Pharmaceuticals and personal care products (PPCPs) constitute a broad class of emerging contaminants, belonging to the list of high production volume chemicals that are currently used for human and veterinary application (e.g., pharmaceuticals, sunscreens, cosmetics, insect repellents, and soaps). These substances have been continuously discharged to the aquatic environment, with resulting environmental and human health impact. In this work, a headspace solid phase microextraction (HS-SPME) method coupled with gas chromatography and MS detection (GC/MS) was optimized for the simultaneous determination of 21 target PPCPs in water samples. The analytes included fragrances, UV-filters, antiseptics, estrogens, anti-inflammatory drugs and pesticides. SPME is an environmentally-friendly alternative to the common approaches, because it achieves extraction and clean-up in a single step eliminating the need for solvents and expensive equipments. An on-fiber SPME derivatization, using silyl reagents, was performed for the analysis of more polar acidic compounds. An experimental design approach was applied to systematically investigate and optimize the operative parameters affecting the extraction recovery: extraction temperature and time, derivatization time, desorption temperature and time. The optimal conditions were: extraction time of 125min at 40°C; derivatization time of 30.5 min; desorption time of 2 min at 300°C. Under these conditions, good repeatability was assessed as RDS% values ≤ 10% for underivatized PPCPs and ≤ 20% for derivatized ones. The method detection limits were between 0.7 and 9.0 ng L-1, with the highest values in the range 2.5-9.0 ng L-1 for the derivatized analytes. Method accuracy was evaluated on spiked tap water samples: recoveries varied from 85 to 103% and from 75 to 110 % for non derivatized and derivatized compounds, respectively. The results obtained indicate the potentiality of the method for the determination of the investigated analytes at trace levels.
DEVELOPMENT OF A SPME/GC/MS METHOD FOR THE SIMULTANEOUS DETERMINATION OF PHARMACEUTICALS AND PERSONAL CARE PRODUCTS IN ENVIRONMENTAL WATERS
BASAGLIA, Giulia;PIETROGRANDE, Maria Chiara
2012
Abstract
Pharmaceuticals and personal care products (PPCPs) constitute a broad class of emerging contaminants, belonging to the list of high production volume chemicals that are currently used for human and veterinary application (e.g., pharmaceuticals, sunscreens, cosmetics, insect repellents, and soaps). These substances have been continuously discharged to the aquatic environment, with resulting environmental and human health impact. In this work, a headspace solid phase microextraction (HS-SPME) method coupled with gas chromatography and MS detection (GC/MS) was optimized for the simultaneous determination of 21 target PPCPs in water samples. The analytes included fragrances, UV-filters, antiseptics, estrogens, anti-inflammatory drugs and pesticides. SPME is an environmentally-friendly alternative to the common approaches, because it achieves extraction and clean-up in a single step eliminating the need for solvents and expensive equipments. An on-fiber SPME derivatization, using silyl reagents, was performed for the analysis of more polar acidic compounds. An experimental design approach was applied to systematically investigate and optimize the operative parameters affecting the extraction recovery: extraction temperature and time, derivatization time, desorption temperature and time. The optimal conditions were: extraction time of 125min at 40°C; derivatization time of 30.5 min; desorption time of 2 min at 300°C. Under these conditions, good repeatability was assessed as RDS% values ≤ 10% for underivatized PPCPs and ≤ 20% for derivatized ones. The method detection limits were between 0.7 and 9.0 ng L-1, with the highest values in the range 2.5-9.0 ng L-1 for the derivatized analytes. Method accuracy was evaluated on spiked tap water samples: recoveries varied from 85 to 103% and from 75 to 110 % for non derivatized and derivatized compounds, respectively. The results obtained indicate the potentiality of the method for the determination of the investigated analytes at trace levels.I documenti in SFERA sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
