Validation of HPLC Multi-residue Method for Determination of Fluoroquinolones, Tetracycline, Sulphonamides and Chloramphenicol Residues in Bovine Milk

Moudgil, Pallavi; Bedi, Jasbir Singh; Aulakh, Rabinder Singh; Gill, Jatinder Paul Singh; Kumar, Amit

doi:10.1007/s12161-018-1365-0

Cited by 165 publications

(57 citation statements)

References 27 publications

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“…The performance characteristics of the method are comparable with those obtained by other methods, including those in which dispersive solid-phase microextraction [6] and ultrasound-assisted dispersive extraction [8] were applied for the determination of tetracycline residues in milk samples.…”

Section: Discussionsupporting

confidence: 58%

“…Many sample preparation strategies have been developed for the isolation and clean-up of tetracycline residues in milk throughout the years, such as solid phase extraction (SPE) with various types of sorbents [4,5], solid phase microextraction (SPME) [6], hollow-fiber liquid phase microextraction (HF-LPME) [7] and ultrasound assisted dispersive extraction [8].…”

Section: Introductionmentioning

confidence: 99%

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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

2019

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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].

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Section: Discussionsupporting

confidence: 58%

Section: Introductionmentioning

confidence: 99%

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

2019

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“…HPLC is the most commonly used method in the detection of antibiotic residues because of high separation and satisfactory quantitation performance [4–6]. Owing to the complexity of the food matrix composition and relatively low concentration of TCs residues, an effective matrix separation, purification, and preconcentration procedure are usually required prior to detection [7], such as SPE [8, 9], LLE [10, 11], and matrix solid‐phase dispersion (MSPD) [2, 12].…”

Section: Introductionmentioning

confidence: 99%

Preparation of hydrophilic molecularly imprinted solid‐phase microextraction fiber for the selective removal and extraction of trace tetracyclines residues in animal derived foods

Lü

et al. 2020

J of Separation Science

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The present work reported a novel hydrophilic and selective solid-phase microextraction fiber by improved multiple co-polymerization method immobilization of tetracycline molecularly imprinted polymer on a stainless steel wire and directly coupled with high-performance liquid chromatography for sensitive determination of trace tetracyclines residues in animal derived foods. The developed molecularly imprinted polymer coated solid-phase microextraction fibers were characterized through scanning electron microscopy, Fourier transfer infrared spectroscopy, thermogravimetric analysis, and adsorption experiments, the fiber with cross-linked and porous structure was observed and high thermal and chemical stability. The maximum adsorption capacity of this fiber with good selectivity reached 2.35 µg/mg in aqueous matrices, and showed good repeatability (relative standard deviation ≤ 6.6%, n = 5) and satisfying reproducibility between fiber to fiber (relative standard deviation ≤ 7.8%, n = 5). Under the optimized solid-phase microextraction conditions, satisfactory linearity (5-1000 µg/L) and detection limits (0.38-0.72 µg/kg, S/N = 3) for all the tetracyclines were obtained. The practicality of this method was proved by adding tetracycline, oxytetracycline at three levels to milk, chicken, and fish samples with good recoveries of 77.3-104.4%. K E Y W O R D Shigh-performance liquid chromatography, hydrophilic molecularly imprinted polymers, solid-phase microextraction, tetracyclines 2172

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“…Many articles have reported on the determination and catalytic degradation of OTC, with the aid of modern instrumental analysis methods and on design of novel materials. Various detection methods, including spectrophotometry, fluorescence microscopy, high‐pressure liquid chromatography (HPLC) with UV or fluorescence or MS detection, sensor or aptasensor, optical methods, fluorescent probes, capillary electrophoresis systems coupled with electrochemiluminescence (CE‐ECL), and so on, have been reported for determination of OTC in environmental, food or biological samples . Although these methods can basically meet the requirements for detection, they are time‐consuming, use expensive equipment, have tedious sample pretreatment, among other shortcomings .…”

Section: Introductionmentioning

confidence: 99%

“…Various detection methods, including spectrophotometry, [14,15] fluorescence microscopy, [16] high-pressure liquid chromatography (HPLC) with UV or fluorescence or MS detection, [17][18][19][20] sensor or aptasensor, [21,22] optical methods, [23] fluorescent probes, [24] capillary electrophoresis systems coupled with electrochemiluminescence (CE-ECL), [25] and so on, have been reported for determination of OTC in environmental, food or biological samples. [26][27][28][29] Although these methods can basically meet the requirements for detection, they are time-consuming, use expensive equipment, have tedious sample pretreatment, among other shortcomings. [30] Therefore, it is very important to establish a rapid, simple detection method for OTC determination to protect people's health.…”

Section: Introductionmentioning

confidence: 99%

Determination of oxytetracycline hydrochloride in milk and egg white samples using Ru(bipy)₃²⁺–Ce(SO₄)₂ chemiluminescence

et al. 2019

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A novel, rapid and sensitive chemiluminescence (CL) method for the determination of oxytetracycline hydrochloride (OTCH) is described in this paper. The presented method was based on the fact that OTCH could immensely enhance the CL of the reaction of cerium sulfate and tris(2,2‐bipyridyl) ruthenium (II) in acidic medium. Under optimal experimental conditions, CL intensity was favorably linear for OTCH in the range 5.0 × 10−7 to 5.0 × 10−5 g/ml, with a detection limit of 1.5 × 10−7 g/ml (S/N = 3). The relative standard detection was 4.76% for 5.0 × 10−6 g/ml (n = 11). This method was successfully applied to the analysis of OTCH in milk and egg white samples. According to the results of the kinetic curves for OTCH in the Ru(bipy)32+–Ce(SO4)2 CL system, together with CL and ultraviolet (UV)–visible spectra, the possible mechanism of the CL reaction is discussed briefly.

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Validation of HPLC Multi-residue Method for Determination of Fluoroquinolones, Tetracycline, Sulphonamides and Chloramphenicol Residues in Bovine Milk

Cited by 165 publications

References 27 publications

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

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

Preparation of hydrophilic molecularly imprinted solid‐phase microextraction fiber for the selective removal and extraction of trace tetracyclines residues in animal derived foods

Determination of oxytetracycline hydrochloride in milk and egg white samples using Ru(bipy)₃²⁺–Ce(SO₄)₂ chemiluminescence

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Validation of HPLC Multi-residue Method for Determination of Fluoroquinolones, Tetracycline, Sulphonamides and Chloramphenicol Residues in Bovine Milk

Cited by 165 publications

References 27 publications

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

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

Preparation of hydrophilic molecularly imprinted solid‐phase microextraction fiber for the selective removal and extraction of trace tetracyclines residues in animal derived foods

Determination of oxytetracycline hydrochloride in milk and egg white samples using Ru(bipy)32+–Ce(SO4)2 chemiluminescence

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Determination of oxytetracycline hydrochloride in milk and egg white samples using Ru(bipy)₃²⁺–Ce(SO₄)₂ chemiluminescence