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中国精品科技期刊2020
王伟宏,胡菊丽,吴定涛,等. 基于UPLC-Q-Exactive-MS/MS的藜麦皂苷提取物及入血成分分析[J]. 食品工业科技,2023,44(9):296−308. doi: 10.13386/j.issn1002-0306.2022050100.
引用本文: 王伟宏,胡菊丽,吴定涛,等. 基于UPLC-Q-Exactive-MS/MS的藜麦皂苷提取物及入血成分分析[J]. 食品工业科技,2023,44(9):296−308. doi: 10.13386/j.issn1002-0306.2022050100.
WANG Weihong, HU Juli, WU Dingtao, et al. Analysis of Quinoa Saponin Extract and Blood Constituents Based on UPLC-Q-Exactive-MS/MS[J]. Science and Technology of Food Industry, 2023, 44(9): 296−308. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2022050100.
Citation: WANG Weihong, HU Juli, WU Dingtao, et al. Analysis of Quinoa Saponin Extract and Blood Constituents Based on UPLC-Q-Exactive-MS/MS[J]. Science and Technology of Food Industry, 2023, 44(9): 296−308. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2022050100.

基于UPLC-Q-Exactive-MS/MS的藜麦皂苷提取物及入血成分分析

Analysis of Quinoa Saponin Extract and Blood Constituents Based on UPLC-Q-Exactive-MS/MS

  • 摘要: 运用超高效液相色谱-四级杆-静电场轨道离子阱联用质谱(UPLC-Q-Exactive-MS/MS)对藜麦皂苷提取物的主要化学成分及大鼠口服入血成分进行分析鉴定。采用Hypersil Gold VANQUISH C18色谱柱(2.1 mm×100 mm,1.8 μm),流动相为甲酸水-甲酸乙腈梯度洗脱,柱温30 ℃,分析时间35 min,流速0.3 mL·min−1。采用电喷雾离子源(ESI),正、负离子源,Full ms/dd-ms2模式检测。结果显示方法的回收率、基质效应、精密度和稳定性等均符合生物样品的测定要求。在藜麦皂苷提取物中共鉴定到15种皂苷,按苷元构型分为齐墩果酸型皂苷3种,常春藤型皂苷5种,商陆酸型皂苷6种,Serjanic acid型皂苷1种。选用雄性Sprague-Dawley(SD)大鼠,以175.5 mg·kg−1灌胃给予藜麦皂苷提取物,于给药后0、0.5、1、2、4 h下,眼眶取血,大鼠血浆以盐酸丁螺环酮为内标,用甲醇沉淀蛋白,离心,微孔滤膜过滤后进样分析。结果显示在入血成分中共检测到6种原型皂苷以及微量水解后的常春藤皂苷元和Serjanic acid苷元。通过对提取物组成成分及入血成分分析,共鉴定出藜麦皂苷中15个皂苷类化合物及裂解规律,发现了大鼠血浆入血成分相对含量变化情况。初步阐明了藜麦三萜皂苷的化学组成以及体内代谢特征,为藜麦进一步研究和开发应用提供理论依据。

     

    Abstract: The main chemical components of saponins extracted from quinoa and the components in the blood of rat after oral administration were analyzed and identified by ultra-performance liquid chromatography coupled with Q-Exactive mass spectrometry (UPLC-Q-Exactive-MS/MS). Hypersil Gold VANQUISH C18 column (2.1 mm×100 mm, 1.8 μm) was used. The mobile phase was formic acid water-formic acid acetonitrile gradient elution, the column temperature was 30 ℃, the analysis time was 35 min, the flow rate was 0.3 mL·min−1. Electrospray ion source (ESI), positive and negative ion sources and Full ms/dd-ms2 mode were used for detection. The results showed that the recovery rate, matrix effect, precision and stability of the method met the requirements of biological samples. A total of 15 saponins were identified in the saponin extract of quinoa, which were divided into three oleanolic acid saponin types, five hederagenin saponin types, six phytolaccagenic acid saponin types and one serjanic acid saponin type according to the configuration of aglycones. Male Sprague Dawley (SD) rats were selected as the experimental object, after intragastric administration of quinoa saponin extract at 175.5 mg·kg−1, at 0, 0.5, 1, 2 and 4 hours after administration, blood was taken from the orbit, the plasma of rats took buspirone hydrochloride as the internal standard, precipitated protein with methanol, centrifuged, filtered by microporous membrane, and then injected for analysis. The results showed that six prototype saponins and trace hydrolyzed hederagenin and serjanic acid glycosides were detected in the blood components of rat plasma. Through the analysis of the components of the extract and the components entering the blood, 15 saponins in quinoa saponins were identified and their cleavage laws were found, and the changes in the relative contents of the components into the blood of rat plasma were found. The chemical composition and metabolic characteristics of triterpenoid saponins in quinoa were preliminaries elucidated, which provided a theoretical basis for further research and application of quinoa.

     

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