MOF-801/聚合物整体柱的制备及对异牡荆素的固相萃取

doi:10.3969/j.issn.1000-1565.2025.02.007

摘要/Abstract

摘要： 异牡荆素是一种天然的碳苷黄酮类活性物质,具有抗癌、抗炎等多种药理活性,但是其有效成分的分离纯化是开发的难点和关键.因此,制备了MOF材料MOF-801,利用MOF材料上带有的—COOH基团,对其进行衍生化反应,使其表面带有C=C终端,然后与共聚单体(甲基丙烯酸月桂酯,LMA)、交联剂(乙二醇二甲基丙烯酸酯)、致孔剂(正己醇)和引发剂(偶氮二异丁腈)混合均匀后制备MOF-801/聚合物整体柱.通过扫描电子显微镜(SEM)、红外光谱(FT-IR)和氮气吸附-脱附等方法进行表征,结果显示,MOF-801和MOF-801/聚合物整体柱均已成功合成.将MOF-801/聚合物整体柱用作固相萃取(SPE)吸附剂,通过与高效液相色谱(HPLC)仪联用对中药中的抗癌活性成分异牡荆素进行在线富集纯化.结果显示,所制备的聚合物整体柱对异牡荆素具有较好的富集能力,并能去除中药中的部分杂质.

关键词: 聚合物整体柱, 固相萃取(SPE), 异牡荆素, MOF-801

Abstract: Isovitexin is a natural active substance of carboglycoside flavonoids, which has many pharmacological activities such as anti-cancer and anti-inflammation, but its content in medicinal plants is low, and the Chinese herbal medicine extract has some problems such as complex matrix. Therefore, it is necessary to establish a suitable method to enrich and purify isovitexin. In this paper, MOF material MOF-801 was first prepared, and the surface of MOF material was derivatized with —COOH group, so that it had a C=C terminal. Then, it was mixed with comonomer(methyl lauryl acrylate, LMA), cross-linking agent(ethylene glycol dimethacrylate), pore-forming agent(n-hexanol)and initiator(azodiisobutyronitrile)to prepare MOF-801/polymer monolithic column. Then, MOF-801 and MOF-801/ polymer monolithic column were characterized by scanning electron microscope(SEM), FT-IR and nitrogen adsorption-desorption method, which showed that the polymer monolithic column had been successfully synthesized. MOF-801/polymer monolithic column was used as solid-phase extraction(SPE)- DOI:10.3969/j.issn.1000-1565.2025.02.007MOF-801/聚合物整体柱的制备及对异牡荆素的固相萃取柳苹,刘海燕(河北大学药学院,河北省公共卫生安全重点实验室,药物化学与分子诊断教育部重点实验室,河北保定 071002)摘要:异牡荆素是一种天然的碳苷黄酮类活性物质,具有抗癌、抗炎等多种药理活性,但是其有效成分的分离纯化是开发的难点和关键.因此,制备了MOF材料MOF-801,利用MOF材料上带有的—COOH基团,对其进行衍生化反应,使其表面带有C=C终端,然后与共聚单体(甲基丙烯酸月桂酯,LMA)、交联剂(乙二醇二甲基丙烯酸酯)、致孔剂(正己醇)和引发剂(偶氮二异丁腈)混合均匀后制备MOF-801/聚合物整体柱.通过扫描电子显微镜(SEM)、红外光谱(FT-IR)和氮气吸附-脱附等方法进行表征,结果显示,MOF-801和MOF-801/聚合物整体柱均已成功合成.将MOF-801/聚合物整体柱用作固相萃取(SPE)吸附剂,通过与高效液相色谱(HPLC)仪联用对中药中的抗癌活性成分异牡荆素进行在线富集纯化.结果显示,所制备的聚合物整体柱对异牡荆素具有较好的富集能力,并能去除中药中的部分杂质.关键词:聚合物整体柱;固相萃取(SPE);异牡荆素;MOF-801中图分类号:O658 文献标志码:A 文章编号:1000-1565(2025)02-0165-11Preparation of MOF-801/polymer monolithic column and solid phase extraction of isovitexinLIU Ping, LIU Haiyan(Key Laboratory of Medicinal Chemistry and Molecular Diagnosis Ministry of Education, Key Laboratory of Public Health Safety of Hebei Province, College of Pharmacy, Hebei University, Baoding 071002, China)Abstract: Isovitexin is a natural active substance of carboglycoside flavonoids, which has many pharmacological activities such as anti-cancer and anti-inflammation, but its content in medicinal plants is low, and the Chinese herbal medicine extract has some problems such as complex matrix. Therefore, it is necessary to establish a suitable method to enrich and purify isovitexin. In this paper, MOF material MOF-801 was first prepared, and the surface of MOF material was derivatized with —COOH group, so that it had a C=C terminal. Then, it was mixed with comonomer(methyl lauryl acrylate, LMA), cross-linking agent(ethylene glycol dimethacrylate), pore-forming agent(n-hexanol)and initiator(azodiisobutyronitrile)to prepare MOF-801/polymer monolithic column. Then, MOF-801 and MOF-801/ polymer monolithic column were characterized by scanning electron microscope(SEM), FT-IR and nitrogen adsorption-desorption method, which showed that the polymer monolithic column had been successfully synthesized. MOF-801/polymer monolithic column was used as solid-phase extraction(SPE)- 收稿日期:2024-05-29;修回日期:2024-11-06 基金项目:国家自然科学基金资助项目(21974034) 第一作者:柳苹(1998—),女,河北大学在读硕士研究生,主要从事分离材料制备方向研究.E-mail:2761787123@qq.com 通信作者:刘海燕(1971—),女,河北大学教授,博士,主要从事分离材料的制备及对天然产物中抗癌活性成分的富集纯化研究. E-mail:lhy1610@hbu.edu.cn 第2期柳苹等:MOF-801/聚合物整体柱的制备及对异牡荆素的固相萃取河北大学学报(自然科学版) 第45卷adsorbent, and the anticancer active ingredient isovitexin was enriched and purified online by combining with high performance liquid chromatography(HPLC). The results showed that the prepared polymer monolithic column has good ability to enrich isovitexin and remove impurities.

Key words: polymer monolithic column, solid phase extraction(SPE), isovitexin, MOF-801

中图分类号:

O658

柳苹,刘海燕. MOF-801/聚合物整体柱的制备及对异牡荆素的固相萃取[J]. 河北大学学报(自然科学版), 2025, 45(2): 165-175.

LIU Ping, LIU Haiyan. Preparation of MOF-801/polymer monolithic column and solid phase extraction of isovitexin[J]. Journal of Hebei University(Natural Science Edition), 2025, 45(2): 165-175.

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