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建立高分离度快速液相色谱质谱联用(UFLC-QTRAP-MS-MS)同时测定蚁巢伞属3种鸡(土从)中15种氨基酸和12种核苷类成分的方法。采用Waters XBridge Amide色谱柱(2.1 mm×100 mm,3.5μm),流动相为0.2%甲酸水-0.2%甲酸乙腈,梯度洗脱,柱温30℃,流速0.6 mL·min~(-1),采用电喷雾正离子源(ESI+),多反应离子监测(MRM)模式进行检测。采用PCA主成分分析法对不同品种的蚁巢伞属鸡(土从)进行综合评价。结果 15种氨基酸成分和12种核苷成分在一定浓度范围内均呈良好的线性关系,相关系数均大于0.997 3,精密度,重复性和稳定性良好;加样回收率在95.14%~105.0%,RSD均小于5.0%。PCA分析显示在氨基酸中,鸡(土从)综合评价指数分最高;在核苷中,黄鸡(土从)综合评价指数最高。所建立的方法准确、重复性好,可用于蚁巢伞属3种鸡(土从)中15种氨基酸和12种核苷类成分的同时测定,为蚁巢伞属鸡(土从)资源内在质量的综合评价、全面控制以及合理开发应用提供新的方法参考。
A method for the simultaneous determination of 15 kinds of amino acids and 12 kinds of nucleosides in three species of Antarctica from soil by UFLC-QTRAP-MS-MS was established. The mobile phase consisted of 0.2% formic acid and 0.2% formic acid in a mobile phase using a Waters XBridge Amide column (2.1 mm × 100 mm, 3.5 μm). The mobile phase consisted of gradient elution at 30 ℃ with a flow rate of 0.6 mL · min -1. Electrospray positive ionization (ESI +) and multi-reactive ion monitoring (MRM) were used for detection. PCA principal component analysis of different varieties of Antarctic chicken (soil from) a comprehensive evaluation. Results The 15 kinds of amino acids and 12 kinds of nucleosides showed a good linear relationship in a certain range of concentration with the correlation coefficients above 0.997 3. The precision, repeatability and stability were good. The recoveries ranged from 95.14% to 105.0% , RSD less than 5.0%. PCA analysis showed that among amino acids, chicken (soil from) the highest comprehensive evaluation index; in nucleosides, yellow chicken (soil from) the highest comprehensive evaluation index. The established method is accurate and reproducible, and can be used for the simultaneous determination of 15 kinds of amino acids and 12 kinds of nucleoside constituents in 3 species of Antarctica, Quality comprehensive evaluation, comprehensive control and rational development and application of new methods for reference.