异甘草素键合硅胶固定相的合成及应用
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摘要
以10μm硅胶为基质,异甘草素为配体,采用液相连续反应法及中间体法依次合成了异甘草素键合硅胶固定相ISLSP-Ⅰ和ISLSP-Ⅱ。采用FTIR及SEM对合成的固定相进行表征。将ISLSP-Ⅰ固定相填充于50 mm×10 mm i.d. 1号色谱柱中,将ISLSP-Ⅱ固定相填充于30 mm×10 mm i.d. 2号色谱柱中,系统评价了两种方法合成的固定相的色谱性能。结果表明:两根色谱柱的柱效及峰型均较好,大流速下测试组分的保留主要决定于传质阻力。在甲醇-水体系下,2号色谱柱表现出明显的反相色谱分离机制。合成的固定相稳定性良好,使用6个月后,测试组分在两根色谱柱上的保留时间相对偏差不超过0.9%。2号色谱柱对多组分标准样品及中药提取物均具有良好的分离能力。
New isoliquiritigenin bonded silica gel stationary phases(ISLSP-Ⅰ, ISLSP-Ⅱ) were synthesized using 10 μm silica gel as the substrate and isoliquiritigenin as the ligand by continuous liquid phase reaction and intermediate method, respectively. The synthesized stationary phases were characterized by FTIR and SEM. The stationary phase ISLSP-Ⅰ was packed in a 50 mm × 10 mm i.d. column 1. The stationary phase ISLSP-Ⅱ was packed in a 30 mm × 10 mm i.d. column 2. Their chromatographic performances were systematically evaluated. The results showed that the column efficiency and peak shapes of these two chromatographic columns were good. The retention time of test components at large flowrate was mainly determined by mass transfer resistance. In the methanol and water mixed solvent, column 2 exhibited a certain reversed-phase chromatographic separation mechanism. For test components, the relative deviation of retention time on the two columns did not exceed 0.9% after 6 months of use, indicating that the synthesized stationary phases had good stability. In addition, the two columns had good separation abilities for the multi-components standard sample mixtures and the Chinese medicine extracts.
New isoliquiritigenin bonded silica gel stationary phases(ISLSP-Ⅰ, ISLSP-Ⅱ) were synthesized using 10 μm silica gel as the substrate and isoliquiritigenin as the ligand by continuous liquid phase reaction and intermediate method, respectively. The synthesized stationary phases were characterized by FTIR and SEM. The stationary phase ISLSP-Ⅰ was packed in a 50 mm × 10 mm i.d. column 1. The stationary phase ISLSP-Ⅱ was packed in a 30 mm × 10 mm i.d. column 2. Their chromatographic performances were systematically evaluated. The results showed that the column efficiency and peak shapes of these two chromatographic columns were good. The retention time of test components at large flowrate was mainly determined by mass transfer resistance. In the methanol and water mixed solvent, column 2 exhibited a certain reversed-phase chromatographic separation mechanism. For test components, the relative deviation of retention time on the two columns did not exceed 0.9% after 6 months of use, indicating that the synthesized stationary phases had good stability. In addition, the two columns had good separation abilities for the multi-components standard sample mixtures and the Chinese medicine extracts.
引文
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[15]Xu Lili(许丽丽),Ren Nailin(任乃林),Lin Zeling(林泽玲).Preparation and application of an emodin-bonded silica gel chromatographic column for high performance liquid chromatography[J].Chin JChromatogr(色谱),2014,32(8):798-803.
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[3]Ding X L,Yang J,Dong Y M.Advancements in the preparation of high-performance liquid chromatographic organic polymer monoliths for the separation of small-molecule drugs[J].J Pharm Anal,2018,8(2):75-85.
[4]Jiao Chunxia(焦春霞),Wang Gang(王刚).Research progress on the bonded silica gel stationary phase of natural product components with high performance liquid chromatography[J].Journal of Food Safety and Quality(食品安全质量检测学报),2018,9(10):2304-2310.
[5]Li Laisheng(李来生),Chen Hong(陈红),Ma Haiping(马海萍),et al.Preparation,characterization and performance evaluation of magnolol-bonded silica gel liquid chromatography stationary phase[J].Chem J Chin Univ(高等学校化学学报),2012,33(4):707-713.
[6]Li Laisheng(李来生),Chen Xiongquan(陈雄泉),Yang Hanrong(杨汉荣),et al.Preparation and characterization of baicalin-bonded silica gel stationary phase[J].Anal Chem(分析化学),2007,7(9):1279-1284.
[7]Fang Yishan(方奕珊),Li Laisheng(李来生),Chen Hong(陈红),et al.Study on the quercetin-bonded silica gel phase for the separations of polar compounds by high-performance liquid chromatography[J].Chin J Appl Chem(应用化学),2013,30(1):79-87.
[8]Xu Lili(许丽丽),Zhong Minghua(衷明华),Chen Xiaojing(陈小静).Preparation and chromatographic performance of a eugenolbonded silica gel stationary phase for high performance liquid chromatography[J].Chin J Chromatogr(色谱),2015,33(5):461-467.
[9]Gu Xiaojuan(谷晓娟),Han Yaqiong(韩亚琼),Li Xinyi(李心怡),et al.Preparation,characterization and application of ginsenoside Rg1bonded silica gel stationary phase[J].Res Dev Nat Prod(天然产物研究与开发),2014,26(6):824-829.
[10]Zhang Y,Luo H,Carr P W.Silica-based,hyper-crosslinked acid stable stationary phases for high performance liquid chromatography[J].JChromatogr A,2012,1228:110-124.
[11]Wu T Y,Khor T O,Saw C L,et al.Anti-inflammatory/anti-oxidative stress activities and differential regulation of Nrf2-mediated genes by non-polar fractions of tea Chrysanthemum zawadskii and licorice Glycyrrhiza uralensis[J].AAPS J,2011,13(1):1-13.
[12]Chen H-Y,Huang T-C,Shieh T-M,et al.Isoliquiritigenin induces autophagy and inhibits ovarian cancer cell growth[J].Int J Mol Sci,2017,18(10):2025.
[13]Cronin H,Draelos Z D.Top 10 botanical ingredients in 2010anti-aging creams[J].J Cosmet Dermatol,2010,9(3):218-225.
[14]Chen Tianbao,Deng Shaoxiong,Lin Rong.The inhibitory effect of Isoliquiritigenin on the proliferation of human arterial smooth muscle cell[J].BMC Pharmacol Toxicol,2017,18:57.
[15]Xu Lili(许丽丽),Ren Nailin(任乃林),Lin Zeling(林泽玲).Preparation and application of an emodin-bonded silica gel chromatographic column for high performance liquid chromatography[J].Chin JChromatogr(色谱),2014,32(8):798-803.
[16]Lu Peizhang(卢佩章),Dai Chaozheng(戴朝政),Zhang Xiangmin(张祥民).Theoretic bases of chromatography:Second Edition[M].Beijing:Science Press(科学出版社),1997:273.