طراحي و ساخت اسپكترومتر تحرك يوني با منبع يونيزاسيون الكترواسپري به عنوان آشكار ساز در دستگاه كروماتوگرافي مايع ﴿HPLC-ESI-IMS ﴾ وآناليز آنتي هيستامين ها و سموم قارچ كش

چكيده انگليسي :

Design and Construction of Electrospray Ion Mobility Spectrometry as Detector in Liquid Chromatography HPLC ESI IMS and Analysis of Antihistamines and Pesticides Ali Moradmand A moradmand@ch iut ac ir 5 April 2011 Department of Chemistry Isfahan University of Technology Isfahan 84156 83111 Iran Degree M Sc Language Farsi Prof T Khayamian Taghi@cc iut ac ir Abstract Due to the proteomics revolution multi dimensional separation and detection instruments arerequired to evaluate biomolecule and complex natural samples An ion mobility spectrometry withelectrospray ionization source ESI IMS designed and cunstracted as detector in high performanceliquid chromatography HPLC many HPLC detectors require analytes to have specific chemicalproperties i e UV detectors require analytes to be chromophores and do not offer additionalcomponent information besides HPLC retention times Unlike many HPLC detection methods IMSdoes not require specific analyte properties and provides a second dimension of information ionmobilities The coupling of HPLC with ESI IMS would provide a selective and sensitive detectorwithout the expensive and extensive requirements of MS In this study electrospray ionization ESI ion mobility spectrometry IMS was evaluated as an additional separation after HPLC separations Due to differences in the two mobile phase flow rate HPLC and ESI IMS a splitter was built todivide the flow rate of HPLC column with the ratio of 1 100 Furthermore Coupling of HPLC toESI IMS was carried out by using a modified HPLC tube and directly was used as the needle ofelectrospray for the first time Effect of electric field around the grid was investigated to enhanceresolution of the ESI IMS Imaging system was designed for the first time for ESI IMS This systemallows us to monitor any changes in electrospray We could find conditions for producing a stableelectrospray For this purpose two 5mW diode Layzers were used to lighten the electrosprays area Due to the rapid separation times of IMS multiple IMS spectra were obtained within a single HPLCpeak A mixture of five pesticides were determined using liquid chromatography electrosprayionization ion mobility spectrometry LC ESI IMS to describe the response and analyticalperformance of an ion mobility spectrometer as a detector for liquid chromatography Coelution oftwo peaks due to non optimal HPLC conditions occurred and these two peaks could not bedistinguished by HPLC with UV detection In contrast the single ion mobility spectrum providedseparation of each pesticide as well as providing a second degree of analyte identification HPLCretention time and IMS mobility Detection limit for Carbaryl Amitraz Captafol Folpet andPhosmet were about 0 03 0 2 4 4 18 5 and 0 3 respectively In spite of splitting detection limit forCarbaryl and Phosmet by ESI IMS were lower than UV Vis detector In the second part of thisproject the potential of HPLC ESI IMS for simultaneous determination of Antihistamines wereinvestigated Detection limit for Promethazin Clemastin Cyproheptadine Ketotifen Cinnarizine anddiphenhydramine were about 2 6 0 7 0 9 1 3 0 9 and 0 8 respectively Diphenhydramine andPromethazine that have similar drift time and ESI IMS cannot separate them analyze by HPLC ESI IMS by two dimension separation The detection limits for some compounds were lower in HPLC ESI IMS than that in HPLC UV Vis in spite of splitting However the detection limits for othercompounds could be reduced using a capillary column instead of a traditional column Keywords Ion mobility spectrometry High performance liquid chromatography Antihistamine

مرادمند، علي

طراحي و ساخت اسپكترومتر تحرك يوني با منبع يونيزاسيون الكترواسپري به عنوان آشكار ساز در دستگاه كروماتوگرافي مايع ﴿HPLC-ESI-IMS ﴾ وآناليز آنتي هيستامين ها و سموم قارچ كش

سموم آفت كش