الفصل الكروموتوكرافي لبعض الاحماض الامينية بواسطة طريقة كروموتوكرافيا السائل العالية الاداء باستعمال طور ثابت جديد == Chromatographic Separation of Some Amino Acids by High Performance Liquid Chromatography Method Using A New Stationary Phase
Author name:
علي عباس رسول
General topic:
Chemistry
Specific topic:
Chemistry
Degree:
Master
University:
Al-Nahrain University - College Of Science - Chemistry Department
Language:
English
University location:
Baghdad
First pages:
25T1661 - p.pdf
Abstract:
New stationary phase for high performance liquid chromatographyhas been prepared by the reaction of Neutral red solution with Weaklyacidic cation exchanger resin . The stability of the new attachedfunctional group on the resin was studied against different solvents suchas benzene, ethanol, acetonitrile, acetone, methanol, chloroform, andpetroleum ether as well as NaOH and HCl solutions. The new preparedresin was found stable and no depletion of the Neutral red moiety fromthe resin was noticed with the above materials .The FTIR analysis hasconfigured the attachment of Neutral red on the resin as well as thephysical appearance of the new resins.The new stationary phase has been packed into stainless steel column. The pKa value for new resins has been calculated. The pKa for Weakly acidic - Neutral red resins were 7.15. The chromatographic performance of the packed column was characterized. The number of plate numbers N, height equivalent of a theoretical plates H, capacity factors Ḱ, selectivity factors α, and peaks asymmetry, and Resolution RRsR were measured by analyzing different analytes on the new columns using different mobile phase compositions and flow rates.These parameters were measured from analysis of some amino acids such as Histidine, Phenylalanine, Tryptophan, and Tyrosine. The analysis of amino acids using Weakly acidic - Neutral red column has performed using %10 acetonitrile in buffer phosphate as mobile phase.The average value of plate numbers N was (316.59) . The plate heights H was averaged (0.085) cm , capacity factors Ḱ were ranged from (1.8 - 2.86). Separation factors α were ranged from (0.21 - 1.17), and peak asymmetry value were range from (0.99 - 1.09). Resolution RRsR were ranged from (0.93 - 3.77).IIThe analysis of amino acids using a new stationary phase has performed using buffer phosphate as mobile phase . The average value of plate numbers N was (234.79) , plate heights H was (0.107)cm , capacity factors Ḱ were ranged from (1.13 - 4.73) , separation factors α were ranged from (0.23 - 1.22) , peak asymmetry value were range from (1.10 - 1.18) and resolution were (0.93).R.S.D were ranged from(0.04 - 1)% , recovery were ranged from (93.8 - 97.12)% , The relative errors were ranged from ( - 2.88 - - 6.2) % .Calibration curves for all analyzed compound were linear from their detection limits to at least 50 ppm with correlation coefficient ranged from(0.9991 - 0.9996).The detection limits were ranged from(0.05 - 0.25) ppm at signal to noise ratio of three or more.
