Validation of a HPLC Method for the Quantitative Analysis of 16-Poly Aromatic Hydrocarbon from Water Sample

S, Suchithra A. (2015) Validation of a HPLC Method for the Quantitative Analysis of 16-Poly Aromatic Hydrocarbon from Water Sample. Masters thesis, Indian Institute of Science Education and Research Kolkata.

PDF (MS dissertation of Suchithra.A. S. (10MS72)) Suchithra_A_S-10MS72.pdf - Submitted Version Restricted to Repository staff only Download (1MB)

Abstract

Polycyclic aromatic hydrocarbons or poly aromatic hydrocarbons are group of organic arene compounds composed of two or more aromatic benzene rings with molecular masses ranging from 128 Dalton to 278 Dalton. Polycyclic aromatic hydrocarbons (PAHs) were ranked as the ninth most threatening compounds to human health in 2001.There are hundreds of polycyclic aromatic hydrocarbons (PAHs) in the environment, among them; sixteen PAHs have been classified as priority pollutants by the United States Environmental Protection Agency. Serious health concerns have arisen as many PAH has been classified as carcinogenic or mutagenic. The objective of the study was to identify the PAH concentration in water samples collected from different places. This method describes a procedure for determination of sixteen polycyclic aromatic hydrocarbons (PAHs) in water samples using high performance liquid chromatography (HPLC) using diode array detector (DAD) and Fluorescence detector (FLD). The method has been validated with linearity, limits of detection (LOD), limit of quantification (LOQ), accuracy in terms of percent recovery, and precision in terms of repeatability. HPLC parameters such as flow rate and mobile phase composition for the determination of PAHs using ultra violet-diode array detector (UV-DAD) and fluorescence detector (FLD) are also analyzed. When direct injection of water sample for PAH analysis in HPLC was done, the concentration seems to be too small to analyze accurately (ppb level). Hence PAH pre-concentration was necessary and PAH extraction has been carried out by solid phase extraction (SPE) using dichloromethane (DCM) solvent for water samples. Linearity of calibration curve for all sixteen PAH in the concentration range of 0.2 -25 ug/mL ranged between R², 0.93-0.99. Analysis of percent recovery of 16 PAHs from produced water sample and spiked di water and analyzed by DAD ranged between 75 ± 5.8 and 94 ± 1.8 respectively and when analyzed by FLD, percent recoveries were found between 81 ± 7.6 and 94 ± 2.3 respectively. The estimated LOQ for DAD ranged between 0.19 ppm and 1.83 ppm and for FLD, LOQ ranged between 0.11ppm and 2.4 ppm. However, from the chromatograph and recovery study, FLD found to be advisable for most of the PAHs except few. The water samples analyzed were collected from Stugatcher and preserved with 6N Hydrochloric acid (HCl).

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