核磁共振氢谱定量检测3 种食用菌麦角固醇

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δ 0.63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。

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

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-18H 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.