建立了液相色谱串联质谱(LC-MS-MS)法测定青花菜中L-硒甲基硒代半胱氨酸(SeMC)含量的方法.植物样品经沸水提取,以甲醇-0.1%七氟丁酸水溶液 (30: 70)为流动相,滤液经Waters Symmetry C18(50 mm×3.9 mm,5 μm)分离,经在线电喷雾离子源(ESI)正离子化后,采用多反应离子监测方式(MRM)选择m/z 184.0→(167.0,94.9)测定SeMC.SeMC的线性范围为0~200 mg/L,准确度在96%~114%之间,日内日间精密度(RSD)在±10%内.检出限为0.1 mg/kg.结果表明:本方法高效、准确,特异性强,样品处理简单,可准确定量富硒青花菜中的SeMC.
A HPLC-MS/MS method was established for the determination of methylselenocysteine (SeMC) content in broccoli powder. Broccoli powder samples were extracted with deionized water at 100℃ for 1 hour, filtered through 0.2μm filter, and then separated on Waters Symmetry C18 ( 150 mm × 3.9 mm, 5 μm) column with methanol -0. 1% heptafluorobutyric acid (30:70, V/V) as mobile phase, at a flow rate of 500 μL/min. Electrospray ionization source (ESI) was applied and operated in positive ion mode, and multiple reactions monitoring (MRM) mode was adopted. SeMC was quantified by monitoring the: ion transition of m/z 184.0→( 167.0; 94.9). The linear calibration curves were obtained over the concentration range of 0 - 200 mg/L for SeMC . The lowest detection limit (S/N = 3 ) was 0.1 mg/kg for SeMC. The spiking recov- ery of SeMC varied between 96% - 114% with in 10% of inter-and intra-day precision (RSD).