Detection of selected corticosteroids and anabolic steroids in calf milk replacers by liquid chromatography–electrospray ionisation – Tandem mass spectrometry

Chiesa, Luca Maria; Nobile, Maria; Biolatti, B.; Pavlović, Radmila; Panseri, Sara; Cannizzo, Francesca Tiziana; Arioli, Francesco

doi:10.1016/j.foodcont.2015.09.028

Cited by 17 publications

(11 citation statements)

References 20 publications

(14 reference statements)

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“…The CE was adjusted in the MRM mode for each transition monitored in order to reach the highest sensitivity and specificity for the two isomers. The Synergi Hydro RP column was our first choice as we used it successfully for anabolic hormone determination, [23,24,26] Also here, in the case of nandrolone, it showed good performances and satisfactory peak shapes and baseline separation. The m/z values of the selected precursor and fragment ions used for MS detection are generally in agreement with those previously reported in the literature, especially when it concerns quantifier ions for αand β-nandrolone (transition 275 → 109) and d3-β-nandrolone (transition 278 → 109).…”

Section: Methods Validationmentioning

confidence: 90%

“…Therefore, the gradient elution programme of 0.1% formic acid in water and methanol with suitable flow rate was carefully optimized until it permitted the complete separation of the two isomers. The Synergi Hydro RP column was our first choice as we used it successfully for anabolic hormone determination, [23,24,26] Also here, in the case of nandrolone, it showed good performances and satisfactory peak shapes and baseline separation. The MRM chromatogram of a sample spiked with 5 ng/mL αand β-nandrolone is presented in Figure 2.…”

Section: Methods Validationmentioning

confidence: 90%

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Evaluation of nandrolone and ractopamine in the urine of veal calves: liquid chromatography‐tandem mass spectrometry approach

Chiesa

Panseri

Cannizzo

et al. 2016

Drug Testing and Analysis

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Research articles LC-MS/MS technology allows the direct detection of glucuronoconjugated metabolites. PI scan, NL scan and SRM methods, have demonstrated to be useful for the detection of unknown unpredicted and predicted glucuronide MTD metabolites in metabolic studies. Thirteen glucuronide metabolites were observed, and one of them was resistant to enzymatic hydrolysis, not detectable using the traditional GC-MS strategies. Sport supplements may contain steroids never approved for therapeutic use. In this study, 18 sport supplements purchased online underwent organic solvent extraction and subsequent isolated steroid tested for intrinsic androgen bioactivity. Many were found to be strong androgens. These potent pharmacologically active steroids are being used without regulatory control or consumer awareness of their potential adverse effect. Avidin-biotin technology was used for the implementation of an enzyme-linked immunosorbent assay (AB-ELISA) as a sensitive method for the detection of anabolic androgenic steroids (AAS) present in dietary supplements. Assembled AB-ELISAs were characterized and used for detection of various AAS in 49 samples of counterfeit dietary supplements. The concordance between UHPLC-MS and the CR corrected data from AB-ELISA indicated the potential of this method even to quantification of some steroids. Nandrolone (anabolic steroid) and ractopamine (β-adrenergic agonist) are used quite frequently in food-producing livestock, but little is known about their synergic action when they are administered together. The objective of this study was to determine levels after experimental treatment of bovines with both of the above-mentioned drugs. For this purpose two specific analytical methods based on liquid chromatography-tandem mass spectrometry were developed. The use of tandem yeast and mamma-lian cell in vitro androgen bioassays to detect androgens in internet-sourced sport supplements 545-552 We evaluated the effectiveness of drugs testing using hair and nails and the feasibility of determining when drugs were ingested by measuring the time courses of drug concentrations in hair and toenails after single administrations of various drugs. For most basic compounds, the maximum concentrations in hair segments tended to be higher than those in nails. Nails were an effective specimen to detect neutral and weakly acidic compounds. In this work, we aimed to develop a new, simple and confident sensory platform for cocaine detection. For the fabrication of this test system, surface of μ-well plates was modified with quantum dots (QDs) and then cocaine-binding aptamer modified gold nanoparticles (Apt-AuNP) were covalently attached to the QDs. Detectable signals were obtained owing to the target-induced conformational change of aptamer which gives rise to close interaction of QDs with their quencher, AuNPs. Hence, decrease in fluorescence intensity as a cocaine response was recorded. The developed test system-called as Aptamer Folding based Sensory Device, (AFSD)-was evaluated in terms of main a...

