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中国精品科技期刊2020
刘博,张树军,杨伊妮,等. 利用UPLC法对玉米须萜类物质提取工艺的比较分析[J]. 食品工业科技,2023,44(14):282−289. doi: 10.13386/j.issn1002-0306.2022080314.
引用本文: 刘博,张树军,杨伊妮,等. 利用UPLC法对玉米须萜类物质提取工艺的比较分析[J]. 食品工业科技,2023,44(14):282−289. doi: 10.13386/j.issn1002-0306.2022080314.
LIU Bo, ZHANG Shujun, YANG Yini, et al. Comparative Analysis on Terpenoids of Extraction Process from Stigma Maydis by UPLC Method[J]. Science and Technology of Food Industry, 2023, 44(14): 282−289. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2022080314.
Citation: LIU Bo, ZHANG Shujun, YANG Yini, et al. Comparative Analysis on Terpenoids of Extraction Process from Stigma Maydis by UPLC Method[J]. Science and Technology of Food Industry, 2023, 44(14): 282−289. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2022080314.

利用UPLC法对玉米须萜类物质提取工艺的比较分析

Comparative Analysis on Terpenoids of Extraction Process from Stigma Maydis by UPLC Method

  • 摘要: 为研究玉米须中萜类成分的提取工艺。本文以玉米须中含有的玉米烯F(1)、3β-羟基-对映-贝壳杉-15-烯-17-酸-18-酯(2)和4α-羟基-19-降-对映贝壳杉烷型-15-烯-17-酸(3)为标准品,建立了玉米须提取物中三种萜类成分含量的测定UPLC分析方法。其色谱条件为:采用Polar C18 100Ȧ(4.6 mm×150 mm,2.6 µm)色谱柱,以甲醇(A)、0.1%磷酸-水溶液(B)为流动相梯度洗脱,流速1.0 mL/min,柱温40 ℃,波长220 nm,进样量5 μL。结果表明,玉米烯F(1)在0.96~192.0 μg/mL范围内,3β-羟基-对映-贝壳杉-15-烯-17-酸-18-酯(2)和4α-羟基-19-降-对映贝壳杉烷型-15-烯-17-酸(3)在5.0~200.0 μg/mL范围内线性关系良好(r>0.9993),定量限(LOQ,S/N=10)均在5.0~10.0 μg/g之间,平均加样回收率为89.1%~105.8%,相对标准偏差(RSD)均小于2%。表明该方法具有较高的准确度和检测灵敏度,能够准确地对玉米须样品中三种萜类成分进行定量分析,为玉米须萜类成分的进一步深化研究提供科学参考。利用该分析方法优化玉米须中三个萜类成分的提取工艺为:采用加热回流提取法,20%甲醇-水溶液作为提取溶剂,料液比为1:25,提取时间1 h。

     

    Abstract: An extraction process of terpenoids from stigma maydis was discussed in this paper. Firstly, a UPLC analytical method was established based on the three standard substances tigmene F(1), 3β-hydroxy- ent-kaur-15-en-17-oic acid-18-ester(2), and 4α-hydroxy-19-nor-ent-kaur-15-en-17-oic acid (3) from stigma maydis. The chromatography condition was determined as C18 100Ȧ column (4.6 mm×150 mm, 2.6 µm) eluted with MeOH (A)-0.1% phosphoric acid (B) in gradient with the 1.0 mL/min flow rate. The column temperature was 40 ℃ with a 10 μL injection volume. The detection wavelength was set at 220 nm. Results showed that, three terpenoids had good linearity (r>0.9993) in the concentration range of 0.96~192.0 μg/mL (stigmene F) and 5.0~200.0 μg/mL (3β-hydroxy-ent-kaur-15-en-17-oic acid-18-ester and 4α-hydroxy-19-nor-ent-kaur-15-en-17-oic acid), respectively. They showed the same limits of quantitation (LOQ, S/N=10) ranged from 5.0 μg/g to 10.0 μg/g, similar average recovery rate of 89.1%~105.8%, and with could be used for quantitative analysis and provided research reference for terpenoids in stigma maydis. Finally, guided by the optimized analytical method, the extraction process for the three terpenoids from stigma maydis was determined as follows: The extract solvent was 20% MeOH-H2O, which was 25 times weight of stigma maydis, and with refluxed extraction for 1 h.

     

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