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目的研究适于液相色谱-电喷雾串联质谱法(LC-MS/MS)定量测定富硒葱蒜类植物中Se-甲基-硒半胱氨酸(MSeC)的提取液的最佳制备条件。方法用4种提取剂(纯水、甲醇、丙酮和乙酸乙酯)、2种提取方法(超声提取和沸水提取)、不同水提取温度(70、80、90和100℃)和时间(45、60、75和90min)对富硒大蒜中的MSeC的最佳提取条件依次筛选研究,获得满足最大量测得MSeC的样品制备方法。按照选择条件提取洋葱、韭葱和大葱加标粉制剂,并采用LC-MS/MS测定MSeC含量,计算加标回收率。结果4种提取剂的超声提取对比分析发现,纯水提取蒜粉中MSeC的量最大,沸水浴加热比单独超声处理能够提高蒜粉中MSeC的提取率。水加热提取温度和时间二因素正交设计优选实验证实,蒜粉中MSeC最佳提取制备条件为100℃提取90min,该提取条件处理其他葱蒜类粉制剂的MSeC加标回收率在91%～108%之间。结论沸水提取90min适用于LC-MS/MS在线定量分析葱蒜类植物中MSeC的待测液的制备。
Objective To study the optimum conditions for the determination of Se-methyl-selenomethionine (MSeC) extract in Se-enriched garlic plants by liquid chromatography-electrospray ionization tandem mass spectrometry (LC-MS / MS) . Methods Four extraction methods (pure water, methanol, acetone and ethyl acetate), two extraction methods (ultrasonic extraction and boiling water extraction), different water extraction temperature (70,80,90 and 100 ℃) and time (45, 60, 75 and 90 min), the optimal extraction conditions for MSeC in Se-enriched garlic were selected and studied in order to obtain the sample preparation method that satisfied the maximum MSeC measurement. Onion, leek and green onions were extracted according to the selection conditions, and the MSeC content was determined by LC-MS / MS. The spiked recoveries were calculated. Results The ultrasonic extraction of four kinds of extractants showed that MSeC was the most abundant in garlic powder extracted by pure water, and the extraction rate of MSeC in garlic powder could be increased by boiling water bath heating compared with ultrasonic treatment alone. Water heating extraction temperature and time two-factor orthogonal design optimization experiments confirmed that the MSeC optimal extraction of garlic powder preparation conditions for the extraction of 100 ℃ 90min, extraction conditions for other onion garlic MSeC spiked recovery of 91% 108% between. Conclusion The boiling water extraction 90min is suitable for the on-line quantitative determination of MSeC in onion and garlic plants by LC-MS / MS.