Multi-residue method for trace level determination of pharmaceuticals in solid samples using pressurized liquid extraction followed by liquid chromatography/quadrupole-linear ion trap mass spectrometry.
ABSTRACT A simple and sensitive method for simultaneous analysis of 43 pharmaceutical compounds in sewage sludge and sediment samples was developed and validated. The target compounds were extracted using pressurized liquid extraction (PLE) and then purified and pre-concentrated by solid phase extraction (SPE) using a hydrophilic-lipophilic balanced polymer. PLE extraction was performed on temperature of 100 degrees C, with methanol/water mixture (1/2, v/v) as extraction solvent. The quantitative analysis was performed by liquid chromatography tandem mass spectrometry using a hybrid triple quadrupole-linear ion trap mass spectrometer (LC-QqLIT-MS). Data acquisition was carried out in selected reaction monitoring (SRM) mode, monitoring two SRM transitions to ensure an accurate identification of target compounds in the samples. Additional identification and confirmation of target compounds were performed using the Information Dependent Acquisition (IDA) function. The method was validated through the estimation of the linearity, sensitivity, repeatability, reproducibility and matrix effects. The internal standard approach was used for quantification because it efficiently corrected matrix effects. Despite the strong matrix interferences, the recoveries were generally higher of 50% in both matrixes and the detection and quantification limits were very low. Beside the very good sensitivity provided by LC-QqLIT-MS, an important characteristic of the method is that all the target compounds can be simultaneously extracted, treated and analysed. Hence, it can be used for routine analysis of pharmaceuticals providing large amount of data. The method was applied for the analysis of pharmaceuticals in river sediment and wastewater sludge from three treatment plants with different treatment properties (i.e. capacity, secondary treatment, quality of influent waters). The analysis showed a widespread occurrence of pharmaceuticals in the sludge matrices.
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ABSTRACT: The aim of this study was to develop an analytical method for the analysis of a wide range of hormonal steroids and pharmaceutical compounds in sewage sludge. Thus, 136 substances were selected, including 119 pharmaceuticals and 17 hormonal steroids. An innovative sample preparation procedure based on the quick, easy, cheap, effective, rugged and safe (QuEChERS) method was developed. The analysis was then performed using liquid chromatography coupled with time-of-flight mass spectrometry. This analytical procedure was validated by evaluating the specificity, quadratic curve fitting, recovery, reproducibility and limits of detection and quantification. The method allows the analysis of the majority of the target compounds with limits of detection ranging from 1ng/g to 2500ng/g, depending on the nature of the substance. The protocol was then successfully applied to various types of sludge (limed, digested, dried, liquid and composted) collected in several sewage works in France. Among the target compounds, 34 were quantified at levels up to 6000ng/g. Among the most commonly detected pharmaceuticals were the antiemetic domperidone (mean concentration 769ng/g) and the antiepileptic lamotrigine (mean concentration 31ng/g) whose presence had, to our knowledge, never been shown in sludge.Journal of Chromatography A 03/2013; · 4.61 Impact Factor
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ABSTRACT: Non-steroid anti-inflammatory drugs (NSAIDs) are frequently occurring in sludge and waters from sewage treatment plants (STPs). Sludge obtained from sewage treatment is often applied as a fertilizer in agriculture and not many studies about the uptake of pharmaceuticals into crops can be found. In this paper, we present a greenhouse experiment to study the presence of four NSAIDs (naproxen, ketoprofen, diclofenac and ibuprofen) in two different crops (soybean and wheat) after application of sludge as a fertilizer. Two different amounts of sludge were added to the soil; the recommended amount (with respect to phosphorus content) and the double recommended amount. One treatment without sludge was also included as a blank. The crops were harvested after 60 as well as 110days. Only diclofenac and ibuprofen were detected in the sludge in concentrations of 22 and 217ngg-1 dry weight, respectively. None of the NSAIDs were detected in the crops from any of the treatments. Compared to the amounts applied to the soil, detection limits correspond to an uptake of less than 2% for diclofenac and 0.8% for ibuprofen.Science of The Total Environment 02/2013; 449C:385-389. · 3.26 Impact Factor
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ABSTRACT: The presence of pharmaceuticals in aquatic environment has become a topic of concern because of their potential adverse effects on human health and wildlife species. A total of 45 dewatered sewage sludge samples were collected throughout China and analyzed for 30 commonly consumed pharmaceutical residues. Ofloxacin was found to be the dominant contaminant with concentrations up to 24760μgkg(-1), followed by oxytetracycline (5280μgkg(-1)), norfloxacin (5280μgkg(-1)) and ketoprofen (4458μgkg(-1)). The concentration of pharmaceutical residues varied greatly depending on the operation conditions of wastewater treatment plants and sampling locations. Poor agreement was found between the predicted (calculation based on the annual consumption and coefficient of sludge water partition) and detected concentrations of the pharmaceuticals indicating that the occurrence of pharmaceutical residues was affected by various factors such as loading rates, sewage properties and the chemical properties such as the contribution from polar groups. National wide fate and ecotoxicity study is required for the development of control strategies.Chemosphere 07/2013; · 3.14 Impact Factor