Analysis of meat samples for anabolic steroids residues by liquid chromatography/tandem mass spectrometry.

A rapid, specific and highly sensitive multi-residue method for the determination of anabolic steroid residues in bovine, pork and poultry muscle tissues was developed. The sample preparation involves enzymatic digestion followed by extraction with methanol. The crude extract was cleaned up by solid-phase extraction (SPE) combining C18 and NH2 columns. The detection was carried out by a highly sensitive liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) method using both positive and negative ionization modes. Natural and synthetic steroids covering different polarities could be extracted, concentrated and purified using one single method. Mobile phase com…

Procedures for Antibiotic Residues in Bovine Muscle Tissues

Abstract Acetonitrile extraction followed by primary-secondary amine dispersive SPE cleanup QuEChERS (quick, easy, cheap, effective, rugged, and safe), was compared to pressurized liquid extraction (PLE) using water at 70°C for 10 min at 1500 psi for the determination of 16 veterinary drugs in bovine muscle tissues by LC/MS/MS. PLE was significantly more effective for the extraction of veterinary drugs (ranging from 69 to 103% with RSD ≤ 18%) than QuEChERS (ranging from 19 to 89% with RSD ≤ 19%). Linearity of the calibration curves was obtained over the range considered (from 10 μg/kg or LOQ to 1000, μg/kg) with r2 ≥ 0.99 for all the analytes by both methods. Although an internal standard w…

Multiple-stage mass spectrometric analysis of six pesticides in oranges by liquid chromatography–atmospheric pressure chemical ionization–ion trap mass spectrometry

Abstract Six pesticides were determined by liquid chromatography (LC) with positive ion (PI) atmospheric pressure chemical ionization quadrupole ion-trap tandem mass spectrometry (APCI–MS–MS). Ion fragmentation was studied by MS, MS 2 and MS 3 . Fragmentation of the pesticides produced ions formed by various losses from the side-chains and through heterocyclic ring opening, but without any common fragmentation pathway. Multiple reaction monitoring (MRM) of MS, MS 2 and MS 3 was used to identify and quantify the pesticides. The samples were extracted with ethyl acetate and dried over anhydrous sodium sulfate. Comparison of the three MS modes showed that MS 3 is slightly less sensitive but mu…

Risk assessment on the presence of pharmaceuticals in sediments, soils and waters of the Pego-Oliva Marshlands (Valencia, eastern Spain).

9 páginas, 3 figuras, 2 tablas.

Analytical method for simultaneous determination of pesticide and veterinary drug residues in milk by CE-MS

10 páginas, 2 figuras, 4 tablas.

Comparison of microextraction procedures to determine pesticides in oranges by liquid chromatography-mass spectrometry.

A liquid chromatographic-mass spectrometric method has been developed for the determination of bitertanol, carbendazim, fenthion, flusilazole, hexythiazox, imidacloprid, methidathion, methiocarb, pyriproxyfen and trichlorfon. Two procedures, based on stir bar sorptive extraction (SBSE) and matrix solid-phase dispersion (MSPD), have been evaluated for the extraction of these compounds in oranges. Their respective advantages and disadvantages are also discussed. The recoveries obtained by MSPD ranged from 47 to 96% and the relative standard deviations (RSDs) ranged from 1 to 15%, whereas with the SBSE method the recoveries were between 8 and 84% and the RSDs between 4 and 16%. Although, the l…

Liquid chromatography-mass spectrometry in food safety.

Abstract The use of powerful mass spectrometric detectors in combination with liquid chromatography has played a vital role to solve many problems related to food safety. Since this technique is especially well suited for, but not restricted to the analysis of food contaminants within the food safety area, this review is focused on providing an insight into this field. The basic legislation in different parts of the world is discussed with a focus on the situation within the European Union (EU) and why it favors the use of liquid chromatography–mass spectrometry (LC–MS). Main attention in this review is on the achievements that have been possible because of the latest advances and novelties…

Combined use of liquid chromatography triple quadrupole mass spectrometry and liquid chromatography quadrupole time-of-flight mass spectrometry in systematic screening of pesticides and other contaminants in water samples

As a suitable way for routine screening of pesticides and control of other organic contaminants in water, the combination of liquid chromatography triple quadrupole tandem mass spectrometry (LC-QqQ-MS/MS) and liquid chromatography-hybrid quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) has been applied to the analysis of 63 surface and waste water samples after conventional solid-phase extraction (SPE). The extracts were screened for 43 pesticides or degradation products by LC-QqQ-MS/MS achieving limits of detection (LOD) ranged from 0.04 to 2 ng L(-1). Of the 43 selected pesticides, 33 were detected in water samples. The ESI-QTOF MS instrument was run using two simultaneous acquisi…

Comparison of solid-phase microextraction and stir bar sorptive extraction for determining six organophosphorus insecticides in honey by liquid chromatography-mass spectrometry.

