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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 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 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. [ABSTRACT FROM AUTHOR]

A high-performance liquid chromatography – fluorescence detection (HPLC-FLD) method was established for the determination of piperazine residues in whole eggs, albumen, and yolk employing pre-column derivatization with dansyl chloride. The egg samples were treated by accelerated solvent extraction (ASE) and the analytes purified by solid phase extraction (SPE). Acetonitrile/ultrapure water was used as the mobile phase for gradient elution. The linear dynamic range was from 6.80 to 200.0 µg/kg for whole eggs, 7.50 to 200.0 µg/kg for albumen, and 6.50 to 200.0 µg/kg for yolk with coefficients of determination (R2) greater than or equal to 0.9992. The average recoveries of piperazine from egg samples were from 72.86 to 89.26% when the concentrations were equal to the limit of quantification, 0.5 times the maximum residue limit, equal to the maximum residue limit, and twice the maximum residue limits. The relative standard deviations were between 1.73 and 4.99%. The limits of detection of piperazine in eggs were from 1.92 to 2.50 µg/kg, and the limits of quantification were between 6.50 and 7.50 µg/kg. The method meets the requirements of the European Union, the Ministry of Agriculture of the People's Republic of China and the U.S. Food and Drug Administration (FDA) for the determination of veterinary drug residues. The validated HPLC-FLD method was successfully applied to the determination of piperazine residues in 50 eggs purchased from local supermarkets. [ABSTRACT FROM AUTHOR]

Accelerated solvent extraction (ASE) and solid‐phase extraction (SPE) conditions were optimized by a high‐performance liquid chromatography‐fluorescence detector (HPLC‐FLD) method for the detection of piperazine in chicken tissues and pork. Piperazine residues were determined by precolumn derivatization with trimethylamine and dansyl chloride. Samples were extracted with 2% formic acid in acetonitrile using an ASE apparatus and purified using a Strata‐X‐C SPE column. The monosubstituted product of the reaction of piperazine with dansyl chloride was 1‐dansyl piperazine (1‐DNS‐piperazine). Chromatographic separations were performed on an Athena C18 column (250 × 4.6 mm, id: 5 μm) with gradient elution using ultrapure water and acetonitrile (5:95, V/V) as the mobile phase. The calibration curves showed good linearity over a concentration range of LOQ‐200.0 μg/kg with a coefficient of determination (R2) ≥ .9992. The recoveries and relative standard deviations (RSD values) ranged from 78.49% to 97.56% and 1.19% to 5.32%, respectively, across the limit of quantification (LOQ) and 0.5, 1, and 2.0 times the maximum residue limit (MRL; μg/kg). The limits of detection (LODs) and LOQs were 0.96 to 1.85 μg/kg and 3.20 to 5.50 μg/kg, respectively. The method was successfully applied for the validation of animal products in the laboratory. [ABSTRACT FROM AUTHOR]

An innovative, rapid and stable method for simultaneous determination of three tetracycline (oxytetracycline, tetracycline and doxycycline) and two fluoroquinolone (ciprofloxacin and enrofloxacin) residues in poultry eggs by ultra-high performance liquid chromatography–fluorescence detection (UPLC-FLD) was established and optimized. The samples were homogenized and extracted with acetonitrile/ultrapure water (90:10, v/v) and then purified by solid-phase extraction (SPE). LC separation was achieved on an ACQUITY UPLC BEH C18 column (1.7 µm, 2.1 mm × 100 mm), and the mobile phase was composed of acetonitrile and a 0.1 mol/L malonic acid solution containing 50 mmol/L magnesium chloride (the pH was adjusted to 5.5 with ammonia). When the five target drugs were spiked at the limit of quantification, 0.5 times the maximum residue limit (MRL), 1.0 MRL and 2.0 MRL, the recoveries were above 83.5% and the precision ranged from 1.99% to 6.24%. These figures of merit complied with the parameter validation regulations of the EU and U.S. FDA. The limits of detection and quantifications of the targets were 0.1–13.4 µg/kg and 0.3–40.1 µg/kg, respectively. The proposed method was easily extended to quantitative analyses of target drug residues in 85 egg samples, thus demonstrating its reliability and applicability. [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 simple, rapid and novel method for the detection of residues of thiamphenicol (TAP), florfenicol (FF) and its metabolite, florfenicol amine (FFA), in poultry eggs by ultra-performance liquid chromatography-fluorescence detection (UPLC-FLD) was developed. The samples were extracted with acetonitrile-ammonia (98:2, v/v) using accelerated solvent extraction (ASE) and purified by manual degreasing with acetonitrile-saturated n-hexane. The target compounds were separated on an ACQUITY UPLC® BEH C18 (2.1 mm × 100 mm, 1.7 μm) chromatographic column using a mobile phase composed of 0.005 mol/L NaH2PO4, 0.003 mol/L sodium lauryl sulfate and 0.05% trimethylamine, adjusted to pH 5.3 ± 0.1 by phosphoric acid and acetonitrile (64:36, v/v). The limits of detection (LODs) and limits of quantification (LOQs) of the three target compounds in poultry eggs were 1.8–4.9 µg/kg and 4.3–11.7 µg/kg, respectively. The recoveries of the three target compounds in poultry eggs were above 80.1% when the spiked concentrations of three phenicols were the LOQ, 0.5 maximum residue limit (MRL), 1.0 MRL and 2.0 MRL. The intraday relative standard deviations (RSDs) were less than 5.5%, and the interday RSDs were less than 6.6%. Finally, this new detection method was successfully applied to the quantitative analysis of TAP, FF and FFA in 150 commercial poultry 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]

• Simultaneous determination of tetracycline, oxytetracycline, doxycycline, enrofloxacin and ciprofloxacin residues in chicken muscles by UPLC-FLD. • The fluorescence detector output signals were processed by dual-channel detection. • The sample pretreatment process was optimized. A sensitive, rapid and efficient ultra-performance liquid chromatography-fluorescence detection (UPLC-FLD) method was established for detecting tetracycline (TC), oxytetracycline (OTC), doxycycline (DOX), enrofloxacin (ENR) and ciprofloxacin (CIP) residues in chicken muscle. Moreover, the fluorescence detector output signals were processed by dual-channel detection. The samples were extracted with a mixture of acetonitrile and 0.1 M citric acid containing 100 mM magnesium chloride (1:1, V/V, adjusted the pH to 5.0 with ammonia) using liquid-liquid extraction (LLE) and purified by Oasis PRiME hydrophilic-lipophilic balance (HLB) solid-phase extraction (SPE) cartridges (60 mg/3 mL). The target compounds were separated on an ACQUITY UPLC BEH C 18 (100 mm × 2.1 mm, 1.7 μm) chromatographic column using a mobile phase composed of acetonitrile and 0.1 M malonic acid solution containing 50 mM magnesium chloride hexahydrate, and the pH was adjusted to 5.5 by adding ammonia. The limits of detection (LODs) and limits of quantification (LOQs) of the five target compounds in chicken muscle were 0.1–13.1 μg/kg and 0.4–39.4 μg/kg, respectively. The recoveries of the five target compounds in chicken muscles were above 87.33 % when the spiked concentrations were at the LOQ, 0.5 maximum residue limit (MRL), 1.0 MRL and 2.0 MRL. The intraday relative standard deviations (RSDs) were less than 4.91 %, and the interday RSDs were less than 5.13 %. Ultimately, this novel detection method was successfully applied to the quantitative analysis of TC, OTC, DOX, ENR and CIP in 20 commercial chicken samples from local supermarkets. [ABSTRACT FROM AUTHOR]