Development of a High Pressure Liquid Chromatography with Diode Array Detection Method for the Determination of Four Tetracycline Residues in Milk by Using QuEChERS Dispersive Extraction

Abstract

QuEChERS (quick, easy, cheap, effective, rugged and safe) dispersive extraction was applied for the extraction of tetracyclines (oxytetracycline, tetracycline, chlorotetracycline and doxycycline) from milk. Target analytes were determined by an accurate and sensitive chromatographic analytical method, which was validated in terms of 2002/6572/EC decision. The analytes were separated on an Orbit 100C 4 (5 µm, 250 × 4.0 mm) analytical column under a gradient mobile phase composed of a mixture of 0.01 M oxalic acid, 10 −4 M Na 2 EDTA and acetonitrile. For the extraction of isolated compounds from sorbent, a methanol and 0.01 M oxalic acid mixture (1:1 v/v) was used, leading to relative recovery rates from 83.07% to 106.3% at concentration levels in the range 100-200 µg/kg. The within-laboratory reproducibility, expressed as a relative standard deviation, was <15.5%. Decision limits ranged between 100.3 µg/kg and 105.6 µg/kg and the detection capability varied between 100.6 µg/kg and 109.7 µg/kg. Ruggedness was evaluated by following the Youden approach, in terms of milk mass, sorbent mass, centrifugation time, vortex time, type and volume of organic solvents and evaporation temperature.Separations 2019, 6, 21 2 of 9 solid-phase extraction (D-SPE) clean-up step. This process was firstly developed for the extraction of pesticides from different matrices, such as soil [10], sugarcane juice [11], honey [12], wheat grains, flour and bran [13], but also for the extraction of drugs and phenols from soil [14-16] and veterinary drug residues from foods of animal origin [17][18][19].Although a number of methods [20,21] can be found in the literature employing mass spectrometric detection for confirmation purposes, this instrumentation is not always available in analytical laboratories. The aim of this study was to develop a simple and quick HPLC-DAD method for the determination of four tetracyclines (oxytetracycline, tetracycline, chlorotetracycline and doxycycline) in milk using QuEChERS dispersive extraction. The method was validated according to the European Union Decision 2002/657/EC with regards to selectivity, linearity, accuracy, precision, sensitivity and ruggedness by applying the Youden approach [22].

FTIR spectroscopy with chemometrics for determination of tylosin residues in milk

“…The screening tests are nonspecific, while the chromatographs are specific and quantify the substance; however, they are laborious, use many chemical reagents, require trained personnel and their analytical speed is low 2,36 . Even with studies to increase their analytical efficiency, 37–39 chromatographic techniques continue to use noxious reagents, requiring time and trained personnel. For the offer of safe food, it is essential that the number of samples evaluated increases, which implies the search for other techniques and methodologies.…”

Assessment of various veterinary drug residues in animal originated food products

“…LOD were 48, 44, and 8mg/kg, for Oxy-tet + , Tet + , and Chlor-tet + , respectively, and average recovery found between 71 and 110%. Marinou et al [ 17 ] developed and validated an HPLC as per European Union Decision 2002/657/EC with DAD using a simple sample extraction procedure with acetonitrile as an extraction solvent and for clean-up C18 and PSA are used in Tet + , Oxy-tet + , and Chlor-tet + in milk sample. The method was linearity, ruggedness, selectivity, precision and accuracy, and sensitivity.…”

One Pot Synthesis of Nanofiber-Coated Magnetic Composites as Magnetic Dispersive Solid-Phase Extraction Adsorbents for Rapid Determination of Tetracyclines in Aquatic Food Products

“…Toxicology studies of TCs indicate that these antibiotics show quite serious side effects, such as abdominal discomfort, epigastric pain, nausea, vomiting and anorexia, discoloration of teeth, and inhibition of bone growth in children. Furthermore, when entering the environment, TCs may lead to the induction and spread of drug-resistant bacteria, which poses a long-term potential threat to human health and the ecological environment [4][5][6][7][8]. Consequently, it is necessary to develop a fast, sensitive, and reliable method to detect and quantify TC residues in food samples.…”