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Ma W.,East China University of Science and Technology | Xu H.,East China University of Science and Technology | Xu H.,Shanghai Huazhen Scientific and Technological Co. | Liu Z.,East China University of Science and Technology | And 3 more authors.
Chinese Journal of Chromatography (Se Pu) | Year: 2010

A monolithic column of macro porous poly (glycidyl methacrylate-divinylbenzene) (poly (GMA-D VB)) has been prepared by free radical polymerization within the confines of a chromatographic stainless steel tube (50 mm × 4. 6 mm). For the best separation and low back pressure, orthogonal experiments were carried out with V (cyclohexanol): V (dodecanol); V(GMA): y(DVB) and BPO dosage as the three main factors. The characteristic feature of the column, including specific surface area, pore volumexas weu as pore diameter distribution, was studied by scanning electron microscopy (SEM) mercury intrusion porosimetry analysis and BET analysis. The obtained optimum preparation conditions were that the volume ratio of GMA, DVB, cyclohexanol and dodecan of'was 0. 825: 0. 825: 1. 32: 2. 03 and the BPO dosage was 0. 7% (mass percentage), then it was heated at 70 °C for 24 h. Using this monolithic column; benzene and ethylbenzene and a drug of oxiracetam can be well separated on a high performance liquid chromatographic (HPLC) system equipped with a ultraviolet (UV) detector at 254 nm. A Soluution of acetonitrile-water (50: 50, v/v) for the separation of benzene and ethyl-benzertfflNand acetonitrile-water (80: 20, v/v) for the separation of oxiracetam were used as mobile phases at a flow rate of 1 mL/min. The theoretical plate number was 37 000 plates/m and the resolution of peak width at half height (-R 1/2) was 7. 14. The separation time was less than 10 min. The monolithic column prepared by this method is reproducible and has high column efficiency. It is an economical method to prepare monolithic column, which can be applied to separate small molecules.


Wang H.,East China University of Science and Technology | Wang H.,Shanghai Huazhen Scientific and Technological Co. | Xu H.,East China University of Science and Technology | Xu H.,Shanghai Huazhen Scientific and Technological Co. | And 6 more authors.
Lizi Jiaohuan Yu Xifu/Ion Exchange and Adsorption | Year: 2010

The performance of adsorption for limonin with six macroporous resins AB-8, HZ-816, HZ-818, HZ-803, HZ-806 and D-101 was investigated. And HZ-816 resin, which the better macroporous adsorption resin was chosen, was used to do separation and purification research. The result shows that HZ-816 resin can adsorb and desorb limonin better. The best technology parameters of adsorption and desorption were obtained. After treated with HZ-816, the yield of limonin was 60%, and the content of hmonin was increased from 2.1% to 47.1% with 22 times as high as the crude extracts.

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