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目的:建立液质联用技术同时测定不同产地淡豆豉中38种核苷和氨基酸类含量的方法。方法:采用超快速液相色谱和三重四极杆-线性离子阱串联质谱以及亲水色谱柱(2.1 mm×100 mm,3.5μm),流动相0.2%甲酸水-0.2%甲酸乙腈梯度洗脱,流速0.6 m L·min-1,采用电喷雾正离子化及多反应监测模式(MRM),对安徽、江苏、河南3个产区不同采收期共8个批次淡豆豉中的22种氨基酸类和16种核苷类成分进行含量测定;并对结果进行PCA-DA聚类分析及t检验。结果:所建方法使淡豆豉中22种氨基酸类和16种核苷类成分得到较好分离,浓度与峰面积呈良好的线性关系,加样回收率在93.74%~104.32%,RSD在0.6%~3.5%;8个批次样品基本可以测得22种氨基酸类和16种核苷类成分,各批次间核苷与氨基酸的含量都有明显差异,总氨基酸质量分数在7.241~34.21 mg·g-1,总核苷质量分数在14.21~82.53 mg·g-1;不同产地样品的氨基酸含量高低排序为安徽产>江苏产>河南产,不同产地样品的核苷含量高低排序为江苏产与安徽产>河南产,同一产地贮存时间短的样品总氨基酸和总核苷含量也高于贮存时间长的。结论:该方法适用于38种核苷和氨基酸类成分含量的同时测定,比较了不同产地淡豆豉的差异性,在一定程度上反应了不同产区间淡豆豉的质量优劣,为后续药效活性研究提供参考。
OBJECTIVE: To establish a method for the simultaneous determination of 38 nucleosides and amino acids in Diospyros currant by using liquid chromatography-mass spectrometry (LC-MS / MS). Methods: Ultra-fast liquid chromatography (LC-MS / MS) and triple quadrupole-linear ion trap tandem mass spectrometry were used. The mobile phase consisted of a mobile phase of 0.2% formic acid and 0.2% Flow rate of 0.6 m L · min-1, using electrospray positive ionization and multi-reaction monitoring mode (MRM), Anhui, Jiangsu, Henan, And 16 kinds of nucleosides. The results were analyzed by PCA-DA cluster analysis and t-test. Results: The results showed that 22 kinds of amino acids and 16 kinds of nucleosides were separated well, and the linear relationship was obtained between the concentration and the peak area. The recoveries were 93.74% -104.32%, RSD was 0.6% ~ 3.5%. The results showed that the content of nucleosides and amino acids in all batches was significantly different, with the total amino acids in the range of 7.241 ~ 34.21 mg · g-1, the total content of nucleosides was 14.21 ~ 82.53 mg · g-1. The order of amino acid content in samples from different areas was Anhui> Jiangsu> Henan. Anhui Province> Henan Province, the same place of storage short sample total amino acids and total nucleosides content is also higher than the storage time. Conclusion: This method is suitable for the simultaneous determination of 38 kinds of nucleosides and amino acids, comparing the differences between different regions, and to a certain extent, it reflects the quality advantages and disadvantages of different regions. Provide a reference for activity research.