UPLC-QTOF-MS分析乌蔹莓成分及多组分定量研究

UPLC-QTOF-MS Analysis and Multicomponent Quantitative Analysis of Cayratia Japonica

  • 摘要: 目的 定性分析乌蔹莓化学成分并对其主要成分建立定量分析方法。方法 采用高效液相色谱-四极杆飞行时间质谱(UPLC-QTOF-MS)技术,选用ACQUITY UPLC HSS T3色谱柱(2.1 mm×50 mm,1.8 μm),以0.1%甲酸水溶液(A)-乙腈(B)为流动相进行梯度洗脱,流速为0.4 mL/min,质谱采用电喷雾(ESI)离子源,在正、负离子模式下采集数据。运用PeakView软件对结果进行分析,根据化合物的相对保留时间、准分子离子峰和碎片离子峰等信息,并结合对照品和相关文献进行成分鉴定。采用UPLC法对4个主要成分(木犀草素-7-O-葡萄糖苷、芹菜素-7-O-葡萄糖苷、木犀草素、芹菜素)建立含量测定方法。结果 从乌蔹莓中共推断并鉴定出31个化学成分,包括黄酮及其苷类6个,香豆素类3个,萜类及三萜类7个,脂肪酸酯类7个,其他类8个。3批乌蔹莓中木犀草素-7-O-葡萄糖苷、芹菜素-7-O-葡萄糖苷、木犀草素、芹菜素含量范围分别为0.061%~0.15%、0.077%~0.14%、0.011%~0.028%、0.020%~0.062%。结论 该分析方法可以快速、准确地分析乌蔹莓中的化学成分,建立的定量方法为乌蔹莓质量控制及制剂开发奠定了基础。

     

    Abstract: OBJECTIVE To qualitative analysis of the chemical constituents of Cayratia japonica and establish a quantitative analysis method for the main components. METHODS ACQUITY UPLC HSS T3 chromatographic columns (2.1 mm×50 mm, 1.8 μm) were selected, acetonitrile (B)-0.1% formic acid aqueous solution (A) was used as mobile phase for gradient elution, a flow rate of 0.4 mL/min, mass spectrometry using electrospray (ESI) ion source to collect data in positive and negative ion mode.The results were analyzed by PeakView software. Then according to the relative retention time, excimer ion peak and fragment ion peak of the compound, the chemical composition was analyzed according to the reference material and related literature. The quantitative analysis of four main components (luteolin-7-O-glucoside, apigenin-7-O-glucoside, luteolin, apigenin) were established. RESULTS A total of 31 chemical constituents were identified in Cayratia japonica, including 7 flavonoids and their glycosides, 3 coumarins, 7 terpenoids and triterpenoids, 7 fatty acid esters and 8 other classes. The contents of luteolin-7-O-glucoside, apigenin-7-O-glucoside, luteolin and apigenin in three batches of Cayratia japonica were 0.061%~0.15%, 0.077%~0.14%, 0.011%~0.028% and 0.020%~0.062%, respectively. CONCLUSION This method can analyze quickly and accurately the constituents of Cayratia japonica and the quantitative analysis method could be used for quality control of Cayratia japonica.

     

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