高效液相色谱法同时测定水产品中13种磺胺类药物残留的研究

建立了一种同时测定水产品(鳗鱼、鮰鱼、龙虾)中13种磺胺类药物残留的高效液相色谱法。样品经乙腈提取,正己烷液-液分配,阳离子固相萃取小柱净化后,采用高效液相色谱分离,紫外检测器检测,外标法定量。13种磺胺类药物在0.1～5.0μg/ml范围内线性关系良好,相关系数R2为0.9997～0.9999,加标回收率为62%～97%,相对标准偏差为2.01%～10.46%。定量测定低限磺胺二甲嘧啶、磺胺甲氧嘧啶、磺胺-6-甲氧嘧啶、磺胺氯哒嗪、磺胺甲基异恶唑、磺胺二甲异恶唑、磺胺间二甲氧嘧啶、磺胺喹恶啉为0.02mg/kg,磺胺嘧啶、磺胺吡啶、磺胺噻唑、磺胺甲基嘧啶、磺胺甲噻二唑为0.05mg/kg。     

动物性食品中磺胺类药物残留分析研究进展

介绍了动物性食品中磺胺类药物残留的来源和危害,着重对动物性食品中常见的磺胺类药物残留的分析方法进行了综述,为研究最有效的检测方法奠定了基础。     

恩诺沙星注射液在猪体内残留消除规律研究

目的研究恩诺沙星注射液在猪体内的残留消除规律。方法本实验采用30头约50 kg重长白猪,随机分为2组,给药组25头,对照组5头。给药组用药量为每次2.5mg恩诺沙星/kg,每日1次,连用3d(1个疗程),使用1个疗程,对照组不给任何抗菌药物,与给药组同环境饲养。在最后一次给药6 h、24 h(1 d)、72 h(3 d)、120 h(5 d)、168 h(7 d)时采集肉、肝、肾、脂肪样本,经液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)测定组织中的恩诺沙星及其代谢物环丙沙星残留量之和,并利用WT1.4软件计算休药期。结果恩诺沙星注射液在猪肉中的休药期为3.17 d;在肾脏中的休药期为3.75 d;在肝脏中的休药期为8.18 d;在脂肪总的休药期为4.09 d。结论为保证兽药使用安全、食品安全和消费者健康,推荐恩诺沙星注射液在猪体内的休药期为9 d。     

肉制品中亚硝酸盐残留的控制

简述了亚硝酸盐在肉制品加工中的作用,以及过量使用亚硝酸盐的危害,通过亚硝酸盐作用机理的简述,以及亚硝酸盐作用效应的分析,探讨了亚硝酸盐在肉制品中残留情况的控制方法。     

DNA tests based on coat colour genes for authentication of the raw material of meat products from Iberian pigs

Traceability in the meat supply chain depends on systems based on electronic identification, but DNA tests would be suitable to audit the genetic origin of some labelled meat products. Differentiated labelling is required for highly prized meat products from purebred Iberian pigs and from animals crossbred with the Duroc breed. A panel of breed specific markers based on polymorphisms found in two coat colour genes was investigated in the present study. The genotyping of the G/C or A/G polymorphisms at nucleotide positions ?160 and 727 bp of the melanocortin receptor 1 (MC1R) gene can be indistinctly used to discriminate the Duroc specific allele (MC1R*4) from all the alleles (MC1R*3, MC1R*6 and MC1R*7) found in the Iberian breed. It allows one to differentiate unambiguously samples from purebred Iberian and Duroc crossbred genotypes. The additional genotyping of the A/G polymorphism at position 2462 of the pink‐eyed dilution (OCA2) gene, four microsatellites (SW24, SW413, SW874 and SW1057) and nine amplified fragment length polymorphism (AFLP) markers would allow one to detect Duroc crossbred genotypes with a probability of exclusion of the pure Iberian origin greater than 0.968. The validation of batches of marketed products may be achieved with more single tests on pooled DNA samples. Copyright © 2004 Society of Chemical Industry     

中国与主要贸易国水产品中农药残留限量标准对比分析

中国是水产品生产和消费大国,近年来,为有效控制水产养殖过程中的病虫害,部分农药被作为除藻剂、杀虫剂等大量应用于养殖生产中,导致水产品中农药残留超标事件频发.农药最大残留限量(maximum residue limit,MRL)标准是国际水产品贸易的主要技术性手段和市场准入门槛,也是各国构建贸易壁垒的主要措施.为进一步完...     

