Determination of pharmaceuticals in soils and sediments by pressurized liquid extraction and liquid chromatography tandem mass spectrometry.
The present work describes the development of a sensitive analytical method based on pressurized liquid extraction (PLE) and pre-concentration by solid-phase extraction (SPE), followed by liquid chromatography-electrospray tandem mass spectrometry (LC-ESI-MS/MS) for the determination of seventeen pharmaceuticals in soils and sediments. The method is based on sample homogenisation using Na(2)-EDTA washed sand and extraction with water at 90 degrees C. Special emphasis was placed on the optimization of the extraction procedure to develop a green method that reduces, at a maximum, the use of organic solvents in order to eliminate matrix components during the clean-up. The proposed method was linear in a concentration range from 0.3 to 333ngg(-1), with correlation coefficients higher than 0.993. Method detection (MDLs) and quantification (MQLs) limits ranged from 0.1 to 6.8ngg(-1) and from 0.25 to 23ngg(-1), respectively. Absolute recoveries were analyte dependent, varying between 50% and 105% at the MQL level, except for fenofibrate (40%) and diclofenac (34%). The intra-day and inter-day precision was given by RSD values from 0.7% to 7.9% and from 1.6% to 14.5%, respectively. Acetaminophen, carbamazepine, ciprofloxacin, clofibric acid, codeine, diazepam, fenofibrate, metropolol, ofloxacin and propanolol were detected at concentrations from MDL to 35.62ngg(-1) in soils and sediments from marsh areas. Due to the low recoveries, results for fenofibrate and diclofenac can only be considered as semi-quantitative. The method was fully suitable for the other 15 pharmaceuticals.
Vazquez-Roig
Pablo
P
Laboratori de Bromatologia i Toxicologia, Facultat de Farmàcia, Universitat de València, Av. Vicent Andrés Estellés s/n, 46100 Burjassot, València, Spain. pablo.vazquez@uv.es
Segarra
Ramón
R
Blasco
Cristina
C
Andreu
Vicente
V
Picó
Yolanda
Y
D005591:Chemical Fractionation / Q000379:methods*; D002853:Chromatography, Liquid / Q000379:methods*; D019015:Geologic Sediments / Q000737:chemistry*; D016014:Linear Models; D004364:Pharmaceutical Preparations / Q000032:analysis* / Q000737:chemistry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012987:Soil / Q000032:analysis*; D012989:Soil Pollutants / Q000032:analysis*; D053719:Tandem Mass Spectrometry / Q000379:methods*
D004364:Pharmaceutical Preparations; D012987:Soil; D012989:Soil Pollutants