Abstract Two approaches based on sorptive extraction, solid-phase microextraction (SPME) and stir bar sorptive extraction (SBSE), in combination with liquid chromatography (LC)–atmospheric pressure chemical ionization mass spectrometry (MS) have been assayed for analyzing chlorpyriphos methyl, diazinon, fonofos, phenthoate, phosalone, and pirimiphos ethyl in honey. In both, SPME and SBSE, enrichment was performed using a poly(dimethylsiloxane) coating. Significant parameters affecting sorption process such as sample volume, sorption and desorption times, ionic strength, elution solvent, and dilution (water/honey) proportion were optimized and discussed. Performance of both methods has been …

Nanoparticles in Foods, Determination of

This article discusses the state of the art in the identification and determination of nanoparticles in food. It is of utmost importance to determine, in addition to the particle-size distribution, the chemical composition as well as the physical and chemical properties of the nanomaterials within the sample. After a brief description of what nanomaterials are and how to classify them, sources and routes of nanomaterials to food are discussed. The article then follows the debate on legislative consideration, which has emerged very recently. Its main aim is to deliver information on how nanomaterials are determined in food because of the number of challenges that arise when analyzing food an…

Advances in the analysis of legal and illegal drugs in the aquatic environment

We review the current methods developed for the analysis of legal and illegal drugs (LIDs) and their metabolites in environmental samples. We discuss the advantages and the pitfalls of multi-class methods with emphasis on new strategies for sample preparation and recent technical developments. Finally, we present the applicability of these methods to the analysis of LIDs in protected environmental areas.

Simultaneous determination of imidacloprid, carbendazim, methiocarb and hexythiazox in peaches and nectarines by liquid chromatography–mass spectrometry

Abstract A liquid chromatographic (LC) atmospheric pressure chemical ionization mass spectrometric (MS) method is described for determining imidacloprid, carbendazim, methiocarb and hexythiazox in peaches and nectarines. The samples were extracted with ethyl acetate and anhydrous sodium sulfate. Recoveries yield for spiking samples were ranged from 64±9% (R.S.D) for carbendazim to 108±14% (R.S.D.) for hexythiazox at the concentration of 0.1 mg kg−1 (n=5). The correlation coefficients were greater than 0.998 over the range between 0.02 and 2 mg kg−1. The limits of quantitation (LOQ) were 0.02 mg kg−1 for all the pesticides. The applicability of the method to detect and quantify imidacloprid,…

Determination of benzoylurea insecticides in food by pressurized liquid extraction and LC-MS

A method based on pressurized liquid extraction and LC-MS/MS has been developed for determining nine benzoylureas (BUs) in fruit, vegetable, cereals, and animal products. Samples (5 g) were homogenized with diatomaceous earth and extracted in a 22 mL cell with 22 mL of ethyl acetate at 80 degrees C and 1500 psi. After solvent concentration and exchange to methanol, BUs were analyzed by LC-MS/MS using an IT mass analyzer, which achieved several transitions of precursor ions that increase selectivity providing identification. LOQs were between 0.002 and 0.01 mg/kg, which are equal or lower than maximum residue limits established by the Codex Alimentarius. Excellent linearity was achieved over…

Determining nanomaterials in food

Abstract Nanotechnology has emerged as one of the most innovative technologies and has the potential to improve food quality and safety. However, there are a few studies demonstrating that nanomaterials (NMs) are not inherently benign. This review highlights some current applications of NMs in food, food additives and food-contact materials, and reviews analytical approaches suitable to address food-safety issues related to nanotechnology. We start with a preliminary discussion on the current regulatory situation with respect to nanotechnology in relation to foods. We cover sample preparation, imaging techniques (e.g., electron microscopy, scanning electron microscopy and X-ray microscopy),…

Determination of fungicide residues in fruits and vegetables by liquid chromatography–atmospheric pressure chemical ionization mass spectrometry

