الاستخلاص بنقطة الغيمة لتقدير الكلور امفينيكول طيفيا في المستحضرات الصيدلانية == CLOUD POINT EXTRACTION FOR THE SPECTROPHOTOMETRIC DETERMINATION OF CHLORAMPHENICOL IN PHARMACEUTICAL PREPARATIONS
Author name:
ضياء يحيى عزيز الحميدي
Supervisor name:
عباس نور محمد الشريفي
General topic:
Chemistry
Specific topic:
Chemistry
Degree:
Master
University:
University of Babylon - College Of Science
Language:
English
University location:
Babylon
First pages:
25T1546 - p.pdf
Abstract:
In this thesis chloramphenicol drug was determined by three methods with spectrophotometric technique.In the first method chloramphenicol was reacted with p - N,NDimethyl - aminobenzaldehyde and form yellow Schiff base product which gave higher absorbance at 436.5 nm. Schiff base reaction occurs between two compounds, one contains amino group and the other contains carbonyl group but chloramphenicol is nitro compound therefore it must convert nitro group in drug to amino group therefore reduction process to nitro group necessary for convert it to amino group.Therefore optimum conditions of reduction process were studied to know exactly the volume of concentrated hydrochloric acid which will give higher absorbance of product. Also amount of zinc, temperature of heating and time from heating during the reduction process were studied. Other optimum conditions of reaction also were studied and Calibration curve constructed and regression equation known (y = 0.0556x + 0.0246), also range of concentration which obeys Beer - Lambert Law was (0.1 - 12)ppm, Molar absorptivity (1.8 * 104 ), Sandell's sensitivity (1.8 * 10 - 2), LOD and LOQ (0.037) and (0.124) respectively. also other studies were performed such as accuracy and precision, Molar ratio method, continues variation method, reaction mechanism, Stability constant of product, Analytical applications and t - test and F - test. The proposed method was successfully in determination of chloramphenicol (CAP) in pharmaceutical preparations with good values of recovery presents (97.6% - 102.5%) and Relative Error E% between ( - 2.351 - 2.562).In the second method, chloramphenicol was reacted with 1,2 - Naphthoquinone - 4 - Sulphonic Acid Sodium Salt in basic medium by condensation reaction and form orange - red product which gave higher absorbance at 489 nm.Optimum conditions of reaction were studied and Calibration curve constructed and regression equation known (y = 0.0577x - 0.0006), also range of concentration which obeys Beer - Lambert Law was (1 - 9)ppm, Molar absorptivity (1.86 * 104), Sandell's sensitive (1.73* 10 - 2), LOD and LOQ (0.068) and (0.207) respectively. Also other studies were performed such accuracy and precision, Molar ratio method ,continues variation method, reaction mechanism, stability constant of product, analytical applications and t - test and F - test. The proposed method was successfully in determination CAP in pharmaceutical preparations with good values of recovery presents (96.149% - 103.307%) and Relative Error E% between ( - 3.851 - 3.307) In the third method, cloud point extraction was applied by extractingthe product used in the second method because there is interaction between the alkaline medium and reagent, this the interaction leads to develop colored reagent and some of radiation absorbed at maximum wavelength of product therefore used cloud point extraction to remove the interference and enhancing sensitivity of method and increasing stability of product.Chloramphenicol was reacted with 1,2 - Naphthoquinone - 4 - Sulphonic Acid Sodium Salt in basic medium by condensation reaction forming orange - red product by using same optimum condition of reaction in the second method then the product was extracted from the solution by using cloud point extraction technique.Optimum conditions of cloud point extraction were studied and Calibration curve was constructed and regression equation known (y = 0.2318x + 0.0639), the range of concentration that obeys Beer - Lambert Law was (0.1 - 6) ppm, Molar absorptivity (7.49 * 104), Sandell's sensitivity (4.31* 10 - 3), LOD and LOQ (0.032) ppm and (0.097)ppm respectively. Also Recovery of solute ( was(99.92), preconcentration factor (fc) (3.33333) and phase volume ratio (Rv) (0.3), also other studies were performed such accuracy and precision, analytical applications and test and F - test. The proposed method was successful in determine chloramphenicol (CAP) in pharmaceutical preparations with good values of recovery percent (96.091% - 101.834%) and Relative Error E% between ( - 3.909 - 1.834).Finally, this thesis presented a proposal for a new way to deal with the data in the analytical methods, which includes the new equations to find a slop and y - intercept of a straight line equation as well as introduced new parameters to determine the best linear correlation between the results, it is average of recovery (Arec), the sum of the absolute values of the relative error (SARE) in concentration computed as well as the average of the absolute values of relative error ( AARE) that gives the best results and more accurate than the usual equation.
