Development, Optimization, and Validation of Methods for Quantification of Veterinary Drug Residues in Complex Food Matrices Using Liquid-Chromatography—A Review

Manimekalai, M.; Rawson, Ashish; Sengar, Animesh Singh; Kumar, K. Suresh

doi:10.1007/s12161-019-01512-9

Cited by 18 publications

(16 citation statements)

References 102 publications

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“…It should be pointed out that targeted methods are often related to laborious extraction steps, which does not fully match a high throughput routine analysis. As for screening strategies, usually related to simpler sample extraction procedures, similar sensitivity and detection windows than quantification/confirmatory approaches should be delivered in order to prevent false negative results 25 . In this work, liquid–liquid extraction was selected to be evaluated for sample extraction using acetonitrile due to its known ability of extracting both polar and non‐polar compounds 25–27 .…”

Section: Resultsmentioning

confidence: 99%

“…As for screening strategies, usually related to simpler sample extraction procedures, similar sensitivity and detection windows than quantification/confirmatory approaches should be delivered in order to prevent false negative results. 25 In this work, liquid-liquid extraction was selected to be evaluated for sample extraction using acetonitrile due to its known ability of extracting both polar and non-polar compounds. [25][26][27] The addition of NaCl was required to obtain a clear separation between the organic and the aqueous phases.…”

Section: Sample Extractionmentioning

confidence: 99%

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A novel strategy for the detection of boldenone undecylenate misuse in cattle using ultra‐high performance liquid chromatography coupled to high resolution orbitrap mass spectrometry: From non‐targeted to targeted

Rocha

Lana

Assis

et al. 2021

Drug Testing and Analysis

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In this work multivariate strategies were employed in order to highlight new potential biomarkers of interest to detect the exogenous treatment of steers intramuscularly treated with boldenone undecylenate. Serum samples collected from treated (n = 4) and control (n = 8) crossbred animals of varying ages and weights were extracted using a simple sample preparation procedure based on salt assisted liquid-liquid extraction. Data acquisition was performed using liquid chromatography and Q-Exactive™ Orbitrap mass spectrometry. Data processing and treatment were performed using two non-targeted workflows: (1) Compound Discoverer software and (2) XCMS package on the open-source R software combined with MetaboAnalyst. Three potential biomarkers were highlighted taking into account the chromatographic shapes, the feature location on the generated s-plots, the fold change, the adjusted p values, the coefficient of variation in the QC samples and the area under the ROC curves. Predicted formulas based on mass accuracy, structural composition and spectra similarity were proposed. A robust statistical model to predict the boldenone treatment was further developed based on the weighted abundances of the selected biomarkers. The requirements for screening methods were successfully fulfilled, together with a wider detection window in comparison with the monitoring of the deconjugated metabolite boldenone, although biomarker identification studies are still ongoing.

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Section: Resultsmentioning

confidence: 99%

Section: Sample Extractionmentioning

confidence: 99%

A novel strategy for the detection of boldenone undecylenate misuse in cattle using ultra‐high performance liquid chromatography coupled to high resolution orbitrap mass spectrometry: From non‐targeted to targeted

Rocha

Lana

Assis

et al. 2021

Drug Testing and Analysis

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show abstract

“…Good linearity was obtained for all ATB and highly correlated with the amounts injected, the correlation coefficients (r 2 ) ranged from 0.997 to 0.999. The food matrix imposes a lot of interferences and the ability of the method to quantify a particular analyte despite all interferences is measured by the selectivity [36]. The application of the method to different blank milk samples demonstrated that no potential interferences from the matrix were detected at the retention time-windows of three analytes.…”

Section: Validation Of Methodsmentioning

confidence: 99%

HPLC-DAD multi-residue method for determination of florfenicol, penicillin and tetracycline residues in raw cow milk

Jaber¹,

Zahreddine²,

Haidar³

et al. 2021

JCLR

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The existence of antibiotic residues in edible products constitutes a health problem to the consumers. Reversed-phase high-performance liquid chromatography with diode array detection (HPLC–DAD) was optimized and validated for the simultaneous determination of florfenicol (FF), penicillin (PE), and tetracycline (TC) residues in dairy raw milk samples. The determination of these antibiotics was carried out on HP-ODS Hypersil C18 (5μm, 125*4 mm) column at a flow rate (1mL/min) and temperature (35 ⁰C). The extraction method includes deproteinization of the milk sample followed by a solid-phase extraction (SPE) clean-up. The method was validated according to the European Commission Decision 2002/657/EC and the International Conference of Harmonization Guidelines. The recoveries for the studied antibiotics ranged from 82–111.54 % making the method suitable for performing routine analysis. The proposed method was applied for the analysis of antibiotic residues in 50 dairy raw milk samples collected from many regions in Lebanon. The results showed the occurrence of these antibiotics residues in milk collected from different Lebanese regions. The numbers indicate that 22 % of milk samples were found to be positive for FF, 42 % for PE, and 28 % for TC residues.

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“…In contrast, the residual content of veterinary drugs is very small and the polarity difference is large, [8,10] making it difficult for detection since the matrix effects can easily interfere with the result. [17] Conventional detection methods can only carry out quantitative detection of known objects, while they are poor in qualitative determination and deficient in screening suspect products. In order to solve these problems, mass spectrometric database is widely used for qualitative confirmation of suspect objects.…”

Section: Introductionmentioning

confidence: 99%

Optimization of 204 veterinary drug residues method and establishing their mass spectrum library

Fang

et al. 2021

International Journal of Food Properties

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A multi-class multi-residue analytical method was validated in this paper for simultaneously identifying 204 veterinary drugs in pork by UPLC-QTRAP MS/MS, including sulfonamides, quinolones, β-agonists, and nitroimidazoles. MRM-IDA-EPI mode of QTRAP was used to establish a secondary mass spectrum library of these 204 veterinary drugs, which could enhance the qualitative analysis of suspect substances. The separation of substances was performed on a C18 column, with a gradient elution of 0.1% formic acid solution in water and methanol. Electrospray ionization (ESI), fast polarity switching, and scheduled MRM mode were used to collect the characterization results. Factors that affected the recovery were delicately optimized, such as solvent proportion, formic acid content, and purification method. We finally determined the extracting method with formic acidacetonitrile-water (0.1:90:10, v:v:v) and purifying method with Cleanert LipoNo as a package for dispersive solid-phase extraction. Matrix effects on the quantitative results were also investigated. Some compounds had strong matrix inhibition or enhancement, and the matrix matching external standard method was used to quantify the compounds accurately. The correlation coefficient R 2 was over 0.99 within the calibration linearity range for the detected 204 veterinary drugs. The limit of quantification (LOQ) was 0.5 ~ 5 μg/kg. The recoveries ranged from 61.4% to 118.8% with RSDs of 3.1% to 19.2% (n = 6).

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Development, Optimization, and Validation of Methods for Quantification of Veterinary Drug Residues in Complex Food Matrices Using Liquid-Chromatography—A Review

Cited by 18 publications

References 102 publications

A novel strategy for the detection of boldenone undecylenate misuse in cattle using ultra‐high performance liquid chromatography coupled to high resolution orbitrap mass spectrometry: From non‐targeted to targeted

A novel strategy for the detection of boldenone undecylenate misuse in cattle using ultra‐high performance liquid chromatography coupled to high resolution orbitrap mass spectrometry: From non‐targeted to targeted

HPLC-DAD multi-residue method for determination of florfenicol, penicillin and tetracycline residues in raw cow milk

Optimization of 204 veterinary drug residues method and establishing their mass spectrum library

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