Carry-over of Acrylamide from Feed (Heated Potato Product) to Eggs and Body Tissues of Laying Hens

A total of 16 hens were allocated to two groups. Hens were kept individually in a cage battery. During a four-week experiment 120 g feed were given per hen and day of consumption. The diet consisted of commercial potato meal (50%) as well as soy meal, barley and premix. The potato meal for the experimental group was heated for 2 h at 150°C. While the determined acrylamide content in the experimental diet was 671 ± 32 μg per kg, it was 125 ± 40 μg/kg in the diet of the control group. Acrylamide was determined by gas chromatography – mass spectrometry in the diet as well as in body tissue and eggs. During the experiment the acrylamide concentration in the eggs increased in both, the experimental and the control group. After three weeks, the acrylamide concentration in the eggs remained constant (max. 17.2 μg/kg egg). The carry-over rates for acrylamide from the diet to the egg were 0.022 in experimental and 0.010 in control hens. All hens were slaughtered at the end of the trial. The highest content of acrylamide was found in the kidneys of the experimental hens (27.7 μg/kg). It may be concluded that even for the highest acrylamide concentration considered the contribution of poultry products to the total acrylamide intake by humans is low.

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Zusammenfassung. 16 Legehybriden (LSL) wurden in 2 Gruppen aufgeteilt und in Einzelhaltung untergebracht. Die Hennen erhielten über vier Wochen t?glich 120 g Futter. Die Futtermischung setzte sich aus 50% eines küchenfertigen, handelsüblichen Kartoffelpulvers sowie Sojaextraktionsschrot, Gerste und einem Pr?mix zusammen. Das Kartoffelmehl der Versuchsgruppe wurde bei 150°C 2 h lang ger?stet. Die fertige Futtermischung der Versuchsgruppe enthielt 671 ± 32 μg Acrylamid/kg Futter und die Mischung der Kontrollgruppe 125 ± 40 μg/kg. Der Gehalt an freiem, unkonjugiertem Acrylamid in den Proben und im Futter wurde mittels GC-MS untersucht. Im Versuchsverlauf stieg in den Eiern der Hennen beider Gruppen die Acrylamidkonzentration an. Nach einer dreiw?chigen Versuchsdauer ?nderten sich die Konzentrationen an Acrylamid im Ei nicht mehr (max. Konzentration: 17,2 μg/kg Eimasse). Die Carry-over – Faktoren für Acrylamid vom Futter ins Ei betrugen bei den Kontroll- bzw. Versuchstieren 0,022 bzw. 0,011. Die h?chste Acrylamid-Konzentration wurde in den Nieren der Tiere der Versuchsgruppe ermittelt (27,7 μg/kg). Selbst unter Berücksichtigung der h?chsten Acrylamidkonzentrationen ist der Beitrag der Geflügelprodukte an der gesamten Acrylamidaufnahme des Menschen gering.

     

固相萃取-超高效液相色谱-串联质谱法测定鸡蛋中甲硝唑残留

目的 优化固相萃取-超高效液相色谱-串联质谱法(solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry,SPE-UPLC-MS/MS)测定鸡蛋中甲硝唑残留的分析方法.方法 样品经乙酸乙酯提取,用MCX...     

氟苯尼考在产蛋前期鸡蛋中的残留规律及膳食暴露评估

目的：为了探索开产前蛋鸡使用氟苯尼考后产蛋前期鸡蛋中氟苯尼考的残留规律,评估氟苯尼考对鸡蛋安全性的影响,评价其食用风险。方法：蛋鸡开产前不同时间预防性投喂氟苯尼考后测定鸡蛋中氟苯尼考残留量。结果：给药期间鸡蛋中氟苯尼考和氟苯尼考胺的残留量逐渐升高可达到峰值,或停药后1 d达到峰值,最大残留量出现在第4组为515.86 μg/kg。停药后5 d,鸡蛋中氟苯尼考和氟苯尼考胺的残留总量基本小于100 μg/kg。随着蛋鸡日龄的增长,产蛋率逐渐升高,停药后10~14 d鸡蛋中氟苯尼考和氟苯尼考胺残留量低于检出限。结论：对照实验各组鸡蛋中的检出是氟苯尼考和氟苯尼考胺的浓度总和,开产前23 d使用氟苯尼考,开产后所产鸡蛋对成人和婴儿都是安全的。     

