Unit:
Κατεύθυνση Χημική Ανάλυση-Έλεγχος ΠοιότηταςLibrary of the School of Science
Author:
Σπυρόπουλος Σταύρος
Supervisors info:
Κουππάρης Μιχαήλ Καθηγητής ΕΚΠΑ (επιβλέπων), Θωμα?δης Νικόλαος Αναπλ. Καθηγητής ΕΚΠΑ, Οικονόμου Αναστάσιος Αναπλ. Καθηγητής ΕΚΠΑ
Original Title:
Ανάπτυξη, βελτιστοποίηση και επικύρωση αναλυτικών μεθόδων για τον προσδιορισμό ολικής παραφίνης σε κοσμητική κρέμα με σύστημα GC-FID
Translated title:
Development, optimization and validation of analytical methods for the determination of total paraffin in cosmetic cream with GC-FID
Summary:
The purpose of this investigation is the development, the optimization and the
validation of an analytical method for the determination of the total paraffin
liquid and solid in cosmetic cream samples.
The system used was a gas chromatograph with a flame ionization detector
(GC-FID) capillary column MEGA-5HT of MEGA Corporations with internal diameter
0.25 mm, length 30 m and maximum temperature in 350 °C, while the mobile phase
was composed of gas Helium. The typical flow of the mobile phase was 3 mL/min,
the injected volume was 0.5μL and the temperature of injector was 320° C.
Finally it was not possible to establish an analytical method for the
determination of the liquid an solid paraffin at the same time. Therefore two
independent analytical methods for each species were established. For the
conditions optimization in both methods, the single factor, at a time,
sequential optimization method was used. Scalar temperature programs in both
methods were taken place, due to the large amount an the complexity of the
compound about to be determined, while for the quantization of the results for
the solid paraffin the sum of the area of all peaks was calculated and as for
the liquid paraffin the maximum height of the curve was used.
For the validation of the two analytical methods took place the following
experiments:
Specificity of the method, in which the pics obtained from the placebo did not
interfere with the pics of the compound about to be determined in the solid
paraffin. While the maximum height of the signal had not been affected in the
liquid paraffin.
Linearity of the method, in which the correlation calibration coefficient was
higher than 0.99 in both methods.
Precision of the method in which the relative standard deviation of the
results in both analytical methods was within the upper limit of 0.5%.
Robustness of the method, in which small variation in experimental conditions
such as variation rate of the temperature program, in typical flow of the
liquid phase and the initial column temperature did not substantially affect
the final result.
Limit of detection- quantization, in which for the solid paraffin 50ppm and
150ppm were found respectively. While in the liquid paraffin 83ppm and 250ppm
were obtained respectively
Keywords:
Development, Optimization, Validation, Analytical method, Gas-chromatography
Number of index pages:
XII-XV
Number of pages:
[1], XVIII, 91
