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A widely applicable original gas chromatography-tandem mass spectrometry (GC-MS/MS) method was explored to qualitatively and quantitatively measure enrofloxacin and ofloxacin residues in chicken tissues and pork. The experimental samples were processed based on liquid-liquid extraction (LLE) and solid-phase extraction (SPE). Trimethylsilyl diazomethane (TMSD) was chosen to react derivatively with enrofloxacin and ofloxacin. In total, 78.25% ∼ 90.56% enrofloxacin and 78.43% ∼ 91.86% ofloxacin was recovered from the blank fortified samples. The limits of detection (LODs) were 0.7-1.0 μg/kg and 0.1-0.2 μg/kg, respectively. The limits of quantitation (LOQs) were 1.6-1.9 μg/kg and 0.3-0.4 μg/kg, respectively. It was verified that various experimental data met the requirements of the FAO & WHO (2014) for the detection of veterinary drug residues. Real samples obtained from local markets were analysed using the established method, and no residues of enrofloxacin or ofloxacin were detected in the samples., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

A novel precolumn derivatization-GC-MS/MS method was developed for the determination of decoquinate residues in chicken tissues (muscle, liver, and kidney). The samples were extracted and purified by liquid-liquid extraction combined with solid-phase extraction and derivatized with acetic anhydride and pyridine. The recovery rates for decoquinate were 77.38~89.65%, and the intra-day and inter-day RSDs were 1.63~5.74% and 2.27~8.06%, respectively. The technique parameters meet the necessities for veterinary drug residue detection in China, the US, and the EU. Finally, the method was applied to analyze tissues of 60 chickens bought from a neighborhood supermarket, and solely one sample of chicken muscle contained 15.6 μg/kg decoquinate residue.

A novel GC-MS/MS analytical method was established for the qualitative and quantitative determination of tilmicosin in poultry (Jinghai yellow chicken, Gaoyou duck and Yangzhou goose) eggs. The method was based on LLE and SPE for sample extraction and purification. Pyridine and acetic anhydride were used for the derivatization reaction. When tilmicosin was added to blank poultry egg samples at the LOQ and 75 μg/kg, 150 μg/kg, and 300 μg/kg, the recoveries ranged from 72.80% to 88.75%, the intraday and interday RSDs ranged from 2.31% to 4.56% and 3.29%-5.61%, respectively, and the LODs and LOQs ranged from 3.8 to 5.6 μg/kg and 8.4-10.5 μg/kg, respectively. These results confirmed that the parameters of this novel method meet the requirements of the FAO & WHO (2014) for veterinary drug residue testing. Poultry egg samples purchased from the local market were analysed according to the established method and only one egg sample was found to contain 18.9 μg/kg of tilmicosin., (Copyright © 2022 Elsevier Ltd. All rights reserved.)

A widely applicable method involving liquid chromatography-electrospray ionization tandem triple quadrupole mass spectrometry (LC-ESI/MS/MS) was developed for the simultaneous determination of chloramphenicol, thiamphenicol, florfenicol, and florfenicol amine in eggs. Samples were extracted with ethyl acetate-acetonitrile-ammonium hydroxide (49:49:2, v/v) and defatted with hexane saturated with acetonitrile. The analysis was carried out on a mass spectrometer via an electrospray interface operated in the positive and negative ionization modes using deuterated chloramphenicol-d5 as the internal standard. The limits of detection and limits of quantification were 0.04-0.5 μg/kg and 0.1-1.5 μg/kg in eggs, respectively. The average recoveries of the four analytes from egg samples were 90.84-108.23%, with relative standard deviations of less than 9.61%. The corresponding intra-day and inter-day variations were found to be less than 8.11% and 11.30%, respectively. Finally, the new approach was successfully applied to the quantitative determination of these analytes in 50 commercial eggs from local supermarkets., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

An accelerated solvent extraction coupled with gas chromatography-tandem mass spectrometry (ASE-GC-MS/MS) method for detecting dinitolmide residue and its metabolite (3-amino-2-methyl-5-nitrobenzamide, 3-ANOT) in eggs was developed and optimized. The samples were extracted using ASE with acetonitrile as the extractant and were purified by passage through a neutral alumina solid-phase extraction column. Then, the samples were analyzed using the GC-MS/MS method. The optimized method parameters were validated according to the requirements set forth by the European Union and the Food and Drug Administration. The average recoveries of dinitolmide and 3-ANOT from eggs (egg white, egg yolk, and whole egg) at the limit of quantification (LOQ), 0.5 maximum residue limit (MRL), 1 MRL, and 2 MRL were 82.74% to 87.49%, the relative standard deviations (RSDs) were less than 4.63%, and the intra-day RSDs and the inter-day RSDs were 2.96% to 5.21% and 3.94% to 6.34%, respectively. The limits of detection and the LOQ were 0.8 to 2.8 μg/kg and 3.0 to 10.0 μg/kg, respectively. The decision limits (CC α ) were 3001.69 to 3006.48 μg/kg, and the detection capabilities (CC β ) were 3001.74 to 3005.22 μg/kg. Finally, the new method was successfully applied to the quantitative determination of dinitolmide and 3-ANOT in 50 commercial eggs from local supermarkets., (© 2018 John Wiley & Sons, Ltd.)