Doxycycline depletion and residues in eggs after oral administration to laying hens

The depletion of doxycycline (DC) residues in eggs was determined after oral drug administration by drinking water to laying hens. The antibiotic was supplied to birds for 5 consecutive days and the eggs were collected during medication and 18 days after withdrawal. DC residues were determined by LC-MS/MS. DC was isolated from eggs with a solution of 0.02 M of oxalic acid (pH 4), 0.1 M Na₂EDTA and acetonitrile. The limit of detection (LOD) and limit of quantification (LOQ) of the method were 2 and 5 µg kg^–1, respectively. Analyses were performed on whole egg, egg white and yolk separately. DC was detectable 24 h after the beginning of administration. The concentration of antibiotic increased daily, resulting in the highest DC concentration in whole eggs at the first day of the withdrawal period. Thirteen days after withdrawal, the content of DC in whole eggs was below the LOQ of the method. However, some differences were found in the depletion curve of DC between egg white and yolk. Residues of DC in egg white were much higher during treatment and 1 day after withdrawal, but later the concentration in egg white decreased fairly rapidly and a higher DC content in egg yolk was observed. The depletion period was shorter for egg white than for yolk, and DC was detected in the egg white until 12 days after withdrawal and 2 days more in egg yolk than in white. DC reached a peak faster in egg white, but the residues were detectable for longer period in the yolk.     

液相色谱-质谱/质谱法测定鸭蛋中氟苯尼考残留量不确定度评定

目的 对鸭蛋中氟苯尼考残留测定的不确定度进行评定,找出影响检测结果准确性的关键因素,从而提高检测结果准确性。方法 按照GB/T 22338-2008《动物源性食品中氯霉素类药物残留量测定》液相色谱-质谱/质谱法对鸭蛋中氟苯尼考残留量进行测定。依据CNAS-GL006:2018 《化学分析中不确定度的评估指南》建立数学模型,对影响测量结果的不确定度来源如标准物质的纯度、标准物质的称量、标准曲线的配制、样品的称量、样品的制备、标准曲线的拟合、样品测量重复性等因素进行了分析和评定。结果 鸭蛋中氟苯尼考残留量为210 μg/kg,扩展不确定度为18 μg/kg,测定结果表示为：X=(210±18) μg/kg(k=2)。结论 样品测量重复性和标准曲线配制是本次测定测量不确定度的主要来源,在检测过程中应加以控制。     

液相色谱-串联质谱结合谱库检索测定猪组织中13种氟喹诺酮类药物

采用MRM→IDA→EPI→谱库检索模式建立了猪组织中13种氟喹诺酮类药物的液相色谱-电喷雾串联质谱多残留检测方法,结合谱库检索功能同时实现了定性定量分析.组织样品经N,N-二甲基甲酰胺-乙腈混合溶液提取,Waters HLB柱净化,本方法13种氟喹诺酮类药物的线性范围为1.0～5000.0 μg/kg,线性相关系良好...     

氟苯尼考在鸡蛋和蛋鸡组织中的残留规律及预测模型建立

氟苯尼考是一种被广泛应用于动物养殖过程中的抗生素药物,可能残留于畜产品中,被人类长期食用会对机体造成耐药性、免疫抑制等不良影响.本实验旨在探讨蛋鸡摄入不同剂量氟苯尼考后,鸡蛋及各组织中氟苯尼考及其代谢产物氟苯尼考胺的清除规律,建立残留预测数学模型.本实验选取处于产蛋高峰期的罗曼粉壳蛋鸡250只(350日龄、体质量(1....     

