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目的:建立HILIC模式超高效液相色谱串联三重四级杆质谱法(HILIC-UPLC-MS/MS)同时测定酸枣仁中11种核苷及碱基类成分的含量。方法:采用Acquity UPLC BEH Amide色谱柱(2.1 mm×100 mm,1.7μm),配有Amide 1.7μm Van Guard保护柱,以10 mmol·L-1乙酸铵-0.8%乙酸水(A)和0.1%乙酸-乙腈(B)为流动相,梯度洗脱(0~5 min,10%A;5~7 min,10%~40%A),流速0.3 m L·min-1,柱温35℃,进样体积1μL,Waters XevoTMTQ质谱仪以多反应离子监测(MRM)方式,进行正离子检测。结果:所测成分在7 min内实现分离,各核苷及碱基类成分在0.002 32~8.66 mg·L~(-1)与峰面积呈良好的线性关系,相关系数均>0.992 2;加样回收率(n=6)为92.1%~108.2%,RSD均<7%。各批次各核苷及碱基类成分的含量具有一定的差异。10批样品总核苷及碱基类质量分数在24.5~48.48μg·g-1,其中以10号样品含量最低,2号样品最高。各种核苷类成分中,尿苷含量最高(平均值14.84μg·g-1),胸苷质量分数最低(平均值0.14μg·g-1)。结论:该方法具有简便、快速、重复性好,专属性强等特点,适用于酸枣仁中核苷及碱基类成分的快速定量分析。
OBJECTIVE: To establish a HILIC-UPLC-MS / MS method for the simultaneous determination of 11 nucleosides and bases in wild jujube. METHODS: The Amide 1.7 μm Van Guard column was used with Acquity UPLC BEH Amide column (2.1 mm × 100 mm, 1.7 μm). The column was eluted with 10 mmol·L -1 ammonium acetate-0.8% acetic acid in water (A) and 0.1% The mobile phase consisted of acetic acid and acetonitrile (B) with gradient elution (0-5 min, 10% A; 5-7 min, 10% -40% A) at a flow rate of 0.3 m L · min- Injection volume of 1μL, Waters XevoTMTQ mass spectrometer multi-reactive ion monitoring (MRM) mode for positive ion detection. Results: The components were separated within 7 min. The linear relationship between the nucleotide and base components of 0.002 32 ~ 8.66 mg · L ~ (-1) and peak area was obtained, the correlation coefficients were all> 0.992 2. The average recovery (n = 6) was 92.1% -108.2% with RSD <7%. Each batch of nucleoside and base class composition content has a certain difference. The total nucleosides and bases of 10 batches of samples were in the range of 24.5-48.48 μg · g-1, of which the content of 10 samples was the lowest and that of sample No. 2 was the highest. Among all kinds of nucleosides, uridine was the highest (average 14.84μg · g-1) and thymidine was the lowest (average 0.14μg · g-1). Conclusion: The method is simple, rapid, reproducible and specific. It is suitable for rapid quantitative analysis of nucleosides and bases in wild jujube kernels.