Document Type : Original Paper
Authors
- Asma Chanar 1
- Taj Muhammad Jahangir Khuhawar 2
- Muhammad Yar Khuhawar 2
- Muzamil Yar Khuhawar 3
- Saima Ghoto 1
- Muhammad Farooque Lanjwani 4
1 1 Institute of Advanced Research Studies in Chemical Sciences, University of Sindh, Jamshoro, Sindh-76080, Pakistan 2 High Tech Central Resource Laboratory, University of Sindh, Jamshoro, Sindh-76080, Pakistan
2 1 Institute of Advanced Research Studies in Chemical Sciences, University of Sindh, Jamshoro, Sindh-76080, Pakistan 2 High Tech Central Resource Laboratory, University of Sindh, Jamshoro, Sindh-76080, Pakistan 3 Dr. M.A. Kazi Institute of Chemistry, University of Sindh, Jamshoro, Sindh-76080, Pakistan
3 4 Abbott Laboratories (Pakistan) Limited, Hyderabad Road, Landhi, Karachi-75120, Sindh, Pakistan
4 1 Institute of Advanced Research Studies in Chemical Sciences, University of Sindh, Jamshoro, Sindh-76080, Pakistan 2 High Tech Central Resource Laboratory, University of Sindh, Jamshoro, Sindh-76080, Pakistan 3 Dr. M.A. Kazi Institute of Chemistry, University of Sindh, Jamshoro, Sindh-76080, Pakistan 5 USPCAS-W Mehran University of Engineering & Technology, Jamshoro, Sindh-76062, Pakistan
Abstract
A GC-FID procedure was developed for the separation and analysis of six isomers of xylidines (di-methylanilines), aniline and 1,4-Phenylenediamine after derivatization via ethyl chloroformate (ECF). GC separation was from column DB-5 (30m x 0.32mm) with the 0.25 µm layer thickness, 90 ˚C column temperature for 3 min, followed via heating rate 10 to 200 ˚C followed by hold of temperature for 7 min. The 1.5 ml /min was nitrogen flow with divided ratio 10:1. Linear calibration range of each of the compound was obtained with 1-20 ng/ml with coefficient of determination (r2) 0.9969-0.9970. Limits of detections (LOD) calculated as indication to 3:1 noise ratio was within 0.10-0.99 ng/ml. Derivatization, separation and quantitation were replicate in terms of retention time and peak height/peak area with the relative standard deviations within 2.1%. Method was employed for analysis of effluents of dyes manufacturing company and blood samples of workers employed in dyes manufacturing sector. All the six isomers of xylidines and aniline were detected in effluents and human serum samples at the concentration levels within 49-200 µg/ml and 1.7-9.8 ng/ml respectively. Results of analysis were further confirmed by standard addition technique and percent recoveries were calculated within 96-99 and 95-97 along with % RSD within 3.2 and 2.9 from the effluents and the human serum respectively. Central composite design (CCD) was employed to optimise the parameters. The work examines the quantisation of aromatic amines simultaneously in fairly complex matrix of dyes effluents and biological samples (human serum) by simple GC-FID with adequate sensitivity.
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