摘要
目的建立同时测定硒蛋氨酸(SeMet)和硒胱氨酸(SeCys)含量的液相色谱-串联质谱法(LC-MS-MS)。方法色谱柱:Waters Symmetry C18(150mm×3.9mm,5μm);流动相:甲醇+0.1%七氟丁酸水溶液(35+65),流速为500μl/min;以氮气为碰撞气,利用多反应离子监测方式测定SeMet(MRMm/z198.1→181.0,198.1→152.0)和SeCys(MRMm/z337.0→248.0,337.0→88.2)信号。结果SeCys和SeMet检出限分别为2.0ng/ml和0.5ng/ml;以198.1→181.0为定量分析离子对,SeMet的线性回归方程为:y=707x+990,r=0.9993;以337.0→248.0为定量分析离子对,SeCys的线性回归方程为:y=64.3x+695,r=0.9999。结论该方法能够使2种含硒化合物在一次进样中实现完全分离和在线测定,能够满足快速准确检测SeCys和SeMet含量要求。
Objective To establish the method of liquid chromatography-tandem mass spectrometry （LC - MS - MS） in order to determine selenoeystine （SeCys） and selenomethionine （SeMet）. Method The chromatographic column was Waters Symmetry C18 （ 150 mm× 3.9 mm, diameter 5 μm）. The mobile phase was methanol ＋ 0.1% heptafluorobutyric acid （35 ＋ 65 ） at a flow rate of 500μl/min. SeMet and SeCys were detected by monitoring the ion transition of m/z 198.1→181.0, 198.1→152.0 and 337.0→248.0, 337.0→88.2, with nitrogen as collision gas and using multiple reaction monitoring （MRM） mode. Results The determination limits of SeCys and SeMet were 2.0 and 0.5 ng/ml, respectively. The linear regression equations of SeMet and SeCys were y = 707x ＋ 990, r = 0.999 3 and y = 64.3x ＋ 695, r = 0.999 9, respectively. Conclusion SeMet and SeCys could be completely separated and determined for on-line in one injection by this method. The method could meet requirements of fast and accurate determination of SeMet and SeCys.
出处
《中国食品卫生杂志》
2008年第3期204-207,共4页
Chinese Journal of Food Hygiene
基金
国家自然科学基金项目(No·30471454,30170800)
关键词
硒化合物
色谱法
高压液相
光谱法
质量
电喷雾电离
Selenium Compounds
Chromatography, High Pressure Liquid
Spectrometry, Mass, Electrospray Ionization
