Easy Cheap Effective Rugged Safe Research Articles

Development of a Sensitive and Accurate Stable Isotope Dilution Assay for the Simultaneous Determination of Free 4-Hydroxy-2-(E)-Nonenal and 4-Hydroxy-2-(E)-Hexenal in Various Food Matrices by Gas Chromatography–Mass Spectrometry

An analytical method suitable for the determination of 4-hydroxy-2-(E)-nonenal (HNE) and 4-hydroxy-2-(E)-hexenal (HHE) in various food matrices was developed and validated. The method involves the use of deuterated HNE and HHE as internal standards, extraction of the analytes from the matrices followed by derivatization and detection with gas chromatography–mass spectrometry. Four different food matrices were chosen as model systems including vegetable oils, unprocessed meat, fried potato crisps, and infant formula and three different extraction techniques suitable for the different matrices were applied including the Quick Easy Cheap Effective Rugged Safe method. The simplicity of the extraction techniques allows the method to be applied for routine analysis of a large amount of samples. The results verify the accuracy and reproducibility of the analytical technique and its ability to provide reliable quantification of both analytes at concentrations as low as 12.8 ng g−1 in meat samples. Furthermore, a short overview of the levels of HNE and HHE in several products available in the Belgian market is presented.

Multiclass screening method based on solvent extraction and liquid chromatography–tandem mass spectrometry for the determination of antimicrobials and mycotoxins in egg

A QuEChERS (Quick Easy Cheap Effective Rugged Safe)-like extraction method was developed for the simultaneous analysis of veterinary drugs and mycotoxins in hen eggs by liquid chromatography–tandem mass spectrometry (LC–MS/MS) with electrospray (ESI) source. Various classes of antimicrobials (tetracyclines, ionophores, coccidiostats, penicillins, cephalosporins, fluoroquinolones, sulfonamides) and mycotoxins (enniatins, beauvericin, ochratoxins, aflatoxins) were considered for the development of this method. Particular attention was devoted to extraction optimization: different solvents (acetone, acetonitrile and methanol), different pH values and different sample to extracting volume ratios were tested and evaluated in terms of recovery, relative standard deviation (RSD) and ESI signal suppression due to matrix effect. Chromatographic and mass spectrometric conditions were optimized to obtain the best instrumental performances for most of the analytes. Quantitative analysis was performed by means of matrix-matched calibration, in a range that varied depending on the analyte and its established maximum limit, when there was one. Recoveries at 100μgkg−1 spiking level were >62% (3<RSD<17) for all the antimicrobials except lasalocid A (41±10%) and oxacillin (56±17%). The multiclass method proposed is rapid, simple, and involves a low solvent consumption, in line with QuEChERS features and modern analytical requirements.

Ultrasound‐assisted matrix solid phase dispersive extraction for the simultaneous analysis of β‐lactams (four penicillins and eight cephalosporins) in milk by high performance liquid chromatography with photodiode array detection

The application of ultrasound-assisted matrix solid phase dispersive extraction for the confirmatory analysis of 12 β-lactam antibiotics in milk by high performance liquid chromatography with photodiode array detection has been proposed herein. Four penicillins (cloxacillin, dicloxacillin, oxacillin, and amoxicillin) and eight cephalosporins (cefaclor, cefadroxil, ceftiofur, cefuroxime, cefoperazone, cefazolin, cephalexin, and cefotaxime) are effectively extracted using a mixed sorbent of Quick Easy Cheap Effective Rugged Safe technique and OASIS HLB providing a matrix free from any endogenous interference. Examined analytes were well resolved on an Inertsil ODS-3 analytical column with a mobile phase of CH(3)COONH(4) (0.05 M) and acetonitrile delivered under a gradient program. 1,7-Dimethyl-xanthine was used as internal standard. The method was validated meeting the European Legislation determining linearity, selectivity, stability, decision limit, detection capability, accuracy, precision, and ruggedness according to the Youden approach. Recoveries of all antibiotics rated from 85.0 to 115.7%, while RSD values were <12.7%. Finally, the method was successfully applied to milk samples purchased from local market.

QuEChERS Method for the Determination of PAH Compounds in Sardinia Sea Urchin (Paracentrotus lividus) Roe, Using Gas Chromatography ITMS-MS Analysis

Sea urchin roe (Paracentrotus lividus) is an excellent biomarker, and it has been used as a test for toxicology study of chemical pollution of restricted marine areas; in fact, unlike mussels which filter water, it feeds mainly on micro- and macroalgae. Therefore, it is not influenced by the sea tide and meets better the situation of local pollution. A modified Quick Easy Cheap Effective Rugged Safe extraction method coupled with gas chromatography ion trap mass spectrometry analysis has been used to set up a method for the determination of 17 polycyclic aromatic hydrocarbons (PAHs) in P. lividus sea urchin roe. A method validation was performed, and the following parameters have been determined: instrument limit of detection (LOD) and of quantification (LOQ), precision, recovery, and linearity. The method carried out showed good LOD under 1.5 μg/kg and LOQ under 5 μg/kg for all PAHs studied, and these values were in close agreement with quality criteria described in the Commission Regulation (EC) no. 333/2007 concerning the PAH benzo[a]pyrene in foodstuffs. Precision and linearity were in accordance with EC SANCO/10684/2009 values. For all PAHs, recoveries ranged from 72% to 119%, with RSD ranging from 3% to 17% in the most unfavorable case.