Determination of Jujuboside A,Jujuboside B and Spinosin in Semen Ziziphi Spinosae by LC-MS/MS

Objective To develop a LC-MS/MS method for the determination of jujuboside A,jujuboside B and spinosin in Semen Zizyphi Spinosae.Methods The column was Phenomenex Gemini C18(50 mm × 2.0 mm,5 μm),mobile phase consisted of methanol: 5 mmol/L ammonium formate-0.1% formic acid buffer at a flow rate of 0.25 mL/min.The temperature of column was 40 ℃.The LC-MS/MS system was operated by using an electrospray ionization probe in the negative ion mode.Scan mode was in multiple reaction ion monitoring(MRM)mode.The mass charge ration of ion(m/z) was 1251.9→1251.9 for jujuboside A,1089.9→1089.9 for jujuboside B and 607.3→427.1 for spinosin,respectively.Results The linear ranges of jujuboside A,jujuboside B and spinosin were 50 ～ 1000 ng·mL-1,25 ～ 500 ng·mL-1 and 12.5 ～ 500 ng·mL-1,respectively.The lowest limit of quantification(LOQ) of jujuboside A,jujuboside B and spinosin was 5 ng·mL-1,2.5 ng·mL-1and 0.5 ng·mL-1(S/N3),respectively.The average recovery was 99.35 % ～ 101.10%,and RSD 5.01 %(n=9).The average content of jujuboside A,jujuboside B and spinosin in three batches of Semen Zizyphi Jujubae was in the range of 1.28 ～ 1.38 mg·g-1,1.02 ～ 1.11 mg·g-1 and 1.05 ～ 1.24 mg·g-1,respectively.Conclusion A sensitive,accuracy and suitable LC-MS/MS method has been developed,and the method can be applied for the detemination of jujuboside A,jujuboside B and spinosin in Semen Zizyphi Spinosae.