Abstract A liquid chromatography (LC) method for the quantitative determination of five fungicide residues (dichloran, flutriafol, o -phenylphenol, prochloraz and tolclofos methyl) in oranges, lemons, bananas, peppers, chards and onions is described. The residues were extracted by matrix solid-phase dispersion (MSPD) using C 8 . Quantitative analysis was performed by isocratic LC coupled to quadrupole mass spectrometer using atmospheric pressure chemical ionization in the negative ionization mode. The limit of quantification was 0.01 mg kg −1 for flutriafol, o -phenylphenol and dichloran, and 0.1 mg kg −1 for prochloraz and tolclofos methyl. The MSPD method is also suitable for LC–UV analys…

Stereoisomeric profiling of drugs of abuse and pharmaceuticals in wastewaters of Valencia (Spain)

AbstractThe enantiomeric and diastereomeric profiling of chiral pharmaceuticals (ephedrine, norephedrine, atenolol and venlafaxine) and illicit drugs (amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxy-N-methylamphetamine (MDMA) and 3,4-methylenedioxy-N-ethylamphetamine (MDEA)) was undertaken over a period of fourteen consecutive days in three wastewater treatment plants (WWTPs) in the city of Valencia, Spain. Degradation efficiency of WWTPs was found to be compound and enantiomer dependent. Selective enantiomer enrichment was observed for several target analytes. Amphetamine and MDMA were enriched with R(−)-enantiomers. 1S,2S(+)-pseudoephedrine was found …

Screening of currently used pesticides in water, sediments and biota of the Guadalquivir River Basin (Spain)

The occurrence of 50 currently used pesticides and their transformation products in surface and waste waters, sediment and fish in the Guadalquivir River Basin was determined in 2010 and 2011. After selective sample extraction, pesticides were identified and quantified by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). The contamination profile in water and sediments is marked by the presence of organophosphorus and triazines. Transformation products were even at higher concentrations than parent pesticides. A wider range of pesticides was present in water than in sediments but none of them were detected in fish. The mean concentrations ranged from 0.2 to 13.0 ng/L in …

Progress in analysis of residual antibacterials in food

Abstract Residual antibacterials in food constitute a risk to human health. Although epidemiological data on the real magnitude of their adverse effects are very scarce, they indicate that food could be an important avenue for evolution and dissemination of antibiotic-resistant bacteria. Analysis of these residues plays a key role in ensuring food safety, to the point that the European Union has not only established maximum residue limits but also requirements concerning the performance of analytical methods and the interpretation of the results. These specifications have had a great influence on protocols and techniques applied. In this review, we discuss the progress of rapid screening me…

Multi-class determination of antimicrobials in meat by pressurized liquid extraction and liquid chromatography–tandem mass spectrometry

A multi-residue method using pressurized liquid extraction (PLE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed for determining trace levels of 31 antimicrobials, including beta-lactams, lincosamides, macrolides, quinolones, sulfonamides, tetracyclines, nitroimidazoles and trimethoprim. The extraction method required pre-homogeneization of the meat with EDTA-washed sand and subsequent one-static-cycle extraction for 10 min with 40 ml of water at 1500 psi and 70 degrees C. The effect of operation temperature, pressure, flush volume, and static cycles on PLE performance was studied. Average recoveries ranged from 75 to 99% with relative standard deviations <1…

Occurrence and removal efficiency of pesticides in sewage treatment plants of four Mediterranean River Basins.

Removal of contaminants in the sewage treatment plants (STPs) can be incomplete causing their release to the environment. In this paper, the results of an extensive survey on more than 40 pesticides carried out in 2010 and 2011 in 16 STPs of Ebro, Guadalquivir, Jucar and Llobregat Rivers (Spain) are presented. In 2010, of 43 analytes screened, 29 were detected in influent and 28 in effluent samples, meanwhile in 2011, of 50 analytes, 33 and 34 were detected, respectively. Pesticides were in the range of 0.33 ng L(-1) (terbumeton, 2011)-2526.05 ng L(-1) (diuron, 2010) for influent and 0.25 ng L(-1) (terbumeton, 2011)-2821.12 ng L(-1) (carbendazim, 2011) for effluent. Regarding the sludge sam…

Monitoring of five postharvest fungicides in fruit and vegetables by matrix solid-phase dispersion and liquid chromatography/mass spectrometry

