1.Preparation and Characterization of a Novel Isatin Derivative of β-Cyclodextrin-bonded SBA-15 Stationary Phase for HPLC
Yang ZHANG ; Laisheng LI ; Biaoping CHEN ; Rendan ZHOU ; Guizhen NIE
Chinese Journal of Analytical Chemistry 2014;(3):375-383
An isatin derivative ofβ-cyclodextrin Schiff base was first synthesized by the condensation reaction between the carbonyl group of isatin and ethylenediamino group of the mono-substituted β-cyclodextrin. The Schiff base ligand was chemically linked to homemade ordered mesoporous SBA-15 silica gel via 3-( triethoxysilyl) propyl isocyanate coupling agent. In this way, a novel isatin derivative of β-cyclodextrin-bonded SBA-15 stationary phase ( ISCDP) was prepared for HPLC. Its chemical and physical parameters were characterized by infrared spectroscopy, mass spectroscopy, elemental analysis, thermogravimetric analysis, scanning electron microscopy, transmission electron microscopy, X-ray diffraction and BET specific surface area analysis. The basic chromatographic property of ISCDP was evaluated by using polar halogenated uracils and disubstituted benzene positional isomers as solute probes in reversed-phase chromatography. ISCDP was also used to enantioseparate twoβ-blocker drugs in polar organic mode and two dansyl amino acids in reversed-phase mode, respectively. The related chromatographic separation mechanism was also discussed. Above studies were expected to provide experimental basis for the practical application of ISCDP in the future. The results showed that the introduction of isatin indole ring could enhanced the reversed-phase chromatographic separation ability of ISCDP for halogenated uracils within 7 min. The new packing also exhibited high stereoselectivity for the position isomers of nitroaniline, aminophenol and benzenediol, in which the para isomers were finally eluted due to strong inclusion interaction between the isatin derivative of β-cyclodextrin ligand and the isomers. Meanwhile, the introduction of isatin indole ring could also improve the chiral separation ability of ISCDP. For example the fast enantioseparations of chiral β-adrenergic blockers and dansyl-amino acids on ISCDP were achieved within 20 min (Rs>1. 3). Obviously, besides hydrophobicity, various synergistic interactions could enhance the separation selectivities of the new stationary phase for chiral and achiral analytes, including dipole-dipole, hydrogen bonding,π-π and inclusion interactions. The ordered pore structure of SBA-15 facilitated to fast and efficient separation and analysis for drugs with good permeability and low mass transfer resistance.
2.Enantioseparation and Determination of Propranolol in Human Plasma on a New Derivatized β-Cyclodextrin Bonded Phase by HPLC
Rendan ZHOU ; Laisheng LI ; Biaoping CHENG ; Guizhen NIE ; Hongfu ZHANG
Chinese Journal of Analytical Chemistry 2014;(7):1002-1009
A 6-azido-β-cyclodextrin was synthesized and derivatized with p-nitrophenyl isocyanate as chiral ligand. Following that the ligand was chemically bonded to mesoporous SBA-15 via a ‘Click Chemistry ’ reaction of the azido group with alkynyl group. A new p-nitrophenylcarbamoylatedβ-cyclodextrin bonded SBA-15 chiral stationary phase ( NPCSP ) for HPLC was obtained. The new stationary phase was first used to enantioseparate propranolol in human plasma under the polar organic solvent mode. The effects of methanol content , additive concentration of glacial acetic acid/triethylamine in mobile phase and the temperature on the enantioseparation were studied. The optimal chromatographic conditions were as follows: mobile phase was acetonitrile/methanol/glacial acetic acid/triethylamine (90:10:1. 25:2. 25, V/V), temperature 288 K, flow rate of 0. 5 mL/min, injection volume of 20 μL, detection wavelength at 290 nm. The resolution was 2. 04 with a short run time (< 15 min) under the above conditions. The composition of propranolol in plasma was quantitatively measured by HPLC-MS selected ion monitoring mode ( [ M +H ]+ m/z 260 . 10 ) with hydrochlorothiazide as internal standard. And linear range was 2. 5-250 μg/L and with a good linear relationship. The detection limit was 1 μg/L according to S/N=3. The experimental results showed that the chiral stationary phase exhibited excellent chiral separation ability to propranolol and the analysis method for propranolol in plasma was sensitive, accurate, simple and fast, which could be used for the determination of propranolol in plasma and pharmacokinetic studies.
3.Establishment of Quality Control System of Nucleic Acid Detection for Ebola Virus in Sierra Leone-China Friendship Biological Safety Laboratory.
Qin WANG ; Yong ZHANG ; Kai NIE ; Huanyu WANG ; Haijun DU ; Jingdong SONG ; Kang XIAO ; Wenwen LEI ; Jianqiang GUO ; Hejiang WEI ; Kun CAI ; Yanhai WANG ; Jiang WU ; Bangura GERALD ; Idrissa Laybohr KAMARA ; Mifang LIANG ; Guizhen WU ; Xiaoping DONG
Chinese Journal of Virology 2016;32(2):210-214
The quality control process throughout the Ebola virus nucleic acid detection in Sierra Leone-China Friendship Biological Safety Laboratory (SLE-CHN Biosafety Lab) was described in detail, in order to comprehensively display the scientific, rigorous, accurate and efficient practice in detection of Ebola virus of first batch detection team in SLE-CHN Biosafety Lab. Firstly, the key points of laboratory quality control system was described, including the managements and organizing, quality control documents and information management, instrument, reagents and supplies, assessment, facilities design and space allocation, laboratory maintenance and biosecurity. Secondly, the application of quality control methods in the whole process of the Ebola virus detection, including before the test, during the test and after the test, was analyzed. The excellent and professional laboratory staffs, the implementation of humanized management are the cornerstone of the success; High-level biological safety protection is the premise for effective quality control and completion of Ebola virus detection tasks. And professional logistics is prerequisite for launching the laboratory diagnosis of Ebola virus. The establishment and running of SLE-CHN Biosafety Lab has landmark significance for the friendship between Sierra Leone and China, and the lab becomes the most important base for Ebola virus laboratory testing in Sierra Leone.
China
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Ebolavirus
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classification
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genetics
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isolation & purification
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Hemorrhagic Fever, Ebola
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diagnosis
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virology
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Humans
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Laboratories
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manpower
;
standards
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Laboratory Infection
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Quality Control
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RNA, Viral
;
genetics
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Sierra Leone