色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
4期
388-394
,共7页
况媛媛%王彦%谷雪%李静%阎超
況媛媛%王彥%穀雪%李靜%閻超
황원원%왕언%곡설%리정%염초
二元致孔剂%磺酸甜菜碱%两性离子亲水整体柱%毛细管液相色谱%加压毛细管电色谱
二元緻孔劑%磺痠甜菜堿%兩性離子親水整體柱%毛細管液相色譜%加壓毛細管電色譜
이원치공제%광산첨채감%량성리자친수정체주%모세관액상색보%가압모세관전색보
binary porogenic agent%sulfobetaine%zwitterionic hydrophilic monolithic column%capillary liquid chromatography(cLC)%pressurized capillary electrochromatography(pCEC)
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。
使用新型二元緻孔劑聚乙二醇(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-丙烷磺痠內鹽(SPP)為單體,季戊四醇三丙烯痠酯(PETA)為交聯劑,偶氮二異丁腈(AIBN)為引髮劑,通過原位聚閤法製備磺痠甜菜堿型兩性離子親水毛細管整體柱。對各反應物的配比進行瞭優化。結果錶明,噹單體與緻孔劑的質量比為1:2.5,併且緻孔劑中 PEG 與甲醇的質量比為1:2,單體內部 SPP 與 PETA 的質量比為1:1,AIBN 為總質量的0.1%時為最優配比;PEG /甲醇二元緻孔劑的加入實現瞭對整體柱內部孔徑大小的調節,得到瞭結構更為均一,滲透性、機械穩定性良好的毛細管整體柱,併且理論塔闆數與傳統製備方法相比有顯著提高,在毛細管液相色譜模式下最高可達2.4×105塔闆/ m。將製備的整體柱應用于毛細管液相色譜和加壓毛細管電色譜分離酚類、覈苷類等極性小分子混閤物,得到瞭很好的分離效果。
사용신형이원치공제취을이순(PEG)/갑순,이 N,N-이갑기-N-갑기병희선알기병기-N,N-이갑기-N-병완광산내염(SPP)위단체,계무사순삼병희산지(PETA)위교련제,우담이이정정(AIBN)위인발제,통과원위취합법제비광산첨채감형량성리자친수모세관정체주。대각반응물적배비진행료우화。결과표명,당단체여치공제적질량비위1:2.5,병차치공제중 PEG 여갑순적질량비위1:2,단체내부 SPP 여 PETA 적질량비위1:1,AIBN 위총질량적0.1%시위최우배비;PEG /갑순이원치공제적가입실현료대정체주내부공경대소적조절,득도료결구경위균일,삼투성、궤계은정성량호적모세관정체주,병차이론탑판수여전통제비방법상비유현저제고,재모세관액상색보모식하최고가체2.4×105탑판/ m。장제비적정체주응용우모세관액상색보화가압모세관전색보분리분류、핵감류등겁성소분자혼합물,득도료흔호적분리효과。
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.