Simultaneous determination of 11 components in Gengnianning by HPLC-MS/MS
Objective:To establish an HPLC-MS/MS method for simultaneous determination of 11 components(harpagide,salidroside,nuezhenide,lobetyolin,wedelolactone,harpagoside,vaccarin,6-gingerol,atractylenolide Ⅲ,atractylenolide Ⅱ,and atractylenolide Ⅰ)in Gengnianning.Methods:HPLC assay was performed on C18 column(100 mm ×2.1 mm,1.9 μm)with a mixture of methanol and 0.1％formic acid as the mobile phase in gradient elution at a flow rate of 0.3 mL·min-1.The column temperature was 25 ℃ and the injection volume was 1 μL.Detection was carried out on a triple quadrupole mass spectrometer in positive ion mode(harpagide,salidroside,nuezhenide,lobetyolin,wedelolactone and harpagoside)and negative ion mode(vaccarin,6-gingerol,atractylenolide Ⅲ,atractylenolide Ⅱ,and atractylenolide Ⅰ)using an electrospray ion source(ESI).Multiple reaction monitoring(MRM)mode was employed.Results:The calibration curves were lin-ear within the ranges of 1.485-29.71 μg·mL-1,1.620-32.40 μg·mL-1,7.801-156.0 μg·mL-1,0.518-10.35 μg·mL-1,0.167-3.333 μg·mL-1,0.359-7.179 μg·mL-1,1.455-29.10 μg·mL-1,1.520-30.40 μg·mL-1,0.160-3.205 μg·mL-1,0.143-2.864 μg·mL-1 and 0.157-3.136 μg·mL-1 for harpagide,salidroside,nuezhenide,lobetyolin,wedelolactone,harpagoside,vaccarin,6-gingerol,atracty-lenolide Ⅲ,atractylenolide Ⅱ,and atractylenolide Ⅰ,respectively.All 11 components showed good linearity(r≥0.998 0).The average recoveries(n=6)were in the range of 95.9％-102.6％with RSDs within 0.90％-3.0％.The contents of harpagide,salidroside,nuezhenide,lobetyolin,wedelolactone,harpagoside,vaccarin,6-gingerol,atractylenolide Ⅲ,atractylenolide Ⅱ and atractylenolide Ⅰ in 10 tested samples from 5 manufactures were 14.8-104.5,37.6-288.5,335.8-1 332.8,6.2-10.1,6.6-61.8,13.7-75.1,57.4-132.8,16.9-70.6,11.8-33.9,3.4-15.4 and 6.5-12.9 μg·g-1.Conclusion:The developed method is accurate and sensitive.It can be used in quality control of Gengnianning.
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