Response Surface Methodological Approach toward Optimization of a RP-HPLC Method to Determine Paracetamol in Tablets

Response surface methodology (RSM) was applied to develop an RP-HPLC method in which paracetamol was analyzed and determined on a C18 column with UV detection. To explain more, RSM was used to statistically model the impact of flow rate (ml.min-1) (A), column temperature (°C) (B) and mobile phase composition (H2O: MeOH) (C)on the retention time (RT) of Paracetamol within tablets. Introduction: The major goal of this investigation was to optimize an RP-HPLC method which is simple, linear, accurate, sensitive and selective in determination of Paracetamol in solid dosage forms. Methods and Results:Three distinctive levels were dedicated to each evaluated factor.Box-Behnken experimental design including seventeen independent runs within a range of 25-50% MeOH ratio (mobile phase), 25-45 ºC and 0.7-1.3 mL. min-1 flow rate were carried out to explore the effectivefactors onRT of Paracetamol using RP-HPLC method. ANOVA results revealed that quadratic model was significant (Model F-value of 225.65) and could best describe the relationship between dependent variable (RT) and independent ones: RT= 3.30 - 1.2A - 0.38B - 0.80C + 0.30AC + 0.43BC + 0.53A2 As can be understood from the model terms, the most significant term was the solvent ratio and all the factor levels were indirectly proportional to the Rt. Moreover, the interaction of column temperature and solvent ration seemed to be more important. It was also predicted that optimum assay condition included 1:2 ratio of methanol to water, column temperature of 35ºC and mobile phase flow rate of 1.3 mL.min−1. Using this optimum condition, baseline separation of the drug was achieved with a good resolution and a run time of 2.1 min. The optimized method was validated in terms of linearity, accuracy, limit of detection and limit of quantification of paracetamol within a few commercially available Paracetamol tablets. Conclusions:The optimized RP-HPLC technique provided a convenient and efficient method toward qualitative/quantitative analysis of Paracetamol in its tablets. The improved method is also rapid and sensitive enough to be used for single tablet analysis

Validation of an Analytical Method for Determination of Benzoapyrene Bread using QuEChERS Method by GC-MS

A fast and simple modified QuEChERS (quick, easy, cheap, rugged and safe) extraction method based on spiked calibration curves and direct sample introduction was developed for determination of Benzo[a]pyrene (BaP) in bread by gas chromatography-mass spectrometry single quadrupole selected ion monitoring (GC/MS-SQ-SIM). Sample preparation includes: extraction of BaP into acetone followed by cleanup with dispersive solid phase extraction. The use of spiked samples for constructing the calibration curve substantially reduced adverse matrix-related effects. The average recovery of BaP at 6 concentration levels was in range of 95-120%. The method was proved to be reproducible with relative standard deviation less than 14.5% for all of the concentration levels. The limit of detection and limit of quantification were 0.3 ng/g and 0.5 ng/g, respectively. Correlation coefficient of 0.997 was obtained for spiked calibration standards over the concentration range of 0.5-20 ng/g. To the best of our knowledge, this is the first time that a QuEChERS method is used for the analysis of BaP in breads. The developed method was used for determination of BaP in 29 traditional (Sangak) and industrial (Senan) bread samples collected from Tehran in 2014. These results showed that two Sangak samples were contaminated with BaP. Therefore, a comprehensive survey for monitoring of BaP in Sangak bread samples seems to be needed. This is the first report concerning contamination of bread samples with BaP in Iran. © 2016 by School of Pharmacy

Validation of an Analytical Method for Determination of benzo[a]pyrene in bread using QuEChERS method by

Abstract A fast and simple modified QuEChERS (quick, easy, cheap, rugged and safe) extraction method based on spiked calibration curves and direct sample introduction was developed for determination of Benzo[a]pyrene (BaP) in bread by gas chromatography-mass spectrometry single quadrupole selected ion monitoring (GC/MS-SQ-SIM). Sample preparation includes: extraction of BaP into acetone followed by cleanup with dispersive solid phase extraction. The use of spiked samples for constructing the calibration curve substantially reduced adverse matrix-related effects. The average recovery of BaP at 6 concentration levels was in range of 95-120%. The method was proved to be reproducible with relative standard deviation less than 14.5% for all of the concentration levels. The limit of detection and limit of quantification were 0.3 ng/g and 0.5 ng/g, respectively. Correlation coefficient of 0.997 was obtained for spiked calibration standards over the concentration range of 0.5-20 ng/g. To the best of our knowledge, this is the first time that a QuEChERS method is used for the analysis of BaP in breads. The developed method was used for determination of BaP in 29 traditional (Sangak) and industrial (Senan) bread samples collected from Tehran in 2014. These results showed that two Sangak samples were contaminated with BaP. Therefore, a comprehensive survey for monitoring of BaP in Sangak bread samples seems to be needed. This is the first report concerning contamination of bread samples with BaP in Iran