In this present study, we developed a simple, rapid and specific method for the quantitative analysis of the contents of amoxicillin (AMO), AMO metabolites and ampicillin (AMP) in eggs. This method uses a simple liquid-liquid extraction with acetonitrile followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The optimized method has been validated according to requirements defined by the European Union and Food and Drug Administration. Extraction recoveries of the target compounds from the egg at 5, 10 and 25 μg/kg were all higher than 80%, with relative standard deviations not exceeding 10.00%. The limits of quantification in eggs were below the maximum residue limits (MRLs). The decision limits (CCα) ranged between 11.1 and 11.5 μg/kg, while detection capabilities (CCβ) from 12.1 to 13.0 μg/kg. These values were very close to the corresponding MRLs. Finally, the new approach was successfully verified for the quantitative determination of these analytes in 40 commercial eggs from local supermarkets., (Copyright © 2015 Elsevier Ltd. All rights reserved.)

A method based on accelerated solvent extraction (ASE) coupled with gas chromatography tandem mass spectrometry (GC-MS/MS) was developed for the quantitative analysis of spectinomycin and lincomycin in poultry egg (whole egg, albumen and yolk) samples. In this work, the samples were extracted and purified using an ASE350 instrument and solid-phase extraction (SPE) cartridges, and the parameters of the ASE method were experimentally optimized. The appropriate SPE cartridges were selected, and the conditions for the derivatization reaction were optimized. After derivatization, the poultry egg (whole egg, albumen and yolk) samples were analyzed by GC-MS/MS. This study used blank poultry egg (whole egg, albumen and yolk) samples to evaluate the specificity, sensitivity, linearity, recovery and precision of the method. The linearity (5.6–2000 μg/kg for spectinomycin and 5.9–200 μg/kg for lincomycin), correlation coefficient (≥0.9991), recovery (80.0%–95.7%), precision (relative standard deviations, 1.0%–3.4%), limit of detection (2.3–4.3 μg/kg) and limit of quantification (5.6–9.5 μg/kg) of the method met the requirements for EU parameter verification. Compared with traditional liquid–liquid extraction methods, the proposed method is fast and consumes less reagents, and 24 samples can be processed at a time. Finally, the feasibility of the method was evaluated by testing real samples, and spectinomycin and lincomycin residues in poultry eggs were successfully detected. [ABSTRACT FROM AUTHOR]

A method for the simultaneous determination of robenidine, halofuginone, lasalocid, monensin, nigericin, salinomycin, narasin, and maduramicin residues in eggs by liquid chromatography–tandem mass spectrometry (LC–MS/MS) was developed. The sample preparation method used a combination of liquid–liquid extraction (LLE) and solid-phase extraction (SPE) technology to extract and purify these target compounds from eggs. The target compounds were separated by gradient elution using high-performance liquid chromatography (HPLC) and ultra-performance liquid chromatography (UPLC). Tandem mass spectrometry was used to quantitatively and qualitatively analyze the target compounds via electrospray ionization (ESI+) and multiple reaction monitoring mode. The HPLC–MS/MS and UPLC–MS/MS methods were validated according to the requirements defined by the European Union and the Food and Drug Administration. The limits of detection and limits of quantification of the eight coccidiostats in eggs were 0.23–0.52 µg/kg and 0.82–1.73 µg/kg for HPLC–MS/MS, and 0.16-0.42 µg/kg and 0.81-1.25 µg/kg for UPLC–MS/MS, respectively. The eggs were spiked with four concentrations of the eight coccidiostats, and the HPLC–MS/MS and UPLC–MS/MS average recoveries were all higher than 71.69% and 72.26%, respectively. Compared with the HPLC–MS/MS method, utilizing UPLC–MS/MS had the advantages of low reagent consumption, a short detection time, and high recovery and precision. Finally, the HPLC–MS/MS and UPLC–MS/MS methods were successfully applied to detect eight coccidiostats in 40 eggs. [ABSTRACT FROM AUTHOR]

A novel confirmatory analysis method to simultaneously extract, clean-up and detect dinitolmide and its metabolite (3-amino-2-methyl-5-nitrobenzamide, 3-ANOT) in chicken tissues using accelerated solvent extraction (ASE) with a neutral alumina solid-phase extraction (SPE) column coupled with gas chromatography-tandem mass spectrometry (ASE-SPE-GC–MS/MS) was established. GC–MS/MS was performed using a VF-5ht capillary column with helium as the carrier gas, temperature programming, and an inlet temperature of 340 °C. The experimental method was carried out in the electron ionization mode; the full scan mode was used for qualitative analysis, and selective reaction monitoring, combined with an external standard method was used for quantitation. Under the optimized conditions, at the addition levels of the limits of quantitation (LOQs), 0.5 MRL (maximum residue limit), 1 MRL and 2 MRL, the average recoveries of dinitolmide and 3-ANOT in chicken tissues were 81.96–94.31%, and the relative standard deviations (RSDs) were 1.72–5.37%. The limits of detection (LODs) (S/N ≥ 3) of dinitolmide and 3-ANOT in chicken tissues were 0.8–2.5 μg/kg, and the LOQs (S/N ≥ 10) were 2.7–8.0 μg/kg. The method validation parameters met the Chinese Ministry of Agriculture, European Union and United States Food and Drug Administration veterinary drug residue detection requirements. [ABSTRACT FROM AUTHOR]

