An innovative study on the qualitative identification and quantitative determination of spectinomycin and lincomycin residues in poultry (chicken, duck, and goose) muscles and pork using gas chromatography-tandem mass spectrometry (GC-MS/MS) was conducted. The samples were extracted and separated with accelerated solvent extraction (ASE) and then purified and enriched by solid-phase extraction (SPE). Then, the obtained residues were derivatized with 200 mu L bis(trimethylsilyl) trifluoroacetamide (BSTFA) for 60 min at 75 degrees C, and the derivative products were injected into a GC-MS/MS system. Under the optimized conditions, the limits of detection (LODs) and limits of quantification (LOQs) of spectinomycin and lincomycin in samples were 2.5-4.6 mu g/kg and 5.7-7.6 mu g/kg, respectively, the targets' recoveries were 79.7 %-94.2 %, the determination coefficients were 0.9992-0.9998, and the relative standard deviations (RSDs) were 1.2 %-3.5 %. The method revealed good linearity, and the parameters met the European Union requirements for the detection of veterinary drug residues. Poultry muscles and pork were procured from local stores for actual sample testing, confirming the feasibility and practicability of this method. Therefore, this study established an ASE-SPE-GC-MS/MS method to detect spectinomycin and lincomycin residues in animal-derived food.

A fast, simple and efficient ultrahigh-performance liquid chromatography-fluorescence detection (UPLC-FLD) method for the determination of residues of albendazole (ABZ) and its three metabolites, albendazole sulfone (ABZ-SO2), albendazole sulfoxide (ABZ-SO), and albendazole-2-aminosulfone (ABZ-2NH2-SO2), in pig and poultry muscle (chicken, duck and goose) was established. The samples were extracted with ethyl acetate, and the extracts were further subjected to cleanup by utilizing a series of liquid–liquid extraction (LLE) steps. Then, extracts were 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 C18 (2.1 mm × 100 mm, 1.7 μm) chromatographic column, using a mobile phase composed of 31% acetonitrile and 69% aqueous solution (containing 0.2% formic acid and 0.05% triethylamine). The limits of detection (LODs) and limits of quantification (LOQs) of the four target compounds in pig and poultry muscle were 0.2–3.8 µg/kg and 1.0–10.9 µg/kg, respectively. The recoveries were all above 80.37% when the muscle samples were spiked with the four target compounds at the LOQ, 0.5 maximum residue limit (MRL), 1.0 MRL, and 2.0 MRL levels. The intraday relative standard deviations (RSDs) were less than 5.11%, and the interday RSDs were less than 6.29%.

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.

本研究以鸡蛋、鸭蛋、鹅蛋为样本基质,建立一种加速溶剂萃取法结合超高效液相色谱-荧光法（UPLC-FLD）测定禽蛋中甲砜霉素残留。样品通过液-液萃取或加速溶剂萃取方法进行提取,乙腈饱和的正己烷去脂,复溶后利用液相色谱柱进行等度洗脱分离,而后采用荧光检测器进行定量。结果显示:甲砜霉素在空白禽蛋样品中的添加浓度在检测限（Limit of Detection,LOD）-250.0μg/kg范围内,相关系数均大于0.999 5,回收率为82.9%～95.3%,相对标准偏差均低于4.0%。检测限为3.3～3.4μg/kg,定量限为9.7～9.9μg/kg。综上,液-液萃取和加速溶剂萃取法均能很好地提取禽蛋样品中甲砜霉素,同时该检测方法高效、快速,适用于检测禽蛋中甲砜霉素残留。

本研究旨在建立鹌鹑蛋和鸽蛋中甲砜霉素(TAP)残留的超高效液相色谱-荧光检测(UPLC-FLD)方法.以鹌鹑蛋和鸽蛋为试验材料,采用加速溶剂萃取(ASE)技术提取目标物,以乙腈饱和的正己烷去脂,净化后用UPLC-FLD法进行检测分析.结果表明,在鹌鹑蛋和鸽蛋中TAP的添加质量比在定量限(LOQ)至250.0μg/kg内,线性关系良好,决定系数均大于0.9992.TAP添加质量比为LOQ、0.5 MRL、1.0 MRL和2.0 MRL时,在鹌鹑蛋和鸽蛋中的回收率分别为83.23％～95.72％、84.37％～97.12％,检测限(LOD)分别为3.4μg/kg、3.3μg/kg,LOQ分别为9.9μg/kg、9.7μg/kg.检测方法快速、高效、灵敏度高,为鹌鹑蛋和鸽蛋中TAP残留检测提供了新方法.