Abstract A method was developed for monitoring dichloran, flutriafol, o-phenylphenol, prochloraz, and tolclofos-methyl in fruits and vegetables, using matrix solid-phase dispersion and liquid chromatography with mass spectrometry detection. The method was used to determine fungicide content in 200 samples of chards, onions, peppers, bananas, lemons, and oranges. Of the samples examined, 54% contained o-phenylphenol with concentrations ranging from 0.005 to 3.34 mg/kg and 35% showed prochloraz in the range of 0.06–1.95 mg/kg. Dichloran, flutriafol, and tolclofos-methyl were detected only occasionally. Only 4% of the samples exceeded the European Union maximum residue limits. The pesticides i…

Last trends in pesticide residue determination by liquid chromatography–mass spectrometry

Liquid chromatography–mass spectrometry (LC–MS) is as an excellent analytical tool in the determination of pesticides. Multiresidue analysis of these compounds at trace levels is one of the oldest analytical schemes within environmental and food safety. However, the issue of “pesticide residue determination” is still a hot topic for the analytical community. This review discusses current approaches and recent advances in using LC–MS for pesticide identification and quantification. We outline how MS has influenced the sample preparation process. We critically assess and compare various mass spectrometers, highlighting their strengths and limitations. We, then, review the main applications of…

Development of an improved method for trace analysis of quinolones in eggs of laying hens and wildlife species using molecularly imprinted polymers.

A sensitive, selective, and efficient method was developed for simultaneous determination of 11 fluoroquinolones (FQs), ciprofloxacin, danofloxacin, difloxacin, enrofloxacin, flumequine, marbofloxacin, norfloxacin, ofloxacin, oxolinic acid, pipemidic acid, and sarafloxacin, in eggs by molecularly imprinted polymer (MIP) and column liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS). Samples were diluted with 50 mM sodium dihydrogen phosphate at pH 7.4, followed by purification with a commercial MIP (SupelMIP SPE-Fluoroquinolones). Recoveries for the 11 quinolones were in the range of 90-106% with intra- and interday relative standard deviation ranging from …

Solid-Phase Microextraction Liquid Chromatography/Tandem Mass Spectrometry To Determine Postharvest Fungicides in Fruits

A method to determine five postharvest fungicides (dichloran, flutriafol, o-phenylphenol, prochloraz, tolclofos methyl) in fruits (cherries, lemons, oranges, peaches) has been developed using solid-phase microextraction (SPME) coupled to liquid chromatography (LC) with photodiode array (DAD), mass spectrometry (MS), or tandem mass spectrometry (MS/MS) with ion trap detection. Extraction involved sample homogenization with an acetone/water solution (5:1), filtration, and acetone evaporation prior to fiber extraction. The pesticides were isolated with a fused-silica fiber coated with 50-microm Carbowax/template resin. The effects of pH, ion strength, sample volume, and extraction time were in…

Analysis of pesticides in fruits by pressurized liquid extraction and liquid chromatography-ion trap-triple stage mass spectrometry.

A multi-residue method using pressurized liquid extraction (PLE) and liquid chromatography-quadrupole ion trap-triple stage mass spectrometry (LC-IT-MS(3)) has been developed for determining trace levels of pesticides in fruits. The selected pesticides can be distinguished in: benzimidazoles and azoles, organophosphorus, carbamates, neonicotinoids, and acaricides. PLE has been optimized to extract these pesticide residues from oranges and peaches by studying the effect of experimental variables on PLE efficiency. Samples were extracted at high temperature and pressure (75 degrees C and 1500psi) using ethyl acetate as extraction solvent and acidic alumina as drying agent. The recoveries obta…

Nanomaterials in Food, Which Way Forward?

Abstract Nanotechnology has emerged as one of the most innovative technologies occurred in decades and has the potential to improve food quality and safety. At present, there are also a few studies demonstrating that nanomaterials (NMs) are not inherently benign. This chapter highlights some current applications of NMs in food, food additives and food contact materials and reviews analytical approaches suitable to address food safety-related issues of nanotechnology. As starting point, discussion on the current regulatory situation of nanotechnology in relation to food is addressed, followed by a detailed description of sample preparation aspects, separation methods (e.g. field-flow fractio…

Perfluoroalkyl substances in Breast milk, infant formula and baby food from Valencian Community (Spain)