LC-MS/MS法检测卷烟滤嘴截留的烟气TSNAs

为了解滤嘴对烟草特有亚硝胺(TSNAs)的截留效率,采用液相色谱-串连质谱(LC-MS/MS)法测定了30种卷烟样品滤嘴中截留的烟气TSNAs:NNN、NAT、NNK、NAB。用0.1mol/L醋酸铵水溶液萃取烟蒂滤嘴,萃取液过OASIS MCX小柱,用50%(体积分数)甲醇洗脱,洗脱液直接进行LC-MS/MS分析,分析条件为:色谱柱:Waters Symmetry Shield TM RP18柱,柱温:65℃;流动相:50%甲醇水溶液(水中含0.1%醋酸),等度洗脱,流速0.25mL/min。结果显示:①NNN、NAT、NNK和NAB的检测限分别为0.7、0.3、0.6和0.4ng/支,回收率96.0%～103.5%,相对标准偏差(RSD)均小于8%;②NNN、NNK、NAT、NAB的滤嘴截留率分别在16.67%～43.05%、30.51%～55.97%、16.19%～45.00%和41.68%～49.08%范围内;③混合型卷烟滤嘴对NNN、NAT的截留效率要高于烤烟型卷烟,而对NNK、NAB和TSNAs总量,混合型卷烟滤嘴和烤烟型卷烟滤嘴的接近;④醋酸纤维滤嘴对NNK、NAB的截留率与聚丙烯纤维滤嘴相当,...     

LC-MS/MS法分析清爽型黄酒中的嘌呤含量

嘌呤是引起痛风的关键因素,检测黄酒中的嘌呤含量具有重要意义。本研究建立了一种采用液相色谱串联质谱法(LC-MS/MS)测定黄酒中嘌呤含量的方法。结果表明,清爽型黄酒中鸟嘌呤为0.67 mg/L,次黄嘌呤为0.62 mg/L,腺嘌呤为0.82 mg/L,总含量为2.12 mg/L。LC-MS/MS法样品加标回收率在98.2%-100.6%之间,相关系数大于0.995,相对标准偏差为3.8%-5.2%。     

LC-MS/MS法测定人血浆中曲司氯铵的浓度

目的建立测定人血浆中曲司氯铵浓度的LC—MS／MS方法。方法血浆样品经液-液提取后,以甲醇（含0．1％乙酸）：水（含0．1％乙酸＋2．5mmol／L酸铵）（80：20）为流动相,使用Agilent1100VL型离子阱质谱仪,电喷雾离子源正离子模式,采用多反应离子监测方式测定曲司氯铵（MRM,m／z392→164＋182）。结果血浆中曲司氯铵线性范围为0．1～10．0ng／mL,定量下限为0．1ng／mL,准确度85％～115％,日内、日间精密度（RSD）±15％。结论该方法准确,专属性强,可用于曲司氯铵药动学研究。     

卷烟主流烟气中挥发性醛酮的LC-MS/MS分析

采用2,4-二硝基苯肼衍生-LC-MS/MS法测定了32种卷烟样品主流烟气中的甲醛、乙醛、丙烯醛、丙酮、丙醛、巴豆醛、甲基丙烯醛、2-丁酮、丁醛、苯甲醛、戊醛、己醛.结果表明:①方法的检测限为0.1～0.5 ng/mL,回收率在91.6%～100.3%之间,相对标准偏差为3.28%～7.86%;②卷烟样品主流烟气的挥发性醛酮成分中主要为乙醛和丙酮,苯甲醛、已醛含量较小;③与进口烟相比,国产烤烟型卷烟主流烟气中的挥发性醛酮含量相对较高,混合型卷烟的相对较低;④不管是烤烟型还是混合型,焦油量高的卷烟主流烟气中的挥发性醛酮含量均相对较高.     

液相色谱-串联质谱法测定食品中红2G、酸性红、酸性红52着色剂方法研究

建立了食品中红2G、酸性红、酸性红52的高效液相色谱-串联三重四级杆质谱测定方法。样品经聚酰胺粉吸附法净化,以乙腈和乙酸铵为流动相,梯度洗脱分离,在负离子和多反应监测(MRM)模式下进行定性定量分析。食品中红2G、酸性红、酸性红52的方法检出限分别为5μg/L、6μg/L、1μg/L;在30μg/L-1000μg/L浓度范围内线性良好,相关系数较好;方法平均回收率在80%以上,相对标准偏差均小于10%。该方法定性准确、灵敏度高,适用于食品中红2G、酸性红、酸性红52这3种合成着色剂的同时检测。     

