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目的建立超高效液相色谱三重四级杆串联质谱法(UPLC-MS/MS)同时测定浮萍中9种核苷类成分的方法,分析比较不同产地样品中9种成分的差异。方法采用Waters XbridgeTM Amide色谱柱(150 mm×4.6 mm,3.5μm);以0.1%甲酸的水(A)-0.1%甲酸的乙腈(B)溶液为流动相,梯度洗脱,体积流量为0.5 m L/min;柱温30℃,采用电喷雾离子源,正离子检测方式,得到相应的提取离子流图,以峰面积进行定量,用主成分分析和聚类分析方法进行综合评价。结果 9种核苷类成分具有良好的线性关系,r值均大于0.998 9,方法精密度、重复性和稳定性的RSD值均小于3.5%,加样回收率在94.4%~101.9%,RSD在1.73%~3.58%。不同产地浮萍药材中9种核苷在组成和量上均有差异,其中2′-脱氧尿苷、2′-脱氧肌苷在13个产地样品中量均较低,以胞嘧啶最低;尿苷、肌苷、黄嘌呤量较高;13个产地中安徽黄山浮萍中9种核苷总量最高。结论该方法操作简便、准确、重复性好,可为浮萍药材的质量标准制定提供依据。
OBJECTIVE To establish a method for the simultaneous determination of nine nucleosides in duckweed by UPLC-MS / MS and to analyze the differences among the nine constituents in different regions of origin. Methods A Waters XbridgeTM Amide column (150 mm × 4.6 mm, 3.5 μm) was used. The mobile phase consisted of 0.1% formic acid in water (A) and 0.1% formic acid in acetonitrile (B) L / min. The column temperature was 30 ℃. The electrospray ionization (ESI) source and positive ion detection were used to obtain the corresponding ion current extraction map. The peak area was used for quantification. The principal components analysis and cluster analysis were used for comprehensive evaluation. Results The nine nucleosides had a good linear relationship with r values greater than 0.998 9. The RSDs of precision, repeatability and stability were all less than 3.5% and the recoveries were 94.4% -101.9% 1.73% ~ 3.58%. Nine kinds of nucleosides in duckweed medicinal materials of different origins were different in composition and amount, among them, the amount of 2’-deoxyuridine and 2’-deoxyinosine was lower in 13 samples of origin and lowest in cytosine; urine Glycosides, inosine, xanthine amount higher; 13 producing Huangshan duckweed in Anhui highest total amount of nine nucleosides. Conclusion The method is simple, accurate and reproducible. It can provide the basis for the quality standard of duckweed medicinal herbs.