NPLC×RPLC二维液相色谱系统分离分析牛黄解毒片提取物成分的实验研究
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摘要
构建了定量环-阀切换接口的二维液相色谱系统(NPLC×RPLC),采用此系统对牛黄解毒片样品进行分离分析,以4.6mm×50 mm i. d.的SiO_2正相色谱柱为第一维,4.6mm×250 mm i. d.的C18反相色谱柱为第二维。根据有机溶剂的特征,在第一维正相色谱流动相中加入1,4—二氧六环;第二维反相色谱流动相中加入异丙醇,同时通过升高第二维色谱温度的方法增加两维流动相间互溶性,在改善流动相兼容性的同时,有效调整分离选择性。最终,通过总共440min的七次切割共检测出了153个峰,达到950的峰容量。
A two-dimensional liquid chromatography(NPLC×RPLC)was developed. Normal phase liquid chromatography(NPLC)with a SiO_2 column(4.6 mm×50 mm i. d.)was used as the first dimension,and reversed phase liquid chromatogra?phy(RPLC)with a C18 column(4.6 mm×250 mm i. d.)was used as the second loop. As to improve the incompatibility of the two dimensional mobile phase and be good for adjusting the selectivity of separation,1,4-Dioxane was used in the mo?bile phase of the first dimension,and isopropyl alcohol was used in the mobile phase of the second dimension based on the character of organic solvent. By rising the temperature of the second dimension,the system avoid the incompatibility of the two dimensional mobile phase. Niuhuangjiedu Pills was analyzed by this system,the total peak capacity reached 950.
A two-dimensional liquid chromatography(NPLC×RPLC)was developed. Normal phase liquid chromatography(NPLC)with a SiO_2 column(4.6 mm×50 mm i. d.)was used as the first dimension,and reversed phase liquid chromatogra?phy(RPLC)with a C18 column(4.6 mm×250 mm i. d.)was used as the second loop. As to improve the incompatibility of the two dimensional mobile phase and be good for adjusting the selectivity of separation,1,4-Dioxane was used in the mo?bile phase of the first dimension,and isopropyl alcohol was used in the mobile phase of the second dimension based on the character of organic solvent. By rising the temperature of the second dimension,the system avoid the incompatibility of the two dimensional mobile phase. Niuhuangjiedu Pills was analyzed by this system,the total peak capacity reached 950.
引文
[1]Robert E.Murphy,Mark R.Schure,Joe P.Foley.Effect of Sampling Rate on Resolution in Comprehensive Two-Dimensional Liquid Chromatography.Anal.Chem.1998,70:1585-1594.
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[3]高辉,温学森,马小军等.二维液相色谱技术在药物分析中的应用[J].药物分析杂志,2007,27(04):616.
[4]王智聪,张庆合,李彤等.蛋白质组研究中的多维液相色谱技术[J].分析测试学报,2005,24(5):130.
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[6]M.L.Crupi,R Costa,P Dugo,P.et.a1.Food Chemistry.2007,105,771-783.
[7]田宏哲,徐静,关亚风.全二维液相色谱(NPLC×RPLC)接口及其应用[J].高等学校化学学报,2007,28:630.
[2]Martin Gilar,Petra Olivova,Amy E.Daly,et al.Orthogonality of Separation in Two-Dimensional Liquid Chromatography.Anal.Chem.2005,77:6426-6434.
[3]高辉,温学森,马小军等.二维液相色谱技术在药物分析中的应用[J].药物分析杂志,2007,27(04):616.
[4]王智聪,张庆合,李彤等.蛋白质组研究中的多维液相色谱技术[J].分析测试学报,2005,24(5):130.
[5]Joe M.Davis,J.Calvin Giddings.Anal.Chem.1983,55:418-424.
[6]M.L.Crupi,R Costa,P Dugo,P.et.a1.Food Chemistry.2007,105,771-783.
[7]田宏哲,徐静,关亚风.全二维液相色谱(NPLC×RPLC)接口及其应用[J].高等学校化学学报,2007,28:630.