Zhang Yuan-Jiao, Hu Peng, Ma Yun, Cai Jing, Li Yue, Li Xiang, Chen Jian-Wei
Nanjing University of Chinese Medicine, Nanjing 210023, China.
Zhongguo Zhong Yao Za Zhi. 2017 Mar;42(6):1152-1159. doi: 10.19540/j.cnki.cjcmm.20170121.003.
A comprehensive analytical method based on UFLC-QTRAP-MS-MS was developed for the simultaneous determination of 15 kinds of amino acids and 12 kinds of nucleosides of three species in Termitomyces. The separation was carried out on a Waters XBridge Amide column (2.1 mm×100 mm,3.5 μm) with gradient elution of mobile phase of 0.2% formic acid in water-0.2% formic acid in acetonitrile at a flow rate of 0.6 mL•min⁻¹, and column temperature was maintained at 30 ℃. The target compounds were analyzed by the positive ion multiple reaction monitoring (MRM) mode. The principal component analysis(PCA) was made to standardized treatment for the comprehensive evaluation of different species in Termitomyces. The 15 kinds of amino acids and 12 kinds of nucleosides multiple constituents showed good linearity (r>0.997 3) in the range of the tested concentration.The average recoveries ranged from 95.14% to 105.0%,and the relative standard deviations were less than 5.0%. The comprehensive evaluation index obtained with PCA showed that the Termitomyces albuminosus was significantly higher than others in amino acids and in nucleosides, of which the T. aurantiacus was the best. The developed method with good repeatability and accuracy was suitable for the simultaneous determination of multiple functional substances,which provided a new basis for the comprehensive assessment and overall control of the quality of Termitomyces fungi.
建立了一种基于超高效液相色谱-串联四极杆飞行时间质谱（UFLC-QTRAP-MS-MS）的综合分析方法，用于同时测定鸡枞菌三种菌株中的15种氨基酸和12种核苷。分离在Waters XBridge酰胺柱（2.1 mm×100 mm，3.5μm）上进行，流动相为水相0.2%甲酸-乙腈相0.2%甲酸梯度洗脱，流速为0.6 mL•min⁻¹，柱温保持在30℃。目标化合物采用正离子多反应监测（MRM）模式进行分析。通过主成分分析（PCA）对数据进行标准化处理，以综合评价鸡枞菌不同菌株。15种氨基酸和12种核苷多种成分在测试浓度范围内线性关系良好（r>0.997 3）。平均回收率在95.14%至105.0%之间，相对标准偏差小于5.0%。PCA得到的综合评价指标表明，鸡枞菌在氨基酸和核苷方面显著高于其他菌株，其中橙盖鸡枞菌表现最佳。所建立的方法具有良好的重复性和准确性，适用于多种功能物质的同时测定，为鸡枞菌质量的综合评价和全面控制提供了新依据。
