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). 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. 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, namely: extraction temperature and time, derivatization time, desorption temperature and time. The optimum operating conditions were: extraction time of 125 min at a temperature of 40C; derivatization time of 30.5 min; desorption time of 2 min at a temperature of 300C. Under these conditions, good reproducibility was assessed as RDS% values lower than 10% for underivatized PPCPs and lower than 20% for derivatized compounds. 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 obtained results indicate the potentiality of the method for the determination of the investigated analytes at trace levels.

OPTIMIZATION OF A SPME/GC/MS METHOD FOR THE SIMULTANEOUS DETERMINATION OF PHARMACEUTICALS AND PERSONAL CARE PRODUCTS IN WATERS

PIETROGRANDE, Maria Chiara;BASAGLIA, Giulia
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). 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. 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, namely: extraction temperature and time, derivatization time, desorption temperature and time. The optimum operating conditions were: extraction time of 125 min at a temperature of 40C; derivatization time of 30.5 min; desorption time of 2 min at a temperature of 300C. Under these conditions, good reproducibility was assessed as RDS% values lower than 10% for underivatized PPCPs and lower than 20% for derivatized compounds. 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 obtained results indicate the potentiality of the method for the determination of the investigated analytes at trace levels.
SPME/GC/MS METHOD; DETERMINATION OF PHARMACEUTICALS AND PERSONAL CARE PRODUCTS; METHOD OPTIMIZATION
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Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/11392/1700504
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