Simultaneous quantification of nine constituents in Ziziphi Spinosae Semen by HPLC-MS / 中草药

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.