液相色谱-电喷雾离子阱质谱对芥子碱的测定方法

Determination of sinapine by liquid chromatography-electrospray ion-trap mass spectrometry

探讨了采用液相色谱-电喷雾串联质谱法检测小鼠前列腺中芥子碱硫氰酸盐的方法。流动相为V（乙腈）∶V（0.5%乙酸）=20∶80,色谱柱为ZorbaxXDB-C18（150 mm×4.6 mmi.d.,5μm）,流速为0.6 mL/min。芥子碱硫氰酸盐的准分子离子和二级碎片离子分别为m/z 304和m/z 251,方法的检出限为0.7μg/L,线性范围为2.7～80.5μg/L,r为0.9934,相对标准偏差为7.5%～12.9%,样品的回收率为81.2%～102.5%。

In this paper, we developed a reversed-phase high performance liquid chromatography electrospray ionization tandem mass spectrometry for the determination of sinapine in rat plasma. The mixtures were successfully isolated on a Zorbax C18 column （150 × 4.6 mm i.d., 5μm）, using acetonitrile- 0.5% acetic acid （20：80, V/ V） as the mobile phase at a flow rate of 0.6 mL/min. It showed the quasimolecular ion and MS2 fragment ion of sinapine are m/z 304 and m/z 251. The limit of detection （LOD） was 0.7μg/L. The linear plots were obtained between 2.7 and 80.5μg/L and CV is 0.9934. Overall recoveries were between 81.2% - 102.5%. It is a rapid, sensitive and reproducible method.