Pseudoendogenous origin of prednisolone in pigs from the food chain

The debate about the origin of prednisolone in animal organisms has lasted for 5 years. Bovine species have been the most studied, but studies on humans and horses are also present in the literature. Even if prednisolone in pigs does not yet represent a problem for control agencies, interest has recently increased with regard to this species. To date, there has been just a single study in the literature about this topic, performed on 10 sows treated with prednisolone or a synthetic analogue of adrenocorticotropic hormone. We therefore initiated a study on 80 pigs, a number considered representative in relation to the expected frequency (prevalence) of prednisolone detection in urine collected at slaughter. Prednisolone was detected in urine both at the farm and at the slaughterhouse, with a concentration and frequency higher at slaughter. The presence of prednisolone was also studied in the adrenal glands, where the corticosteroids are produced in response to stress, and it was detected in 89% of the samples. These results, together with the similar behaviours of prednisolone and cortisol, i.e. a mutual rise in the two corticosteroids in urine collected at the slaughterhouse and the correlation between the concentrations of the two corticosteroids in the adrenal glands, seem to indicate an endogenous origin of prednisolone in pigs.     

Effect of fiber type on postmortem proteolysis in longissimus muscle of Landrace and Korean native black pigs

The current study was conducted to characterize objective meat quality, fiber type and their relations to postmortem proteolysis in longissimus muscle of Landrace and Korean native black (KNP) pigs. Longissimus muscles from each 10 market-weighted male pigs were removed after conventional slaughtering and chilling procedures, and aged for 1 or 7 days at 4 °C to determine WB-shear force, objective meat color, proportion of myosin heavy chain I (MyHC I), intramuscular fat content and rate of proteolysis by a proteomics approach. KNP had a significantly (p < 0.05) higher content of MyHC I, and that concurred with greatly (p < 0.05) higher intramuscular fat content and Hunter a^* value, and significantly (p < 0.05) lower drip loss than those seen in Landrace. One-dimension SDS-PAGE indicated that GAPDH, troponin I and creatine kinase were prominent proteolytic products during chiller ageing. By applying a gel-based proteome analysis, 26 proteins were identified, which showed different degradation properties during ageing between the breeds. Biopsied sample revealed that myosin regulatory light chain 2, myosin light chain isotype v/sb, fatty acid-binding protein and albumin were expressed at a greatly higher level for KNP, but their relation to fiber type (or genetic background) is unclear. It was particular noticeable that different actin isoforms showed various degradation behavior during ageing time.     

高效液相色谱-质谱联用技术测定豆制品中 7种违禁色素的残留

目的建立高效液相色谱-串联四极杆质谱法(high-performance liquid chromatography-mass spectrometry,HPLC-MS/MS)测定豆制品中二甲基黄、二乙基黄、罗丹明B、碱性橙2、碱性橙21、碱性橙22和碱性嫩黄7种违禁色素残留量的分析方法。方法豆制品经水溶解后,再以乙腈提取7种违禁色素,采用甲醇和0,1%甲酸水溶液作为流动相进行梯度洗脱,流速为0.3 mL/min,经Agilent ZORBAX SB-C_(18)色谱柱(50mm×2.1 mm,3.1μm)进行分离,电喷雾电离源(ESI),正离子模式,多反应监测模式(MRM)对违禁色素的定性离子和定量离子进行监测。结果本方法的线性范围为0~10.0 ng/mL,相关系数(r~2)均大于0.999,加标水平为2.0μg/kg时,回收率范围是80.5%~104.3%,相对标准偏差(n=6)为2.88%~7.63%,检出限为2.0μg/kg。结论该方法前处理简单,分析时间短,适用于对豆制品中7种违禁色素残留的同时检测。     

Ultrasonic and sensory characterization of dry-cured ham fat from Iberian pigs with different genetics and feeding backgrounds

The textural and ultrasonic properties of the subcutaneous fat from five batches of dry-cured hams from animals with different genetics (Iberian, Iberian×Duroc) and type of feeding ("montanera", concentrate feeds with different oleic acid content) were studied and related to the sensory traits (oiliness and brightness) of their biceps femoris muscle. The different genetics and feeding backgrounds found in the batches brought about differences in their ultrasonic velocities (average velocity from 4 to 20°C ranged from 1608 to 1650m/s) and textural parameters (maximum force at 8°C ranged from 11 to 21N). On average, batches with lower textural parameters had lower velocities and higher sensory scores. Ultrasonic measurements were used to carry out a discriminant analysis which allowed 78.3% of the samples to be correctly classified in the batches considered. Therefore, ultrasonic and sensory techniques could be useful in the characterization and differentiation of dry-cured hams from Iberian pigs.     