Environmental and human exposures to perfluoroalkyl substances (PFASs) are of emerging concern since they are persistent and bioaccumulative. The present study reports PFASs levels in human milk, infant formulas and baby food (dry cereals and pots) from the Valencian Community (Spain) in order to evaluate the infant exposure to these substances through the diet. The results show that perfluorobutanoic acid (PFBA) and perfluorooctanoic acid (PFOA) were in all the samples of the four selected matrices (except PFOA in one sample of dry cereal baby food). Perfluoroheptanoic acid (PFHpA) and perfluorodecanoic acid (PFDA) were also detected in 70% of the breast milk samples. In infant formulas, P…

Prospects for combining chemical and biological methods for integrated environmental assessment

Abstract Inherently interdisciplinary, environmental assessment applied to contamination is evolving rapidly, despite associated uncertainties in methodologies and data limitations. Mixtures of known and unknown pollutants can cause toxic effects in the environment. Besides deploying a chemicals-driven strategy for the ecological risk assessment of the pollutants, it is necessary to apply and to explore biological strategies. Consequently, bioassays, biosensors and effect-directed analysis (EDA) to identify pollutants responsible of particular effects have become increasingly important. We give a broad overview of how to assess biological monitoring of ecosystems and chemical monitoring of …

Ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry to identify contaminants in water: an insight on environmental forensics.

Ultra-high pressure liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-QqTOF-MS) acquiring full scan MS data for quantification, and automatic data dependent information product ion spectra (IDA-MS/MS) without any predefinition of the ions by the user was checked for identifying organic contaminants in water samples. The use of a database with more than 2000 compounds achieved high confidence results for a wide number of contaminants based upon retention time, accurate mass, isotopic pattern and MS/MS library searching. More than 20 contaminants, mostly pharmaceuticals, but also mycotoxins and polyphenols were unambiguously identified. Furthermore, the combination of s…

Solid-phase microextraction-liquid chromatography-mass spectrometry applied to the analysis of insecticides in honey

An approach based on solid-phase microextraction-liquid chromatography-mass spectrometry (SPME-LC-MS) has been developed for determining 12 insecticides (bromophos ethyl, chlorpyrifos methyl, chlorpyrifos ethyl, diazinon, fenoxycarb, fonofos, phenthoate, phosalone, pirimiphos methyl, profenofos, pyrazophos, and temephos) in honey. The influence of several parameters on the efficiency of the SPME was systematically investigated. Under optimal conditions, the procedure provided excellent linearity (>0.990), detection and quantification limits (between 0.001 and 0.1 microg g(-1) and between 0.005 and 0.5 microg g(-1), respectively), and precision (<19% at the quantification limits and from 6 t…

Determination of pharmaceuticals in soils and sediments by pressurized liquid extraction and liquid chromatography tandem mass spectrometry

13 páginas, 4 figuras, 6 tablas.

Analytical utility of quadrupole time-of-flight mass spectrometry for the determination of pesticide residues in comparison with an optimized column high-performance liquid chromatography/tandem mass spectrometry method.

Abstract A multiresidue method for the analysis of 30 pesticides with different physicochemical properties in fruits and vegetables was developed. The method involves a rapid and small-scale extraction procedure based on matrix solid-phase dispersion using octadecylsilyl (C18) as the dispersant and dichloromethane as the eluent. The target pesticides were determined using column high-performance liquid chromatography/triple quadrupole-tandem mass spectrometry (LC/QqQ-MS/MS). The method was validated for sensitivity, linearity, reproducibility, and accuracy. A recovery study was conducted at 3 different levels, and the average ranged from 74 to 99 for all of the studied compounds, with relat…

Liquid chromatography-mass spectrometry

Analytical strategies to determine quinolone residues in food and the environment

23 páginas, 5 figuras, 5 tablas.

Analysis of insecticides in honey by liquid chromatography–ion trap-mass spectrometry: Comparison of different extraction procedures

The feasibility of different extraction procedures was tested and compared for the determination of 12 organophosphorus and carbamates insecticides in honey samples. In this sense, once the samples were pre-treated - essentially dissolved in hot water by stirring - and before they could be analyzed by liquid chromatography-ion trap-second stage mass spectrometry (LC-MS(2)), four different approaches were studied for the extraction step: QuEChERS, solid-phase extraction (SPE), pressurized liquid extraction (PLE) and solid-phase microextraction (SPME). The main aim of this work was to maximise the sensitivity of pesticides and to minimise the presence of interfering compounds in the extract. …

Determination of organochlorine pesticide residues in honey from the central zone of Portugal and the Valencian community of Spain

