使用新型二元致孔剂聚乙二醇（PEG）/甲醇，以 N，N-二甲基-N-甲基丙烯酰胺基丙基-N，N-二甲基-N-丙烷磺酸内盐（SPP）为单体，季戊四醇三丙烯酸酯（PETA）为交联剂，偶氮二异丁腈（AIBN）为引发剂，通过原位聚合法制备磺酸甜菜碱型两性离子亲水毛细管整体柱。对各反应物的配比进行了优化。结果表明，当单体与致孔剂的质量比为1：2.5，并且致孔剂中 PEG 与甲醇的质量比为1：2，单体内部 SPP 与 PETA 的质量比为1：1，AIBN 为总质量的0.1％时为最优配比；PEG /甲醇二元致孔剂的加入实现了对整体柱内部孔径大小的调节，得到了结构更为均一，渗透性、机械稳定性良好的毛细管整体柱，并且理论塔板数与传统制备方法相比有显著提高，在毛细管液相色谱模式下最高可达2．4×105塔板/ m。将制备的整体柱应用于毛细管液相色谱和加压毛细管电色谱分离酚类、核苷类等极性小分子混合物，得到了很好的分离效果。
Sulfobetaine-based capillary zwitterionic hydrophilic monolithic columns were syn-thesized with a novel binary porogenic agent of polyethylene glycol(PEG)/ methanol. The poly-mer was prepared with( 3-( metharyloylamino)propyl)dimethyl( 3-sulfopropyl)ammonium hydroxide inner salt( SPP)as monomer,pentaerythritol triacrylate( PETA)as crosslinker, and azobisisobutyronitrile(AIBN)as initiator. In order to optimize the properties,the contents of the polymerization mixture were investigated. The optimum preparation conditions were as follows:the mass ratio of monomer and porogenator = 1 :2. 5;the mass ratio of SPP and PETA =1 :1 in the monomer;the mass ratio of PEG and methanol = 2 :1 in the binary porogenic agent;the content of the initiator( AIBN)= 0. 1% ( m / m). With the binary porogenic agent of PEG /methanol addition,good mechanical stability,homogeneous column bed,good permeability and narrow pore size distribution were obtained. In the capillary liquid chromatography mode, the hydrophilic monolith provided column efficiency up to 2.4×10 5 plates / m which was much higher than that fabricated by traditional method without PEG / methanol. The columns were used in capillary liquid chromatography and pressurized capillary electrochromatography for the separation of a mixture of phenols,nucleosides and so on.
参考文献
| [1] | Chen H S;Shen M;Chen L Y.[J].CHROMATOGRAPHIA,201173(7/8):767. |
| [2] | Ikegami T;Tomomatsu K;Takubo H.[J].Journal of Chromatography A,20081184(1/2):474. |
| [3] | van Nuijs A L N;Tarcomnicu I;Covaci A.[J].Journal of Chromatography A,20111218(35):5964. |
| [4] | Lü H X;An H T;Xie Z H.[J].International Journal of Biological Macromolecules,201356:89. |
| [5] | Alpert A J.[J].Journal of Chromatography A,1990499:177. |
| [6] | 郭志谋;张秀莉;徐青.[J].色谱,200927(05):675. |
| [7] | 白立改;牛文敬;杨更亮.[J].色谱,201331(04):303. |
| [8] | Lmmerhofer M;Svec F;Fréchet J M J.[J].Journal of Chromatography A,2001925(1/2):265. |
| [9] | Wang X C;Lin X C;Xie Z H.[J].Journal of Chromatography A,20091216(21):4611. |
| [10] | 林旭聪;林葭;王家斌.[J].色谱,201028(03):284. |
| [11] | Lin X C;Wang X;Zhao T T.[J].Journal of Chromatography A,20121260:174. |
| [12] | Camilla V;Knut I.[J].MACROMOLECULES,200033(07):2539. |
| [13] | 李新燕;王彦;谷雪.[J].色谱,201028(03):231. |
| [14] | 高也;王彦;王超然.[J].色谱,201130(05):487. |
| [15] | Bristow P A;Knox J H.[J].CHROMATOGRAPHIA,197710(06):279. |
| [16] | Lide D R.CRC Handbook of Chemistry and Physics[M].S.l.:CRC Press,1999 |
| [17] | Ming L C;Li M L;Bi F Y.[J].Journal of Chromatography A,20121230:54. |
| [18] | 黄晓佳;王秋泉;黄本立.[J].分析化学,200533(04):467. |
| [19] | Andreas E K;Yiannis C F;Constantine D S.[J].Journal of Chromatography A,20111218(20):2871. |
| [20] | Lin J;Huang G H;Lin X C.[J].ELECTROPHORESIS,200829(19):4055. |
| [21] | Alpert A J.[J].Analytical Chemistry,200880(01):62. |
| [22] | Lin J;Liu S F;Lin J.[J].Journal of Chromatography A,20111218(29):4671. |
- 下载量()
- 访问量()
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%