title: Application of ethyl chloroformate derivatization for solid-phase microextraction-gas chromatography-mass spectrometric determination of bisphenol-A in water and milk samples.
abstract: A simple and rapid analytical method based on in-matrix ethyl chloroformate (ECF) derivatization has been developed for the quantitative determination of bisphenol-A (BPA) in milk and water samples. The samples containing BPA were derivatised with ECF in the presence of pyridine for 20 s at room temperature, and the non-polar derivative thus formed was extracted using polydimethylsiloxane solid-phase microextraction (SPME) fibres with thicknesses of 100 μm followed by analysis using gas chromatography-mass spectrometry. Three alkyl chloroformates (methyl, ethyl and isobutyl chloroformate) were tested for optimum derivatisation yields, and ECF has been found to be optimum for the derivatisation of BPA. Several parameters such as amount of ECF, pyridine and reaction time as well as SPME parameters were studied and optimised in the present work. The limit of detection for BPA in milk and water samples was found to be 0.1 and 0.01 μg L(-1), respectively, with a signal-to-noise ratio of 3:1. The limit of quantitation for BPA in milk and water was found to be 0.38 and 0.052 μg L(-1), respectively, with a signal-to-noise ratio of 10:1. In conclusion, the method developed was found to be rapid, reliable and cost-effective in comparison to silylation and highly suitable for the routine analysis of BPA by various food and environmental laboratories.
authors: Analytical Chemistry Section, Indian Institute of Toxicology Research, CSIR, P.O. Box 80, M G Marg, Lucknow 226 001, India. mohanitrc@gmail.com
authors: Mohana Krishna Reddy
authors: MK
authors: Mudiam
authors: Rajeev
authors: R
authors: Jain
authors: Virendra K
authors: VK
authors: Dua
authors: Amit Kumar
authors: AK
authors: Singh
authors: V P
authors: VP
authors: Sharma
authors: R C
authors: RC
authors: Murthy
mesh_terms: D000395:Air Pollutants, Occupational / Q000032:analysis / Q000302:isolation & purification; D000818:Animals; D001559:Benzhydryl Compounds; D004968:Estrogens, Non-Steroidal / Q000032:analysis* / Q000302:isolation & purification; D005563:Formic Acid Esters / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry / Q000191:economics / Q000379:methods; D057230:Limit of Detection; D008892:Milk / Q000737:chemistry*; D010636:Phenols / Q000032:analysis* / Q000302:isolation & purification; D052617:Solid Phase Microextraction / Q000191:economics / Q000379:methods; D014867:Water / Q000032:analysis*; D000098826:Bisphenol A Compounds
chemical_list: D000395:Air Pollutants, Occupational; D001559:Benzhydryl Compounds; D004968:Estrogens, Non-Steroidal; D005563:Formic Acid Esters; D010636:Phenols; D014867:Water; C007658:ethyl chloroformate; C006780:bisphenol A; D000098826:Bisphenol A Compounds