In this study nine organochlorine pesticide residues ([alpha]-, [beta]-, and [gamma]-hexachlorocyclohexane (HCH), hexachlorobenzene (HCB), aldrin, p,p'-DDE, p,p'-DDD, o,p'-DDT, and p,p'-DDT) in forty nine samples of honey collected from markets of Portugal and Spain during 2001 and 2002, respectively, were evaluated. For this evaluation, three analytical procedures were studied. The analytical procedure, based on LLE extraction with ethyl acetate followed by gas chromatography-electron-capture detection (GC-ECD) for quantification, and mass spectrometry (GC-MS) for confirmation, has been selected. Recoveries of spiked samples ranged from 68%, for [beta]-HCH, and 126% for p,p'-DDT, for forti…

Determination of dithiocarbamates and metabolites in plants by liquid chromatography–mass spectrometry

Abstract A quantitative matrix solid-phase dispersion and liquid chromatography–atmospheric pressure chemical ionization mass spectrometry (LC–APCI–MS) method is outlined for the simultaneous analysis of dithiocarbamates (DTCs) and their degradation products in plants. Compounds analyzed are dazomet, disulfiram, thiram and the metabolites ethylenthiourea and propylenthiourea. The performance of two different sample preparation protocols, the proposed one and other based on solid-phase extraction, as well as, of both atmospheric pressure ionization sources, APCI and electrospray, were compared. The effect of several parameters on the extraction, separation and detection was studied. Dithioca…

Environmental and food applications of LC-tandem mass spectrometry in pesticide-residue analysis: An overview

An overview is given on pesticide-residue determination in environmental and food samples by liquid chromatography/mass spectrometry/mass spectrometry (LC/MS/MS). Pesticides comprise a large number of substances that belong to many completely different chemical groups, the only common characteristic is that they are effective against pests. They still constitute a challenge in MS because there is no collective pathway for fragmentation. A brief introduction to the theory of tandem MS permits a discussion of which parameters influence the ionization efficiency when the ions are subjected to different actions. Emphasis is placed on the different tandem MS instruments: triple and ion-trap quad…

Assessment of Pesticide Residues in Honey Samples from Portugal and Spain

Fifty samples of honey collected from local markets of Portugal and Spain during year 2002 were analyzed for 42 organochlorine, carbamate, and organophosphorus pesticide residues. An analytical procedure based on solid-phase extraction with octadecyl sorbent followed by gas chromatography-mass spectrometry (GC-MS), for organochlorines, and by liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry (LC-APCI-MS), for organophosphorus and carbamates, has been developed. Recoveries of spiked samples ranged from 73 to 98%, except for dimethoate (40%), with relative standard deviations from 3 to16% in terms of repeatability, and from 6 to 19% in terms of reproducibility. …

Evaluation of 10 pesticide residues in oranges and tangerines from Valencia (Spain)

Abstract One hundred and sixteen orange and tangerine samples from an agricultural cooperative of the Valencian Community (Spain) were analyzed for bitertanol, carbendazim, hexythiazox, imazalil, imidacloprid, methidathion, methiocarb, pyriproxyfen, thiabendazole, and trichlorfon by liquid chromatography–mass spectrometry (LC–MS) after a conventional multiresidue extraction procedure. Of 52 samples that contained pesticide residues, carbendazim was detected in 27 (51.9%) in the concentration range of 0.02–0.04 mg kg−1, hexythiazox in 22 (42.3%) in the concentration range of 0.02–0.05 mg kg−1, imazalil in 8 (15.0%) in the concentration range of 0.02–1.2 mg kg−1, imidacloprid in 5 (9.6%) in a…

Determination of tetracyclines in multi-specie animal tissues by pressurized liquid extraction and liquid chromatography–tandem mass spectrometry

Abstract A specific, sensitive and robust pressurized liquid extraction (PLE) and liquid chromatography tandem mass spectrometry (LC–MS/MS) method for determining tetracycline, chlortetracycline, oxytetracycline and doxycycline in bovine, swine, poultry and lamb muscle tissues is presented. PLE was performed using an ASE ® 200 from Dionex and water as extractant, followed by solid-phase extraction (SPE) using an Oasis HLB cartridge. The method was validated for beef, chicken, pork and lamb meat in compliance with the requirements set by Commission Decision, 2002/657/EC [Commission Decision 2002/657/EC (2002). Implementing Council Directive 96/23/EC concerning the performance of analytical m…