摘要
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 method of high performance liquid chromatography-electrospray ionization-mass spectrometry （HPLC-ESI-MS） was developed for the determination of the content of polysaccharide in Ganoderma capsule and the monosaccharide components. The conditions of polysaccharide hydrolysis of monosaccharides and 1-phenyl-3- methyl-5-pyrazolone （PMP） derivatization were investigated. Ganoderma lucidum polysaccharides were completely hydrolyzed to monosaccharides in 0.5 mol/L trifluoroacetic acid （TFA）, the hydrolysis temperature was set as 70 ℃, and hydrolysis time was optimized to be 30 min. The derivative of the double molecule PMP was obtained from the PMP derivatization, which was carried out at 70℃ for 30 min and followed by cooling down at 4℃. The linear equations of the 5 hydrolyzed monosaccharides were obtained in the range of 0.1 -50 mg/L. The limits of detection （S/N ≥ 3 ） were 0. 025 mg/L, and the recoveries were 95% - 105%, respectively. The relative standard deviations （RSD） were in range of 0.5% 0 3.5%. The established method has high specificity and sensitivity, and can meet the determination requirement for quality control in Ganoderma lucidum capsule.
出处
《分析试验室》
CAS
CSCD
北大核心
2016年第11期1285-1289,共5页
Chinese Journal of Analysis Laboratory
基金
东莞市社会科技发展项目(2013108101032)
广东省公益研究与能力建设专项资金项目(2014A020212692)
东莞市高等院校
科研机构科技计划一般项目(2014106101006)资助
关键词
灵芝胶囊
多糖
三氟乙酸
1-苯基-3-甲基-5-吡唑啉酮
高效液相色谱-质谱法
Ganoderma lucidum capsule
Polysaccharide
Trifluoroacetic acid
1 -phenyl-3-methyl-5-pyrazolone
High performance liquid chromatography mass spectrometry
