Page 123 - 《精细化工》2022年第7期
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第 7 期               董其惠,等:  双相深共熔溶剂提取的银杏果外种皮活性成分的分离回收                                   ·1409·


            附 6 h,解吸剂为无水乙醇(其中,NaOH 添加量为                            biloba extracts: A review of the pharmacokinetics of  the active
                                                                   ingredients[J]. Clinical Pharmacokinetics, 2013, 52(9): 727-749.
            0.05 mol/L),静态解吸 8 h。D201 树脂:疏水相 DES
                                                               [2]   ZHANG X H (张心慧), GUO Q R (郭起荣), WANG G B (汪贵斌),
            提取液用无水乙醇稀释 5 倍,25  ℃吸附 6 h,解吸                          et al. Research progress of Ginkgo biloba sarcotesta[J]. Heilongjiang
            剂为体积分数 75%的乙醇水溶液(其中,HCl 添加                             Agriculture Science (黑龙江农业科学), 2018, (11): 156-160.
                                                               [3]   CUI N, ZHANG L L, QUAN M P, et al. Profile of the main bioactive
            量为  0.01 mol/L),静态解吸 2 h,在此条件下 D201                    compounds and  in vitro biological activity of different solvent
            树脂对银杏酚酸的吸附率为 71.73%,1 次解吸率为                            extracts from Ginkgo biloba exocarp[J]. RSC Advances, 2020, 10(73):
                                                                   45105-45111.
            94.54%,银杏酚酸回收率为 67.81%。由于 HYA-502B
                                                               [4]   ZHANG C, LING F, YI Y L, et al. Algicidal activity and potential
            树脂的 1 次解吸率为 33.43%,因此,对 HYA-502B                       mechanisms of ginkgolic acids isolated from Ginkgo biloba exocarp
            树脂进行两次解吸实验,HYA-502B 树脂第 2 次解                           on Microcystis aeruginosa[J]. Journal of Applied Phycology, 2014,
                                                                   26(1): 323-332.
            吸率为 66.08%,两次总解吸率可达 99.51%,推测                      [5]   ZHANG M N (张梦南). Study on the comprehensive extraction of
            是因为第 2 次静态解吸过程中树脂有一部分破损,有                              active substance from the exocarps of  Ginkgo biloba[D]. Beijing:
                                                                   Beijing Institute of Technology (北京理工大学), 2018.
            利于树脂中银杏酚酸的释放,因此,第 2 次的解吸效
                                                               [6]   TANG S R (唐仕荣), SONG J (宋洁), GU S H (顾绍辉), et al.
            果要明显优于第 1 次的解吸效果。最终选择 HYA502                           Separation and purification for ginkgolic acids from Ginkgo biloba
            树脂为疏水相 DES 提取液中银杏酚酸回收的最佳树                              sarcotesta by microporous adsorption resin and high-speed countercurrent
                                                                   chromatography[J]. Food Science and Technology (食品科技), 2020,
            脂,其对银杏酚酸的吸附率可达 93.79%,总解吸率                             45(1): 280-285, 293.
            可达 99.51%,最终银杏酚酸回收率可达 93.33%。                      [7]  ZHANG H  Y  (张洪玉), ZHAO M J (赵明军), ZHOU Z (周状), et al.
                                                                   Research advance on extraction technology of exopleura of Ginkgo
                                                                   biloba L.[J]. Guangzhou Chemical Industry (广州化工), 2010, 38(11):
            3   结论                                                 3-5.
                                                               [8]   PLOTKA-WASYLKA J, DA LA GUARDIA M, ANDRUCH V, et al.
                 在本课题组前期研究基础上建立了回收银杏果                              Deep eutectic solvents vs ionic liquids: Similarities and differences[J].
            外种皮活性成分的方法。经过一系列的优化实验,                                 Microchemical Journal, 2020, 159: 105539.
                                                               [9]   CAO J, YANG M, CAO F L, et al. Well-designed hydrophobic deep
            最终结果如下:                                                eutectic solvents as green and  efficient  media for the  extraction of
                (1)对于亲水相 DES 提取液中的活性成分——                           artemisinin from Artemisia annua leaves[J]. ACS Sustainable Chemistry
                                                                   and Engineering, 2017, 5(4): 3270-3278.
