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猴耳环多酚改良型双水相萃取体系的建立                                               Δ


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        古丽霞 ,傅咏梅 ,张 蜀 ,林居逸 ,邓 红 ,卢永美(1.广东药科大学广东省药物新剂型重点实验室,广
               1*
                                          1
                                                             1
                        2
        州 510006;2.国药集团广东环球制药有限公司,广东 佛山 528000;3.广东药科大学广东省局部精准药物递
        药制剂工程技术研究中心,广州 510006)
        中图分类号 R284.2          文献标志码 A          文章编号 1001-0408(2021)18-2236-07
        DOI   10.6039/j.issn.1001-0408.2021.18.10

        摘   要   目的:建立猴耳环多酚的改良型双水相萃取体系。方法:以猴耳环多酚含量、提取效率和分配系数为指标,采用单因素实
        验筛选双水相萃取体系的料液比、乙醇质量分数和超声时间。制备猴耳环不同极性部位的双水相萃取液,以多酚含量和抗氧化活
        性[1,1-二苯基-2-三硝基苯肼(DPPH)、2,2′-联氨-双(3-乙基苯并噻唑-6-磺酸)二铵盐(ABTS)的半数抑制浓度(IC50 )]为指标,结合
        多酚类成分与抗氧化活性的灰色关联度分析,筛选改良剂。考察含不同质量分数(0~90%)改良剂的改良型双水相萃取体系对猴
        耳环多酚提取的影响,并与传统提取工艺(超声提取和加热回流提取)进行比较。结果:最优双水相萃取体系为料液比1 ∶ 45,乙醇
        质量分数 40%,硫酸铵质量分数 11%,室温下超声提取 20 min。3 次验证实验中,猴耳环多酚含量、提取效率和分配系数分别为
        (28.35±1.01)%(RSD=3.56%,n=3)、(98.87±0.19)%(RSD=0.19%,n=3)和 13.25±0.71(RSD=5.39%,n=3)。改良剂为乙
        酸乙酯。当乙酸乙酯-乙醇混合溶液中乙酸乙酯的质量分数为70%时,改良型双水相萃取体系提取所得萃取物中多酚含量和抗氧
        化活性与超声提取、加热回流提取比较差异均无统计学意义(P>0.05),但得率和转移率均显著高于超声提取、加热回流提取(P<
        0.05)。结论:成功建立提取得率和转移率优于传统提取方法的改良型双水相萃取体系,可一步提取猴耳环多酚。
        关键词 猴耳环;多酚;改良型双水相萃取;抗氧化活性
        Establishment of Modified Aqueous Two-phase Extraction System of Polyphenols from Archidendron
        clypearia
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        GU Lixia ,FU Yongmei ,ZHANG Shu ,LIN Juyi ,DENG Hong ,LU Yongmei(1. Guangdong Provincial Key
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                             2
        Laboratory of Advanced Drug Delivery Systems,Guangdong Pharmaceutical University,Guangzhou 510006,
        China;2. Sinopharm Group Guangdong Medi-World Pharmaceutical Co.,Ltd.,Guangdong Foshan 528000,
        China;3. Guangdong Provincial Engineering Center of Topical Precise Drug Delivery Systems,Guangdong
        Pharmaceutical University,Guangzhou 510006,China)
        ABSTRACT     OBJECTIVE: To establish modified aqueous two-phase extraction (ATPE) system of polyphenols from
        Archidendron clypearia. METHODS:Taking the polyphenol content,extraction efficiency and partition coefficient of A. clypearia
        as indexes,the solid-liquid ratio,ethanol mass fraction and ultrasonic time of ATPE system were selected by single factor tests.
        The aqueous two-phase extracts from different polar parts of A. clypearia was prepared. The modifier was selected by taking
        polyphenol content and antioxidant activity [IC50 of 1,1-diphenyl-2-trinitrophenylhydrazine (DPPH), 2,2′-hydrazine bis
        (3-ethylbenzothiazole-6-sulfonic acid) diammonium salt (ABTS)] as indicators,combined with the grey correlation analysis
        between polyphenols and antioxidant activity. The effects of modified ATPE system with different mass fraction (0-90%) of
        modifier on the extraction of polyphenols from A. clypearia were investigated and compared with traditional extraction technology
        (ultrasonic extraction and heating reflux extraction). RESULTS:The optimal ATPE system included solid-liquid ratio of 1 ∶ 45,
        ethanol mass fraction of 40%,(NH4 ) 2SO4 mass fraction of 11%,ultrasonic extraction time of 20 min,at room temperature. In 3
        validation tests,polyphenol content,extraction efficiency and partition coefficient were(28.35±1.01)%(RSD=3.56%,n=3),
        (98.87±0.19)%(RSD=0.19%,n=3)and 13.25±0.71(RSD=5.39%,n=3),respectively. The modifier was ethyl acetate. When
        the mass fraction of ethyl acetate in the ethyl acetate-ethanol mixed solvent was 70%,there was no significant difference in the
        content and anti-oxidant activity of polyphenols from A. clypearia of modified ATPE(P>0.05). The yield and transfer rate of it
        were significantly higher than those of ultrasonic extraction and heating reflux extraction (P<0.05). CONCLUSIONS:The
                                                            modified ATPE system with better extraction yield and transfer
            Δ 基金项目:广东省普通高校科研项目重点领域专项(乡村振兴)
                                                            rate than the traditional extraction technology is successfully
        (No.2020ZDZX1030)
                                                            established,which can extract polyphenols from A. clypearia
            * 硕 士 研 究 生 。 研 究 方 向 :药 品 检 验 与 分 析 。 E-mail:
        1048214903@qq.com                                   in one step.
            # 通信作者:高级工程师。研究方向:新药研发与质量标准。                    KEYWORDS     Archidendron clypearia;Polyphenols;Modified
        E-mail:dengh361@sohu.com                            aqueous two-phase extraction;Antioxidant activity


        ·2236 ·  China Pharmacy 2021 Vol. 32 No. 18                                 中国药房    2021年第32卷第18期
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