核磁共振氢谱定量检测3种食用菌麦角固醇  

Quantitative Detection of Ergosterol in Edible Fungi by Nuclear Magnetic Resonance Spectroscopy

作　　者：傅利军 刘莉 张秀敏 马永征 孙勇 岳甜 徐明芳[2] FU Lijun;LIU Li;ZHANG Xiumin;MA Yongzheng;SUN Yong;YUE Tian;XU Mingfang(Beijing Academy of Food Science,Beijing 100068,China;College of Life Science and Technology,Jinan University,Guangzhou 510632,China)

机构地区：[1]北京食品科学研究院,北京100068 [2]暨南大学生命科学技术学院,广东广州510632

出　　处：《食品科学》2021年第20期135-144,共10页Food Science

基　　金：“十三五”国家重点研发计划重点专项(2018YFD0400202);广东省科技计划项目(2015A010107006)。

摘　　要：选择C-18H质子单峰作为麦角固醇的目标定量特征峰,氘代氯仿作为溶剂、吡嗪作为内标物,建立3种食用菌麦角固醇的定量检测方法。通过优化采样参数、采集时间、扫描次数和弛豫延迟时间核磁检测条件,确定δ0.63处的质子单峰C-18H作为麦角固醇的目标定量特征峰;经方法学评价,在0.55~5.30 mg/mg范围内,回归方程线性关系良好,相关系数R2为0.999 7,检出限和定量限分别为0.001 8 mg/mL与0.045 0 mg/mL;平均加标回收率为103.491 9%,方法的精密度与稳定性相对标准偏差均小于2%,食用菌样品检测验证该方法专属性,表明建立的方法对3种食用菌中麦角固醇定量检测具有快速准确的优势。A method for the quantitative determination of ergosterol in edible fungi was established by using deuterated chloroform as the solvent and pyrazine as the internal standard. The C-18 H proton single peak at δ 0.63 was selected as the target characteristic peak after optimizing the sampling parameters, acquisition time(AT), the number of scans(NS)and relaxation delay time(D1). The methodological evaluation results showed that the calibration curve was linear in the concentration range of 0.55–5.30 mg/mg with correlation coefficient(R2) of 0.999 7. The limit of detection and the limit of quantitation were 0.001 8 and 0.045 0 mg/mL, respectively. The relative standard deviation(RSD) values for precision and stability were both less than 2% and the average recovery of the added ergosterol was 103.491 9%. The specificity of the developed method was verified by applying it to detect three varieties of edible fungi samples, indicating that this method has the advantage of rapidity and accuracy.

关 键 词：核磁共振 定量检测 食用菌 麦角固醇 

分 类 号：O657.63[理学—分析化学] TS219[理学—化学]