Physiologically based pharmacokinetic model for quinocetone in pigs and extrapolation to mequindox

ABSTRACT

Physiologically based pharmacokinetic (PBPK) models are scientific methods used to predict veterinary drug residues that may occur in food-producing animals, and which have powerful extrapolation ability. Quinocetone (QCT) and mequindox (MEQ) are widely used in China for the prevention of bacterial infections and promoting animal growth, but their abuse causes a potential threat to human health. In this study, a flow-limited PBPK model was developed to simulate simultaneously residue depletion of QCT and its marker residue dideoxyquinocetone (DQCT) in pigs. The model included compartments for blood, liver, kidney, muscle and fat and an extra compartment representing the other tissues. Physiological parameters were obtained from the literature. Plasma protein binding rates, renal clearances and tissue/plasma partition coefficients were determined by in vitro and in vivo experiments. The model was calibrated and validated with several pharmacokinetic and residue-depletion datasets from the literature. Sensitivity analysis and Monte Carlo simulations were incorporated into the PBPK model to estimate individual variation of residual concentrations. The PBPK model for MEQ, the congener compound of QCT, was built through cross-compound extrapolation based on the model for QCT. The QCT model accurately predicted the concentrations of QCT and DQCT in various tissues at most time points, especially the later time points. Correlation coefficients between predicted and measured values for all tissues were greater than 0.9. Monte Carlo simulations showed excellent consistency between estimated concentration distributions and measured data points. The extrapolation model also showed good predictive power. The present models contribute to improve the residue monitoring systems of QCT and MEQ, and provide evidence of the usefulness of PBPK model extrapolation for the same kinds of compounds.     

多杀菌素在农产品中的残留研究进展

多杀菌素为新型的绿色生物杀虫剂,已广泛应用于农产品生产。目前,世界多国以多杀菌素A和多杀菌素D的总和来评估农产品中的多杀菌素残留,并制定了多杀菌素的每日允许摄入量和农产品中的多杀菌素最大残留限量。研究表明,多杀菌素残留在农产品生产、贮藏及其深加工过程存在不同的保留特性。     

A feasibility study on the use of near-infrared spectroscopy for prediction of the fatty acid profile in live Iberian pigs and carcasses

This work reports on the development and optimisation of NIRS technology for fat characterization both in live pigs and in carcasses in the slaughterhouse; use of this technology would enable implementation of a real-time traceability and control system based on non-destructive sensors. A total of 52 Iberian pig fat samples were analysed using a LabSpec^®Pro A108310 spectrophotometer (Analytical Spectral Device Inc.), with a high-intensity fiber-optic contact probe. Spectra were collected in five analysis modes: from the live animal, from the carcass in the slaughterhouse, from a subcutaneous fat sample with skin, from a skin-free subcutaneous fat sample and from a transverse section. Calibrations were developed for the prediction of the four main fatty acids in Iberian pig fat, obtaining for palmitic acid SECV values of 1.24% for in vivo analysis and 0.82% for carcass analysis, for stearic acid 0.67% and 0.94%, for oleic acid 1.42% and 1.48% and for linoleic 0.36% and 0.55%, respectively. The calibrations accounted for between 60% and 74% of the variation recorded in live animals, and between 31% and 87% of variation in carcasses. These results confirm the feasibility of NIRS technology for the on-site inspection and control of Iberian pig, both in the field and in the slaughterhouse.     

Use of pure glycerol in fattening heavy pigs

Eighty Italian Duroc×Italian Large White pigs (BW 42.6±3.37kg) were used to determine the effects of pure glycerol on growth performance and meat quality of heavy pigs. Pigs were divided into five groups receiving 0% (control), 5% or 10% during the growing and finishing phases (42.6-160kg BW) (G+F5,G+F10) or 5% or 10% during the finishing period (100-160kg BW) (FIN5,FIN10) of pure glycerol in substitution for maize meal (on a dry matter basis). The pigs were slaughtered at approximately 160kg BW. The growth performance of pigs fed 5% glycerol did not differ from controls regardless of feeding duration, whereas those fed 10% glycerol showed reduced growth and poorer feed:gain ratio. Fat quality and meat suitability for raw ham curing were not affected by dietary treatment. Differences were not consistent enough to draw any conclusion about the effects of feeding glycerol on sensory characteristics.     