            萜内酯、黄酮、原花青素,采用 EOPO 萃取回收的                          [10]  GAO J, YOU J Y, KANG J H, et al. Recovery of astaxanthin from
            方法。选用 EOPO 分子量 2650,质量分数为 90%的                         shrimp (Penaeus vannamei) waste by ultrasonic-assisted extraction
            EOPO 水溶液与亲水相 DES 提取液按质量比 4∶6                           using ionic liquid-in-water microemulsions[J]. Food Chemistry, 2020,
                                                                   325: 126850.
            组成回收体系,混合离心后第 1 次重新形成双相,                           [11]  WANG T, WANG Q,  GUO  Q,  et al.  A hydrophobic deep eutectic
            此时活性成分富集在 EOPO 相中,分离出 EOPO 富                           solvents-based integrated method for efficient and green extraction
                                                                   and recovery of natural products from Rosmarinus officinalis leaves,
            集相,在 70  ℃下水浴 90 min,离心后第 2 次重新                        Ginkgo biloba leaves and Salvia miltiorrhiza roots[J]. Food Chemistry,
            形成双相,此时活性成分富集在下相水溶液中,其                                 2021, 363: 130282.
                                                               [12]  LIU Y J, ZHANG H, YU H M, et al. Deep eutectic solvent as a green
            中萜内酯、黄酮和原花青素的回收率分别可达
                                                                   solvent for enhanced extraction of narirutin, naringin, hesperidin and
            89.44%、53.27%和 29.77%。                                 neohesperidin from  Aurantii Fructus[J]. Phytochemical Analysis,
                (2)对于疏水相 DES 提取液中活性成分——银                           2019, 30(2): 156-163.
                                                               [13]  CAO J, YANG M, CAO F L, et al. Tailor-made hydrophobic deep
            杏酚酸,采用大孔树脂吸附回收的方法。选用                                   eutectic solvents for cleaner extraction of polyprenyl acetates from
            HYA-502B 树脂进行静态吸附-解吸回收,疏水相                             Ginkgo biloba leaves[J]. Journal of Cleaner Production, 2017, 152:
                                                                   399-405.
            DES 提取液用无水乙醇稀释 3 倍后用树脂静态吸附                         [14]  WU R (吴蓉), ZHANG  W (张薇), CHEN L Y  (陈璐瑶),  et al.
            6 h,样液体积为 10 mL,树脂用量为 1 g。解吸剂                          Simultaneous  extraction of salidroside  and  tyrosol using deep
                                                                   eutectic solvent: Optimization and recovery[J]. Fine Chemicals (精细
            为碱添加量为 0.05 mol/L 的无水乙醇,解吸剂用量
                                                                   化工), 2019, 36(5): 865-874.
            为 10 mL。静态解吸 8 h,重复解吸 2 次,在此条件                     [15]  WU R (吴蓉), WANG H M (王慧敏), CAO J (曹君),  et al.
            下,大孔树脂对银杏酚酸吸附率为 93.79%,总解吸                             Simultaneous extraction of salidroside and tyrosol from Rhodiolarosea L.
                                                                   using  tailor-made deep eutectic solvents[J]. Chemical Journal  of
            率为 99.51%,银杏酚酸的回收率可达 93.33%。                           Chinese Universities (高等学校化学学报), 2019, 40(5): 918-926.
                 本研究成功建立了分别从亲水相 DES 和疏水相                       [16]  GAO  C, CAI C  Y, LIU J J,  et al. Extraction and preliminary
                                                                   purification of polysaccharides from  Camellia oleifera  Abel. seed
            DES 中回收银杏果外种皮中萜内酯、黄酮、原花青                               cake using a thermoseparating aqueous two-phase system based on
            素和银杏酚酸的方法,该法具有高效、绿色、安全、                                EOPO copolymer  and deep eutectic  solvents[J]. Food  Chemistry,
                                                                   2020, 313: 126164.
            操作简便等优点,具有良好应用前景。
                                                               [17]  SU E Z, DONG Q H, WU R, et al. A two-phase deep eutectic solvent
                                                                   and the preparation method for simultaneous  separation and
            参考文献:                                                  extraction of a variety of active components from the waste Ginkgo
            [1]   UDE C, SCHUBERT-ZSILAVECZ M, WURGLICS M, et al. Ginkgo   biloba exocarp: CN 202111447037.5[P]. 2021-12-01.
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