Accurate mass screening and identification of emerging contaminants in environmental samples by liquid chromatography–hybrid linear ion trap Orbitrap mass spectrometry (original) (raw)
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Journal of Chromatography A, 2012
Acidic pesticide and pharmaceutical contaminants were pre-concentrated and extracted from wastewater samples (500 mL) using solid-phase extraction. Analyte recoveries were 79-96%, with % RSD values in the range, 1.7-7.4%. Analyte identification and quantification were carried out using liquid chromatography-mass spectrometry (LC-MS) with hybrid linear ion trap (LIT) Orbitrap instrumentation. Using a resolution setting of 30,000 FWHM, full-scan MS analysis was performed using heated electrospray ionization (HESI) in negative mode. The high mass resolution capabilities of the Orbitrap MS were exploited for the determination of trace contaminants allowing facile discrimination between analytes and matrix. The dependant scan functions of the Orbitrap MS using higher collisional dissociation (HCD) and LIT MS were evaluated for the confirmation of analytes at trace concentration levels. Mass accuracy for target contaminants using this method was less than 2 ppm. The limits of quantitation (LOQs) were in the range, 2.1-27 ng/L. The inter-day accuracy and precision were measured over a five-day period at two concentrations. The % relative errors were in the range, 0.30-7.7%, and the % RSD values were in the range, 1.5-5.5%. Using this method, 2,4-D, mecoprop, ibuprofen, naproxene and gemfibrozil were identified in several wastewater treatment plants in Ireland.
Journal of Chromatography A, 2001
In order to assess and maintain the quality of surface waters, target compound monitoring is often not sufficient. Many unknown micro-contaminants are present in water, originating in municipal, industrial or agricultural effluents. Some of these might pose a risk to drinking water production and consequently to human health. The possibilities of screening surface water and identification of these non-target water pollutants with modern data acquisition possibilities of hybrid quadrupoleorthogonal acceleration time of flight mass spectrometers (Q-TOF), such as data-dependent MS to MS / MS switching were investigated. Using model compounds, a procedure for the liquid chromatography-tandem mass spectrometry (LC-MS / MS) screening of water extracts was developed, enabling the detection and identification of compounds at levels #0.25 mg/l in surface water. Based on the accurate mass the elemental compositions for the precursor and product ions are calculated. The calculated chemical formulae are searched against the Merck index, the NIST library, an own database containing about 2500 water pollutants (pesticides and other contaminants) as well as a CI-CID library containing tandem MS spectra of about 100 water contaminants. The developed approach was applied for the identification of unknown compounds, present in native surface water extract. For three of these compounds, structures were proposed. Confirmation of the proposed structures with standards was beyond the scope of this study.
Journal of Chromatography A, 2018
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2016
This application note describes the creation of an accurate mass library for relevant environmental contaminants and its application for the screening of pesticides, pharmaceuticals and personal care products, their metabolites, and transformation products in effluents of municipal waste water treatment plants (WWTPs). An Agilent 1290 Infinity LC System coupled to an Agilent 6550 iFunnel Q-TOF LC/MS System was operated in positive and negative electrospray mode using Dual Spray Agilent Jet Stream Technology. Accurate mass spectra were acquired for a large collection of potential environmental contaminants in either one or both ionization modes, and for all relevant ion species. Four WWTPs in central Europe were sampled over 3.5 months, and samples were analyzed using a Target Screening approach including reference standards for 390 contaminants. In addition, an extended suspect screening was done using all compounds included in the Agilent MassHunter Water Screening Personal Compoun...
Molecules
Different groups of organic micropollutants including pharmaceuticals and pesticides have emerged in the environment in the last years, resulting in a rise in environmental and human health risks. In order to face up and evaluate these risks, there is an increasing need to assess their occurrence in the environment. Therefore, many studies in the past couple of decades were focused on the improvements in organic micropollutants’ extraction efficiency from the different environmental matrices, as well as their mass spectrometry detection parameters and acquisition modes. This paper presents different sampling methodologies and high-resolution mass spectrometry-based non-target screening workflows for the identification of pharmaceuticals, pesticides, and their transformation products in different kinds of water (domestic wastewater and river water). Identification confidence was increased including retention time prediction in the workflow. The applied methodology, using a passive sa...