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.

建立了鸡肌肉、鸭肌肉和鹅肌肉中甲砜霉素(TAP)残留的超高效液相色谱荧光检测方法.禽肌肉样品采用了加速溶剂萃取(ASE)进行了提取、净化,乙酸乙酯饱和的正己烷去脂,净化后用超高效液相色谱荧光检测器(UPLC-FLD)进行分析.空白禽肌肉样品中TAP的添加量在LOQ ～ 250.0 μg/kg范围内,线性关系良好,决定系数在0.9997～0.9998之间.TAP添加水平为LOQ,0.5,1.0和2.0倍的最离残留限量(MRL)时,平均回收率在81.6％ ～ 97.2％范围内,相对标准偏差(RSD)在2.3％ ～4.0％之间,日内相对标准偏差在2.4％ ～4.9％之间,日间相对标准偏差在3.1％ ～5.3％之间.TAP在禽肌肉中的检测限(LOD)和定量限(LOQ)的范围分别为3.0 ～ 3.3 μg/kg和8.5～9.0μg/kg.方法 可用于检测禽肌肉中甲砜霉素的残留.

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.

ObjectiveTo establish an analytical method for simultaneous detections of florfenicol (FF) and its metabolite, florfenicol amine (FFA), in animal-derived foods.MethodSamples of pigeon and quail eggs were extracted by the accelerated solvent extraction (ASE) method with acetonitrile-ammonia (98:2, V/V) as the solvent. The extract was degreased and purified with acetonitrile-saturated n-hexane. A mobile phase consisting of 0.005 mol·L−1 NaH2PO4, 0.003 mol·L−1 sodium lauryl sulfate and 0.05% trimethylamine was used in the ultra-high performance liquid chromatography-fluorescence (ASE/UPLC-FLD) determination of FF and FFA contents.ResultHighly correlated linear relationships (R2>0.999 2) within the limit of quantitation (LOQ) were achieved between the peak area and concentration on the target compounds. The average recoveries of the method at the spiked levels of 50.0, 100.0, 200.0 μg·kg−1 and LOQ ranged from 84.69% to 98.04% with RSDs less than 3.7%. The method delivered the limit of detection (LOD) and LOQ on FF in the pigeon eggs at 4.8 µg·kg−1 and 11.2 µg·kg−1, respectively, and those on FFA, at 1.9 µg·kg−1 and 4.8 µg·kg−1, respectively; whereas, those on FF in the quail eggs, at 4.7 µg·kg−1 and 10.6 µg·kg−1, respectively, and those on FFA, at 1.8 µg·kg−1 and 4.6 µg·kg−1, respectively.ConclusionThe newly developed analytical methodology was rapid, simple, sensitive, and considered suitable for FF and FFA determinations in pigeon and quail eggs.

A method for the simultaneous analysis of amoxicillin (AMO), amoxicillin metabolites, and ampicillin residues in edible chicken muscle, liver, and kidney samples via high-performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI/MS/MS) was developed and verified. The extraction and purification procedures involved the extraction of the sample using a liquid-liquid extraction method with acetonitrile to eliminate the proteins. The chicken tissue extract was then injected directly onto an HPLC column coupled to a mass spectrometer with an ESI(+) source. The HPLC-ESI/MS/MS method was validated according to specificity, sensitivity, linearity, matrix effects, precision, accuracy, decision limit, detection capability, and stability, as defined by the European Union and Food and Drug Administration. The linearity was desirable, and the determination coefficients (r2 values) ranged from 0.9968 and 0.9999. The limits of detection and limits of quantification were 0.10–2.20 μg/kg and 0.30–8.50 μg/kg, respectively. The decision limits were 57.71–61.25 μg/kg, and the detection capabilities were 65.41–72.50 μg/kg, and the recoveries of the four target analytes exceeded 75% at the limits of quantification and exceeded 83% at 25, 50, and 100 μg/kg (n = 6 at each level), confirming the reliability of this method for determining these analytes and providing a new detection technology. For real sample analysis, this experiment tested 30 chicken tissue samples, only one chicken muscle, liver, and kidney sample were contaminated with 5.20, 17.45, and 7.33 μg/kg of AMO values, respectively, while other target compounds were not detected in the 30 tested chicken tissue samples.