A high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method and an ultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for determining eight coccidiostat (halofuginone, lasalocid, maduramicin, monensin, narasin, nigericin, robenidine and salinomycin) residues in beef were developed and compared. Samples were extracted with a mixture of acetic acid, acetonitrile and ethyl acetate and were then purified on a C 18 solid-phase extraction (SPE) column. The purified samples were analyzed by HPLC-MS/MS and UPLC-MS/MS, using 0.1% formic acid-water solution (A) and pure methanol (B) as the mobile phase. The samples were fractionated on a C 18 column using different gradient elution procedures, followed by qualitative analysis using a mass spectrometer operated in multiple reaction monitoring (MRM) mode with positive electrospray ionization; the external standard method was used for quantitation. At spiked levels that ranged from the limit of quantification (LOQ) to 100 μg/kg, the average recoveries were 71.96%–100.32% and 71.24%–89.24%, with relative standard deviations (RSDs) of 2.65%–12.38% and 2.98%–14.86% for UPLC-MS/MS and HPLC-MS/MS, respectively. The limits of detection (LODs) and LOQs of the eight coccidiostats were 0.14–0.32 μg/kg and 0.43–1.21 μg/kg, respectively, for UPLC-MS/MS analysis and 0.16–0.58 μg/kg and 0.53–1.92 μg/kg, respectively, for HPLC-MS/MS analysis. Both methods had good accuracy and precision, but UPLC-MS/MS had higher sensitivity than HPLC-MS/MS. [ABSTRACT FROM AUTHOR]

This paper describes a novel method that combines acetic anhydride derivatization with gas chromatography–electron ionization tandem mass spectrometry (GC–EI/MS/MS) for the sensitive and selective determination of piperazine in chicken and pig tissues. Samples were extracted using an accelerated solvent extraction (ASE) apparatus, purified by solid-phase extraction (SPE) and derivatized with acetic anhydride. This optimized method was validated according to the requirements defined by the European Union and the Food and Drug Administration. At the limit of quantification (LOQ) spiked levels of 50.0, 100.0, 500.0, 1000.0 and 2000.0 μg/kg, the average recoveries of piperazine in chicken and pig tissues were 77.46–96.26%, with relative standard deviations (RSDs) of 1.55–6.64%. The intra-day RSDs were 1.39–5.92%, and the inter-day RSDs were 2.24–8.39%. The limits of detection (LODs) and the LOQs were 1.4–1.6 μg/kg and 4.8–5.2 μg/kg, respectively. The decision limits (CC α ) were 102.02–105.17 μg/kg, and the detection capabilities (CC β ) were 104.03–109.09 μg/kg. Finally, the new approach was verified for the quantitative determination of piperazine in 30 commercial chicken and pig tissues from local supermarkets. [ABSTRACT FROM AUTHOR]

[Display omitted] • Nine genera were identified as dominant spoilage bacteria of chilled chicken. • WGCNA analysis detects six modules of highly correlated metabolites. • Integrated microbiome-metabolomics analysis identifies spoilage-related metabolic pathways. • OPLS regression model identifies 51 key metabolites related to the spoilage of chilled chicken. • Correlation analysis provides reveals relationships between spoilage bacteria and metabolites. Spoilage of chilled chicken can occur as a result of microbial development and consumption of meat nutrients by spoilage bacteria, ultimately resulting in the release of undesired metabolites. Characterizing the profiles of the microbiota and metabolites and clarifying their relationships will contribute to an improved understanding of the mechanism underlying chilled chicken spoilage. In the present study, 16S rRNA gene sequencing and ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS)-based untargeted metabolomics analyses were applied to determine the microbial and metabolic profiles in chicken during chilled storage. The microbial and metabolic datasets were subjected to combined analysis using weighted gene co-expression network analysis (WGCNA) and Spearman's correlation analysis. Brochothrix , Carnobacterium , Photobacterium , Pseudomonas , Acinetobacter , Serratia , Kurthia , Shewanella , and Obesumbacterium genera were identified as the dominant spoilage bacteria in chilled chicken. Ten metabolic pathways, including histidine metabolism and purine metabolism, were identified as potential mechanisms underlying chilled chicken spoilage. Correlation analysis demonstrated that spoilage bacterial genera were highly correlated with spoilage-related metabolites. Taken together, the present study proposed an integrated microbiome and metabolomics approach to investigate the mechanism of chilled chicken spoilage caused by microbial activity. The results obtained by this approach provide a comprehensive insight into changes in the microbial and metabolic profiles of chilled chicken during spoilage. [ABSTRACT FROM AUTHOR]