Development of a bar adsorptive micro-extraction–large-volume injection–gas chromatography–mass spectrometric method for pharmaceuticals and personal care products in environmental water matrices

• Published in: Analytical and bioanalytical chemistry Vol. 402; no. 3; pp. 1355 - 1364
• Main Authors: Neng, N. R., Nogueira, J. M. F.
• Format: Journal Article
• Language: English
• Published: Berlin/Heidelberg Springer-Verlag 2012; Springer
• Subjects: Adsorption; Adsorptivity; Analytical Chemistry; Biochemistry; Characterization and Evaluation of Materials; Charcoal - chemistry; Chemistry; Chemistry and Materials Science; Copolymers; Cosmetics - analysis; Food Science; Gas chromatography; Gas Chromatography-Mass Spectrometry - instrumentation; Gas Chromatography-Mass Spectrometry - methods; Laboratory Medicine; Mass spectrometry; Mathematical analysis; Matrices; Matrix methods; Methods; Monitoring/Environmental Analysis; Monitors; Original Paper; Personal care industry; Pharmaceutical Preparations - analysis; Pharmaceuticals; Phases; Polystyrenes - chemistry; Reproducibility of Results; Sensitivity and Specificity; Solid Phase Extraction - instrumentation; Solid Phase Extraction - methods; Sorbents; Toiletries; Water; Water Pollutants, Chemical - analysis; Trace analysis; Sorption-based methods; LVI-GC-MS(SIM); PPCPs; Environmental water matrices; Bar adsorptive micro-extraction (BAμE)
• ISSN: 1618-2642; 1618-2650
• DOI: 10.1007/s00216-011-5515-0

The combination of bar adsorptive micro-extraction using activated carbon (AC) and polystyrene–divinylbenzene copolymer (PS-DVB) sorbent phases, followed by liquid desorption and large-volume injection gas chromatography coupled to mass spectrometry, under selected ion monitoring mode acquisition, was developed for the first time to monitor pharmaceutical and personal care products (PPCPs) in environmental water matrices. Assays performed on 25 mL water samples spiked (100 ng L −1 ) with caffeine, gemfibrozil, triclosan, propranolol, carbamazepine and diazepam, selected as model compounds, yielded recoveries ranging from 74% to 99% under optimised experimental conditions (equilibrium time, 16 h (1,000 rpm); matrix characteristics: pH 5, 5% NaCl for AC phase; LD: methanol/acetonitrile (1:1), 45 min). The analytical performance showed good precision (RSD < 18%), convenient detection limits (5–20 ng L −1 ) and excellent linear dynamic range (20–800 ng L −1 ) with remarkable determination coefficients ( r 2  > 0.99), where the PS-DVB sorbent phase showed a much better efficiency. By using the standard addition methodology, the application of the present analytical approach on tap, ground, sea, estuary and wastewater samples allowed very good performance at the trace level. The proposed method proved to be a suitable sorption-based micro-extraction alternative for the analysis of priority pollutants with medium-polar to polar characteristics, showing to be easy to implement, reliable, sensitive and requiring a low sample volume to monitor PPCPs in water matrices.