Screening and Analysis of Multiclass Veterinary Drug Residues in Animal Source Foods using UPLC-Q-Exactive Orbitrap/MS

A rapid, simple, and sensitive method of detecting veterinary drug residues in animal food sources, including poultry and pork, was developed and validated. The method was optimized for over 155 veterinary drugs of 21 different classes. Sample pretreatment included a simple solid-liquid extraction step with 0.2% formic acid-acetonitrile-water and a purification step with a PRiME HLB (hydrophile-lipophile balance) solid-phase extraction cartridge. Data were collected using ultra-high-performance liquid chromatography coupled to Quadrupole-Exactive Orbitrap mass spectrometry. The limits of detection of 155 veterinary drugs ranged from 0.1 µg/kg to 10 µg/kg. The recovery rates were between 79.2 and 118.5 % in all matrices studied, with relative standard deviation values less than 15% (n = 6). The evaluated method allows the reliable screening, quantification, and identification of 155 veterinary drug residues in animal source food and has been successfully applied in authentic samples.

Mycotoxin Determination in Animal Feed: An LC-FLD Method for Simultaneous Quantification of Aflatoxins, Ochratoxins and Zearelanone in This Matrix

Mycotoxins are toxic compounds for humans and animals that are produced by fungi. Mycotoxin contamination in feed is a global safety concern and effective control of these compounds in this matrix is needed. This study proposes a simple, cost-effective analytical method based on liquid chromatography coupled with a fluorescence detector, which is suitable for the routine monitoring of some of the most important mycotoxins in feed: aflatoxins (G2, G1, B2, and B1), zearalenone, and ochratoxins A and B. Mycotoxin extraction, chromatographic separation and quantification are carried out simultaneously for all mycotoxins. The extraction procedure is performed using acetonitrile, water and orthophosphoric acid (80:19:1). Purification of the extract is carried out using an OASIS PRIME HLB solid-phase extraction cartridge followed by a dispersive liquid–liquid microextraction procedure. Aflatoxins G1 and B1 are derivatized post-column (photochemical reactor at 254 nm) to increase their signal. The method has been validated in feed for pigs, cows, sheep, and poultry with very satisfactory results. The detection limits are 2 μg/kg for aflatoxins B1 and G1, 0.64 μg/kg for aflatoxins B2 and G2, 42 μg/kg for zearalenone, and 5 μg/kg for ochratoxins A and B. These values are low enough to allow for monitoring of these mycotoxins in feed. Global recovery values were between 73.6% and 88.0% for all toxins with a relative standard deviation (RSD) % < 7%. This methodology will facilitate laboratory control and analysis of mycotoxins in feed.

Improved method for determination of waxes in olive oils: reduction of silica and use of a less hazardous solvent

The evaluation of the content of waxes is request both by IOC Trade Standard and by Regulation (EEC) 2568/91 and its further amendments. The official method uses 15 g of silicic acid and elutes several fractions by using huge volumes of dangerous solvent (n-hexane). The developed method uses 1 g of silicic acid with a different particle size and less than 20 mL of solvent mixture, substituting n-hexane with less toxic isooctane. Briefly, after spiking with a suitable internal standard, oil sample is fractionated by SPE (Solid Phase Extraction) cartridge with 1 g of silica, waxes are eluted with 14 mL of isooctane/ethyl ether 99/1 (6 mL discarded and 8 mL collected), then, after elution sample is reconstitute in 200 μL of n-heptane and analysed by capillary GC. Data of “In home” validation, (repeatability, accuracy and recovery) and relative chromatograms are reported in this paper.

Analysis and Evaluation of 7 Indictor Polychlorinated Biphenyls (PCBs) Residues in Dried Kelp by Gas Chromatography (GC)

In this study, a special method was developed for the determination of 7 kinds of polychlorinated biphenyls (PCBs) residues in dried kelp by gas chromatography (GC) with electron capture detector (ECD). The PCBs were extracted with hexane/dichloromethane (1/1, v/v) by ultrasonic extraction. Clean-up methods were used by concentrated sulphuric acid, neutral alumina oxide solid phase extraction cartridge and silica solid phase extraction cartridge. The analytical compounds were quantified by an internal standard method. Under optimal experimental conditions, good linearity was observed in the range of 5~200ng/mL, and the correlation coefficients were 0.9993~0.9998. The limit of quantification (LOQ) for target analytical compounds ranged from 6.0 to 7.5μg/kg. At the spiked levels of 10，20，50 μg/kg，the average recoveries ranged from 81.8% to 105% with the relative standard deviations 3.05%～11.2%. The result showed that the proposed method was accurate and could be used for the determination of the PCBs in dried kelp.

Co-Extraction and Co-Purification Coupled with HPLC-DAD for Simultaneous Detection of Acrylamide and 5-hydroxymethyl-2-furfural in Thermally Processed Foods

Acrylamide and 5-hydroxymethyl-2-furfural (5-HMF) are two of the most abundant compounds generated during thermal processing. A simple method for the simultaneous quantitation of acrylamide and 5-HMF was developed and successfully applied in thermally processed foods. Acrylamide and 5-HMF were co-extracted with methanol and then purified and enriched by an Oasis HLB solid-phase extraction cartridge, simultaneously analyzed by high-performance liquid chromatography and detected with a diode array detector, respectively, at their optimal wavelength. The linear concentration range was found to be 25–5000 μg/L with high linear correlation coefficients (R > 0.999). The limit of detection and the limit of quantitation for acrylamide and 5-HMF were 6.90 μg/L and 4.66 μg/L, and 20.90 μg/L and 14.12 μg/L, respectively. The recovery of acrylamide and 5-HMF in biscuits, bread, Chinese doughnuts, breakfast cereals, and milk-based baby foods was achieved at 87.72–96.70% and 85.68–96.17% with RSD at 0.78–3.35% and 0.55–2.81%, respectively. The established method presents simplicity, accuracy and good repeatability, and can be used for the rapid simultaneous quantitation of acrylamide and 5-HMF in thermally processed foods.