超高效液相色谱—串联四极杆质谱法测定苦荞麦中黄酮类化合物

Determination of flavonoids in tartary buckwheat by UPLC-MS-MS

建立苦荞麦中芦丁、槲皮素和山萘酚含量的超高效液相色谱-串联四级杆质谱联用仪(UPLC-MS-MS)测定方法。试样用甲醇超声波提取,HSSC18超高效液相色谱柱、甲醇-水(0.1%甲酸)流动相分离,以电喷雾离子源负离子检测方式进行质谱分析,多反应监测(MRM)定量。结果表明,在0.1～100μg/mL范围内,芦丁、槲皮素、山萘酚浓度与峰面积均有良好的线性关系,相关系数r2均大于0.99。在低、中、高3个浓度添加水平下,三种物质的回收率均在94%以上,相对标准偏差在2.19～12.54范围内。芦丁检出限为0.01ng/mL,槲皮素、山萘酚检出限为0.1ng/mL。

The objective of this research was to establish a method for detecting Rutin, Quercetin and Kaempferol in tartary buckwheat by UPLC-MS-MS.Tartary buckwheat samples were extracted with methanol in a ultrasonic cleaner,and Rutin,Quercetin and Kaempferol were separated by a HSS C18 UPLC column, with methanol-0.1% formic acid as mobile phase, electrospray ionization was applied and operated in the negative ion mode, then quantified with multiple reaction monitoring （MRM）.Results：Good linearities were observed in the range from 0.1- 100μg/mL,with correlation coefficients above 0.99.The mean recoveries of three levels were all above 94% and the relative standard derivations were between 2.19 and 12.54.The detection limit of Rutin, Quercetin and Kaempferol were 0.0l .0.1 .0.1 ng/mL, resoectivelv.