液相色谱—串联质谱法测定猪可食用组织中氨茶碱残留

目的:研究猪可食用组织中氨茶碱药物残留的定性定量测定方法。方法:建立固相萃取净化结合高效液相色谱—串联质谱法,试样中的氨茶碱药物残留被甲醇溶液提取后,经PRiME HLB固相萃取柱一步净化,随后用C₁₈色谱柱分离,以0.1%甲酸水溶液和乙腈分别作为水相和有机相对氨茶碱进行色谱柱梯度洗脱,利用电喷雾正电压离子化并采用多反应监测模式进行化合物检测,空白基质匹配标准曲线外标法定量。结果:氨茶碱药物在3.5 min内完成仪器分析,不同基质的匹配曲线在0.005～0.1μg/mL质量浓度范围内呈良好的线性关系(R>0.998 0),猪肉、猪肝、猪肾的方法加标平均回收率为87.2%～101.3%,相对标准偏差为0.7%～6.2%(n=6),方法检出限为2μg/kg,定量限为5μg/kg。结论:该方法简便高效、重复性好、灵敏度高,适用于猪的可食用组织中氨茶碱药物残留的定性定量分析。     

中国与主要贸易国水产品中渔药残留标准的对比分析

目的进一步完善水产品中渔药残留标准体系。方法对中国及主要贸易国水产品中禁用渔药有关规定和渔药残留限量标准进行了对比和分析。结果阐明了中国与主要贸易国渔药标准体系之间的差异。结论提出了加大渔药基础研究力度、抓紧规范水产"限用药"的定义和进一步明确限量标准制定原则及思路的措施和建议。     

水产品中亚硫酸盐的安全性及残留状况检测

对水产加工品中亚硫酸盐的安全性和残留状况进行了研究。结果表明：亚硫酸盐在鱼,虾,蟹制品中应用广泛;在不同的水产品加工中,亚硫酸盐的作用不同;制品中亚硫酸盐的残留量因加工方式和添加量而异。综合检测结果表明,亚硫酸盐污染已经成为水产加工品的主要污染因素之一。     

Estimation of residue depletion of cyadox and its marker residue in edible tissues of pigs using physiologically based pharmacokinetic modelling

Physiologically based pharmacokinetic (PBPK) models are powerful tools to predict tissue distribution and depletion of veterinary drugs in food animals. However, most models only simulate the pharmacokinetics of the parent drug without considering their metabolites. In this study, a PBPK model was developed to simultaneously describe the depletion in pigs of the food animal antimicrobial agent cyadox (CYA), and its marker residue 1,4-bisdesoxycyadox (BDCYA). The CYA and BDCYA sub-models included blood, liver, kidney, gastrointestinal tract, muscle, fat and other organ compartments. Extent of plasma-protein binding, renal clearance and tissue-plasma partition coefficients of BDCYA were measured experimentally. The model was calibrated with the reported pharmacokinetic and residue depletion data from pigs dosed by oral gavage with CYA for five consecutive days, and then extrapolated to exposure in feed for two months. The model was validated with 14 consecutive day feed administration data. This PBPK model accurately simulated CYA and BDCYA in four edible tissues at 24–120 h after both oral exposure and 2-month feed administration. There was only slight overestimation of CYA in muscle and BDCYA in kidney at earlier time points (6–12 h) when dosed in feed. Monte Carlo analysis revealed excellent agreement between the estimated concentration distributions and observed data. The present model could be used for tissue residue monitoring of CYA and BDCYA in food animals, and provides a foundation for developing PBPK models to predict residue depletion of both parent drugs and their metabolites in food animals.     

生猪屠宰的管理与未来走向

肉类食品是人类不可缺少的主要食物之一,而猪肉又是我国绝大多数居民的主要肉品来源,目前生猪屠宰行业正在调整变革当中,面对新形势,迫切需要加强对生猪屠宰行业发展的指导,以保障肉品质量安全。本文综述了我国生猪屠宰管理行业的发展现状、发展目标、发展形势及市场前景。     

肉制品中抗生素残留的危害和控制

肉制品中抗生素残留主要来源于注射、口服、饮水等方式,超量的抗生素残留对人体会造成危害。只有加强立法,完善检测方法,建立严格的管理体系,研制新的抗生素替代品,才能有效解决肉制品中抗生素残留问题。