Journal of Chromatography A, 2012
A new approach for the analysis of pharmaceuticals (target and non-target) in water by LC-QTOF-MS is described in this work. The study has been designed to assess the performance of the simultaneous quantitative screening of target compounds, and the qualitative analysis of non-target analytes, in just one run. The features of accurate mass full scan mass spectrometry together with high MS/MS spectral acquisition rates-by means of information dependent acquisition (IDA)-have demonstrated their potential application in this work. Applying this analytical strategy, an identification procedure is presented based on library searching for compounds which were not included a priori in the analytical method as target compounds, thus allowing their characterization by data processing of accurate mass measurements in MS and MS/MS mode. The non-target compounds identified in river water samples were ketorolac, trazodone, fluconazole, metformin and venlafaxine. Simultaneously, this strategy allowed for the identification of other compounds which were not included in the library by screening the highest intensity peaks detected in the samples and by analysis of the full scan TOF-MS, isotope pattern and MS/MS spectra-the example of loratadine (histaminergic) is described. The group of drugs of abuse selected as target compounds for evaluation included analgesics, opioids and psychostimulants. Satisfactory results regarding sensitivity and linearity of the developed method were obtained. Limits of detection for the selected target compounds were from 0.003 to 0.01 g/L and 0.01 to 0.5 g/L, in MS and MS/MS mode, respectively-by direct sample injection of 100 L.
2013
The contamination of drinking water is potentially harmful and poses a risk to public health. If any observation suggests a potential contamination of drinking water, such as consumer complaints about the alteration of the water’s organoleptic properties, the appearance of health problems or an alarm triggered by sensors, a rapid identification of the hazard causing the problem is necessary. With regards to chemical contamination, EU Member States have several strategies to deal with the presence of unknown chemicals in water: there are screening methods as well as systematic approaches used for the analysis and identification of different groups of chemicals. This report provides a brief overview of the existing methods for the non-targeted screening of organic compounds in water samples by means of mass spectrometry. This review is thus based on the studies and explorations that can be performed by different mass spectrometry approaches. In addition, the most relevant European ins...
Journal of Chromatography A, 2011
In this work, a multiclass screening method for organic contaminants in natural and wastewater has been developed and validated for qualitative purposes, i.e. to ensure the reliable and sensitive identification of compounds detected in samples at a certain level of concentration. The screening is based on the use of GC-TOF MS, and the sample procedure involves solid phase extraction with C 18 cartridges. Around 150 organic contaminants from different chemical families were investigated, including PAHs, octyl/nonyl phenols, PCBs, PBDEs and a notable number of pesticides, such as insecticides (organochlorines, organophosphorus, carbamates and pyrethroids), herbicides (triazines and chloroacetanilides), fungicides and several relevant metabolites. Surface water, ground water and effluent wastewater were spiked with all target analytes at three concentration levels (0.02, 0.1 and 1 g/L). Influent wastewater and raw leachate from a municipal solid waste treatment plant were spiked at two levels (0.1 and 1 g/L). Up to five m/z ions were evaluated for every compound. The identification criterion was the presence of, at least, two m/z ions at the expected retention time, measured at their accurate mass, and the accomplishment of the Q/q i intensity ratio within specified tolerances. The vast majority of compounds investigated were correctly identified in the samples spiked at 1 g/L. When analyte concentration was lowered down to 0.1 g/L the identification was more problematic, especially in complex-matrix samples like influent wastewater. On the contrary, many contaminants could be properly identified at the lowest level 0.02 g/L in cleaner matrices. The procedure was applied to the screening of water samples of different origin and matrix composition and allowed the detection of several target contaminants. A highly reliable identification could be carried out thanks to the sensitive full-spectrum acquisition at accurate mass, the high selectivity reached with the use of narrow-mass window extracted ion chromatograms, the low mass errors observed in the positive detections and the Q/q ratio accomplishment.
Journal of Chromatography A, 2009
We describe the development and validation of an on-line solid-phase extraction of large-volume injections coupled to liquid chromatography-tandem mass spectrometry method for the simultaneous quantitation and confirmation of 14 selected trace organic contaminants in drinking and surface water. Selected compounds were: anti-infectives (clarithromycin, sulfamethoxazole and trimethoprim), an anticonvulsant (carbamazepine) and its transformation product 10,11-dihydrocarbamazepine, an antihypertensive (enalapril), antineoplastics (cyclophosphamide and methotrexate), herbicides (atrazine, cyanazine, and simazine) and two of their transformation products (deethylatrazine and deisopropylatrazine) and an antiseptic (triclocarban). The breakthrough volume determinations showed that out of all the investigated sorbents, the Strata-X on-line solid-phase extraction column showed the best performance. The method used a load volume of 10.0 mL and was validated using the corresponding matrices, yielding for most compounds, R 2 > 0.99. Extraction recoveries ranged from 60 to 109%. The intra-and inter-day precision were <14 and <16%, respectively. The method detection limits ranged from 0.6 to 6 ng L −1 . Matrix effects were in general low. The performance of the on-line method was demonstrated with the analysis of real water samples. The application of alternative techniques of confirmation was also explored using accurate mass measurements on a time-of-flight mass spectrometer and the data-dependent reverse energy ramp scan on a triple quadrupole.