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Section: Methods Validationmentioning

confidence: 90%

Section: Methods Validationmentioning

confidence: 90%

Evaluation of nandrolone and ractopamine in the urine of veal calves: liquid chromatography‐tandem mass spectrometry approach

Chiesa

Panseri

Cannizzo

et al. 2016

Drug Testing and Analysis

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“…The efficient removal of lipids from the extract prior to instrumental analysis is crucial to limit interference and increase sensitivity and reproducibility of the analytical method (Table 6). Simple and common defatting procedures reported in the literature are LLE with hexane [184,185] and freezing lipid precipitation (LFP) [186].…”

Section: Removal Of Lipidsmentioning

confidence: 99%

“…Porcine muscle-milk LLE with hexane [184,185] High lipid foodstuff Freezing lipid precipitation (LFP) Effective sample clean-up [186] Milk Lipid precipitation by zinc and tungsten salt solutions in acidic media…”

Section: Technique Effectiveness Referencesmentioning

confidence: 99%

Compensate for or Minimize Matrix Effects? Strategies for Overcoming Matrix Effects in Liquid Chromatography-Mass Spectrometry Technique: A Tutorial Review

et al. 2020

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In recent decades, mass spectrometry techniques, particularly when combined with separation methods such as high-performance liquid chromatography, have become increasingly important in pharmaceutical, bio-analytical, environmental, and food science applications because they afford high selectivity and sensitivity. However, mass spectrometry has limitations due to the matrix effects (ME), which can be particularly marked in complex mixes, when the analyte co-elutes together with other molecules, altering analysis results quantitatively. This may be detrimental during method validation, negatively affecting reproducibility, linearity, selectivity, accuracy, and sensitivity. Starting from literature and own experience, this review intends to provide a simple guideline for selecting the best operative conditions to overcome matrix effects in LC-MS techniques, to obtain the best result in the shortest time. The proposed methodology can be of benefit in different sectors, such as pharmaceutical, bio-analytical, environmental, and food sciences. Depending on the required sensitivity, analysts may minimize or compensate for ME. When sensitivity is crucial, analysis must try to minimize ME by adjusting MS parameters, chromatographic conditions, or optimizing clean-up. On the contrary, to compensate for ME analysts should have recourse to calibration approaches depending on the availability of blank matrix. When blank matrices are available, calibration can occur through isotope labeled internal standards and matrix matched calibration standards; conversely, when blank matrices are not available, calibration can be performed through isotope labeled internal standards, background subtraction, or surrogate matrices. In any case, an adjusting of MS parameters, chromatographic conditions, or a clean-up are necessary.

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“…En los equipos de HPLC, la alta presión es compatible con el sistema cromatográfico. Además, la sofisticación del equipo y las nuevas fases estacionarias aumentan la efectividad de las separaciones, lo que reduce el tiempo de análisis y aumenta la versatilidad y la automatización (Chiesa et al, 2016;Li et al, 2015;Nezhadali et al, 2016).…”

Section: Introductionunclassified

Intervención didáctica para la extracción y cuantificación de esteroides en orina

et al. 2021

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Este artículo describe una estrategia didáctica para la enseñanza de un método de extracción en fase sólida miniaturizada en contextos del trabajo práctico de laboratorio [TPL]. Se parte de los imaginarios previos de los estudiantes para, a partir de algunas sesiones de laboratorio, generar cambios conceptuales y promover un aprendizaje significativo. En este trabajo se relatará la experiencia de conjugar el empleo de una técnica de preparación de muestras —PT-SPE— con un ejercicio de intervención didáctica para el desarrollo de habilidades procedimentales. Se presentan los resultados de la aplicación de TPL en la multideterminación de tres esteroides en muestras de orina al emplear HPLC-DAD-PT-C18-SPE, que presentan adecuados porcentajes de recuperación y parámetros de validación. Los resultados de la intervención muestran una mejoría en habilidades relacionadas con métodos de extracción en fase sólida. Se concluye que hubo cambios conceptuales frente a procesos analíticos, una adecuada familiarización con nuevas metodologías de preparación de muestras, aumento significativo del lenguaje químico y la comprensión de conceptos, junto con la aplicación de procesos cognitivos de bajo orden, para la promoción de habilidades cognitivas de alto orden.

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Detection of selected corticosteroids and anabolic steroids in calf milk replacers by liquid chromatography–electrospray ionisation – Tandem mass spectrometry

Cited by 17 publications

References 20 publications

Evaluation of nandrolone and ractopamine in the urine of veal calves: liquid chromatography‐tandem mass spectrometry approach

Evaluation of nandrolone and ractopamine in the urine of veal calves: liquid chromatography‐tandem mass spectrometry approach

Compensate for or Minimize Matrix Effects? Strategies for Overcoming Matrix Effects in Liquid Chromatography-Mass Spectrometry Technique: A Tutorial Review

Intervención didáctica para la extracción y cuantificación de esteroides en orina

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