超高压液相色谱-四级杆-轨道阱质谱同时测定苦荞酒中的甜菜碱与葛根素

目的 建立苦荞酒中甜菜碱与葛根素的超高压液相色谱-四极杆-轨道阱质谱检测方法。方法 苦荞酒经0.22 μm滤膜过滤、流动相(甲醇〖DK〗∶水=50〖DK〗∶50)稀释后,以C18柱(100 mm×2.1 mm,1.8 μm)分离甜菜碱和葛根素。四极杆和轨道阱质谱检测,使用ESI源,一级与二级质谱同时检测。结果 甜菜碱与葛根素达到良好分离,在100 μg/L~2 000 μg/L范围内线性良好,相关系数均大于0.999。不同水平的加标回收率在96.7%~98.3%之间,相对标准偏差均小于2%。甜菜碱仪器检出限和定量限分别为0.5 μg/L和2.0 μg/L。葛根素仪器检出限和定量限分别为2.0 μg/L和5.0 μg/L。结论 该方法快速、同时、准确,适用于苦荞酒中甜菜碱与葛根素的测定。

Determination of betaine and puerarin in buckwheat wine by ultra-high pressure liquid chromatography-quadrupole orbitrap mass spectrometry

Objective To establish an analytical method for simultaneous determination of betaine and puerarin in buckwheat wine.Method Buckwheat wine was filtered by 0.22 μm filter membrane and diluted by mobile phase(methanol:water=50〖DK〗∶50),then betaine and puerarin were determined by ultra-high pressure liquid chromatography-quadrupole orbitrap mass spectrometry(ESI source)in full scan and MS2 mode.Results A good linear relationship( r >0.999)was observed with betaine and puerarin concentrations from 100 μg/L to 2 000 μg/L.The average recoveries at different levels of betaine and puerarin ranged from 96.7 % to 98.3 % with the relative standard deviations(RSD, n =3)all smaller than 2%.The limits of detection(LOD,S/N=3)and the limits of quantification(LOQ,S/N=10)for betaine were 0.5 μg/L and 2.0 μg/L.The LOD and LOQ for puerarin were 2.0 μg/L and 5.0 μg/L.Conclusion This method is rapid,simultaneous and accurate.It is suitable for the determination of betaine and puerarin in the buckwheat wine.