mobile phase consisted of methanol and 0.1％formic acid(containing 2.5 mmol·L-1 ammonium acetate)solution(gradient elution).The flow rate was 0.3 mL·min-1 and the column temperature was maintained at 35 ℃.Electrospray positive ion source was used for mass spectrometry detection by multiple reaction monitoring mode.RESULTS The liner range of calibration curve was 79.38-3 969 ng·mL-1(r=0.999 9),18.60-929.8 ng·mL-1(r=0.999 8),38.20-1 910 ng·mL-1(r=0.999 9),1.264-252.8 ng·mL-1(r=0.999 3),1.196-239.2 ng·mL-1(r=1.000 0)and 1.268-253.6 ng·mL-1(r=1.000 0)for benzoylmesaconine,benzoy-laconine,benzoylhypaconine,mesaconitine,hypaconitine and aconitine.The RSD of repeatability test(content)was 0.5％-3.2％.The average recoveries was in the range of 98.3％-105.3％.RSD was 1.0％-3.4％.CONCLUSION The method has good sprcificity,sensitivity and accuracy,and it is suitable for the analysis of six alkaloids in Tianma capsule.
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