LC-MS/MS法测定吸烟者和被动吸烟者尿液中的烟碱及其代谢物

以烟碱-d3、可替宁-d3、反3'-羟基可替宁-d3作内标,XDB C18柱作色谱柱,10 mmol/L(pH6.8)乙酸铵水溶液和无水甲醇为流动相,梯度洗脱,流速1 mL/min,采用LC-MS/MS法同时测定了10名吸烟者和5名被动吸烟者尿液中烟碱及其糖苷、可替宁及其糖苷、反3'-羟基可替宁及其糖苷、降烟碱、降可替宁、可替宁氮氧化物和烟碱氮氧化物.结果表明:①烟碱及其代谢物的精密度在2.1%～17.0%之间,回收率在78%～116%之间;②日抽吸20支相同品牌卷烟的吸烟者尿液中烟碱及其9种代谢物的含量差异较大;③被动吸烟者尿液中都检测出烟碱、可替宁、反3'-羟基可替宁,部分检出可替宁糖苷、降烟碱、烟碱氮氧化物,且前3种物质的浓度略高于后3种,但都远远低于吸烟者.烟碱、可替宁、反3'-羟基可替宁有可能作为人体尿液中被动吸烟的生物标记物.     

Assessing the depletion of lincomycin in feathers from treated broiler chickens: a comparison with the concentration of its residues in edible tissues

ABSTRACT

Lincomycin is the first antimicrobial agent described for the lincosamide class and it is commonly used for the treatment of infectious enteric and respiratory diseases in poultry. Maximum residue limits (MRLs) in edible tissues have been established for this antimicrobial, however, no regulation has been proposed yet for by-products that are not intended for direct human consumption. Feathers are a by-product from poultry farming that might be used as an ingredient for diets fed to other farm animal species. The presence of antimicrobial residues in them is not monitored in spite of the fact that several studies have proved that they can persist in feathers. Currently though, no evidence has been presented regarding the behaviour of lincomycin in this matrix. Hence, this work intended to assess the depletion of lincomycin residues in feathers of birds treated with therapeutic doses and compare them with those detected in muscle and liver samples. Samples were collected for several days after ceasing treatment from a group of broiler chickens treated with a 25% lincomycin formulation. Methanol and Florisil® columns were used to extract and retain the analyte, and samples were analysed using a triple quadrupole mass spectrometer (API 5500, AB SCIEX?). On day 1 after ceasing treatment, average concentrations of lincomycin detected in feather samples reached up to 8582 μg kg^?1 and by day 16, these had only declined by 63%, to an average of 3138 μg kg^?1. Lincomycin residues were detected in feathers at every sampling point, even after they were not detectable in edible tissues. Depletion time was 98 days for feathers, considering the LOQ established for the methodology as cut-off value for the calculations. Data showed that lincomycin is highly persistent in feathers, which may result in this matrix becoming a re-entry route for its residues into the food chain.     

超高效液相色谱-串联质谱法检测蛋鸡体内抗病毒药物利巴韦林

为研究禁用抗病毒药物利巴韦林在蛋鸡体内的残留性,对11 只京红蛋鸡以30 mg/kg体质量单次口服灌喂利巴韦林药物,采集给药后不同时间的静脉血,以超高效液相色谱-串联质谱法检测利巴韦林,多反应监测模式和同位素内标法定量。利巴韦林线性范围为5～5 000 ng/mL,检出限为1 ng/mL。在10～1 000 ng/mL范围内样品添加回收率为86.4%～97.1%,批内、批间相对标准偏差均满足定量要求。结果表明,给药后血浆中利巴韦林质量浓度迅速升高,随着代谢消除进行,血浆中利巴韦林质量浓度逐渐下降,至24 h血浆中利巴韦林质量浓度低于方法检出限。蛋鸡口服给药利巴韦林后吸收迅速,到达峰值时间短,体内分布广,消除速度快,残留性不高。     

Effect of added cassava root meal,ZnO and their interaction on the production and quality of eggs from laying hens

Two hundred and sixteen (108 Hisex Brown; 108 Warren Studler) laying hens were given one of 12 dietary treatments. These were four basic diets with 0, 200, 400 and 600 g added cassava kg^?1 and each basic diet was further subdivided and ZnO added to provide 100 and 200 mg Zn kg^?1. None of the production traits measured was significantly affected by either added cassava or ZnO but there was a quadratic response in food intake to added cassava. ZnO addition significantly improved egg quality (assessed by Haugh score) but did not affect shell thickness. Haugh score was significantly affected by added cassava, the responses being significant after 2 weeks storage. The interaction between Zn level and cassava level significantly affected egg quality.