超高效液相色谱串联质谱法测定小麦籽粒中麦黄酮

Determination of Tricin in Wheat Grain by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

麦黄酮是小麦中主要的黄酮类化合物,是重要的天然活性物质。应用超高效液相色谱串联质谱法(UPLC-MS/MS),采用大气压电喷雾离子源,负离子模式,多反应检测(MRM)定性离子对m/z329.4/299.3和定量离子对329.4/314.3,精确测定了小麦籽粒中麦黄酮含量。小麦籽粒中麦黄酮用甲醇超声提取10 min,离心,重复3次,合并上清液,定容,过0.22μm的微孔滤膜待测。结果表明:麦黄酮在1.0～50.0μg/L范围内线性良好,r>0.99。方法检出限为1.2μg/kg。本方法具有灵敏、快速、准确等特点,可用于小麦籽粒中麦黄酮含量的测定。

Tricin （5,7,4＇-trihydroxy 3＇, 5＇-dimethoxyflavone） was observed to be the dominant flavone pigment in wheat. A specific ultra performance liquid chromatography-mass spectrometric method was devel- oped for the determination of tricin in wheat grain. The electrospray ionization was operated in negative ion mode, multiple reaction monitoring （MRM） mode with the primary transitions monitoring of m/z 329.4/ 314.3, and the secondary transitions monitoring of m/z 329.4/299.3. Tricin was extracted by ultrasonically assisted extractions（UAEs） with methanol and sonicated for 10 min in whole wheat meal. The supernatant was recovered by centrifugation. After extracting three time, the combined supernatant were evaporated in vacu- um. Residues were redissolved in HPLC grade methanol and filtered through a 0.22 μm micro filter（ Milli- pore）. The results show that the standard curve of tricin was linear line in the concentration of 1. 0 - 50.0 μg/L, the correlation coefficient （r） was higher than 0.99. The detection limit of the method was 1.2 μg/kg. The assay method was sensitive , accurate, fast and suitable to determine the triein in wheat grain.