ABSTRACT
Objective: To develop an HPLC-MS/MS method for the simultaneous determination of forsythoside A, phillyrin, forsythiaside, rutin, quercetin, isoquercitrin, ferulic acid, and hesperidin in the seed of Forsythia suspense (Thunb.) Vahl. Methods: Chromatographic separation was performed on a Diamonsil C18 column (150 mm × 4.6 mm, 5 μm) with linear gradient elution of methanol and 0.1% formic acid at a flow rate of 800 μL/min, and the injection volume was 10 μL. Multiple-reaction monitoring (MRM) was employed with switching electrospray ion source polarity in negative mode. The ion spray voltage was set at-4 500 V and the turbo spray temperature was maintained at 650℃. Results: All calibration curves showed good linearity within the test ranges. The average recoveries of the compounds ranged from 98.1% to 101.8%. The precisions (RSD) for the investigated components were less than 0.84%. The contents of forsythoside A, phillyrin, forsythiaside and rutin are higher than quercetin, isoquercitrin, ferulic acid and hesperidin. And the average contents of forsythoside A, phillyrin, forsythiaside and rutin are 1 609.78, 80.08, 86.64 and 373.86 μg/g, respectively. Conclusion: An efficient, rapid, and sensitive method is first established for the qualitation and quantification of eight major components in the seed of Forsythia suspense (Thunb.) Vahl. The satisfactory results demonstrate that the method could be applied as a reliable quality control method for the seed of Forsythia suspense (Thunb.) Vahl.
ABSTRACT
Objective: To develop an HPLC-MS/MS method for the determination of jujuboside A, jujuboside B, spinosin, betulinic acid, betulin, rutin, apigenin, hesperidin, and naringin in Ziziphi Spinosae Semen. Methods: Analysis was performed on a Sapphire C18 column (150 mm × 4.6 mm, 5 μm) eluted with acetonitrile and 0.1% methanoic acid solution containing 1 mmol/L ammonium acetate in a gradient program. The flow rate was 1 mL/min, the injection volume was 10 μL, and the column temperature was 30℃. The multiple-reaction monitoring scanning (MRM) was employed for the quantification with switching electrospray ion source polarity in negative mode. The ion spray voltage was set at -4 500 V and the turbo spray temperature was maintained at 650℃. Results: The regression equations showing linear relationships between peak areas and contents of each compound were obtained. The average recoveries of the compounds ranged from 98.04% to 101.5% and the precision in terms of RSD was in the range of 0.03%-0.74%. Conclusion: The method is simple, rapid, and sensitive. It could be used as a quantitative determination method for the nine components in Ziziphi Spinosae Semen.