论文部分内容阅读
建立了测定灵芝胶囊中多糖含量与单糖组分的高效液相色谱-电子喷雾离子源-质谱联用(HPLC-ESI-MS)检测方法,研究了灵芝多糖酸水解为单糖及1-苯基-3-甲基-5-吡唑啉酮(PMP)衍生化的条件,三氟乙酸(TFA)的浓度在0.5 mol/L、水解温度70℃、水解时间30 min时能将灵芝多糖完全水解为单糖,在70℃PMP衍生化反应30 min,4℃冷却,得到双分子PMP单糖衍生物。5种水解后的单糖线性范围为0.1~50 mg/L,检出限为25μg/L(S/N≥3),在3个加标水平(0.1,10,50 mg/g)下,5种单糖平均回收率为95%~105%,精密度(RSD)为0.5%~3.5%。方法能满足对灵芝胶囊质量控制的检测要求。
A HPLC-ESI-MS method for the determination of polysaccharide content and monosaccharide components in Ganoderma lucidum capsules was established. The hydrolysis of Ganoderma lucidum polysaccharides to monosaccharides and 1-benzene 3-methyl-5-pyrazolone (PMP) derivatization conditions, the concentration of trifluoroacetic acid (TFA) at 0.5 mol / L, hydrolysis temperature 70 ℃, hydrolysis time 30 min Ganoderma lucidum polysaccharide completely Hydrolysis of monosaccharides, PMP derivatization reaction at 70 ℃ 30 min, 4 ℃ cooling, to obtain bimolecular PMP monosaccharide derivatives. The linear range of the five monosaccharides after hydrolysis was 0.1-50 mg / L with the detection limit of 25μg / L (S / N≥3). Under the three spiked levels (0.1, 10 and 50 mg / g) The average recoveries of five kinds of monosaccharides were 95% ~ 105% and the precision (RSD) was 0.5% ~ 3.5%. The method can meet the detection requirements of Ganoderma capsule quality control.