Beagle犬体重与各脏器重量之间关系的回归分析

对４５只Ｂｅａｇｌｅ犬的体重与各脏器重量之间的关系进行了回归分析，并计算出相应的直线回归方程。对Ｂｅａｇｌｅ犬的脏器系数进行分析，显示脾脏、胸腺的变异系数较大，提示根据动物的脾脏、胸腺重量来评价其免疫功能时，要慎重考虑。     

Multiresidue analysis of sulfonamides in meat by supramolecular solvent microextraction,liquid chromatography and fluorescence detection and method validation according to the 2002/657/EC decision

A multiresidue method was described for determining eight sulfonamides, SAs (sulfadiazine, sulfamerazine, sulfamethoxypyridazine, sulfachloropyridazine, sulfadoxine, sulfamethoxazole, sulfadimethoxine and sulfaquinoxaline) in animal muscle tissues (pork, chicken, turkey, lamb and beef) at concentrations below the maximum residue limit (100 μg kg⁻¹) set by the European Commission. The method was based on the microextraction of SAs in 300-mg muscle samples with 1 mL of a supramolecular solvent made up of reverse micelles of decanoic acid (DeA) and posterior determination of SAs in the extract by LC/fluorescence detection, after in situ derivatization with fluorescamine. Recoveries were quantitative (98–109%) and matrix-independent, no concentration of the extracts was required, the microextraction took about 30 min and several samples could be simultaneously treated. Formation of multiple hydrogen bonds between the carboxylic groups of the solvent and the target SAs (hydrogen donor and acceptor sum between 9 and 11) were considered as the major forces driving microextraction. The method was validated according to the European Union regulation 2002/657/EC. Analytical performance in terms of linearity, selectivity, trueness, precision, stability of SAs, decision limit and detection capability were determined. Quantitation limits for the different SAs ranged between 12 μg kg⁻¹ and 44 μg kg⁻¹, they being nearly independent of matrix composition. Repeatability and reproducibility, expressed as relative standard deviation, were in the ranges 1.8–3.6% and 3.3–6.1%. The results of the validation process proved that the method is suitable for determining sulfonamide residues in surveillance programs.     

不同月龄Beagle犬的心电图研究

对不同月龄的６６只健康Ｂｅａｇｌｅ犬采用３％戊巴比妥钠麻醉，进行了９个导联的心电图描记和分析。结果表明：健康Ｂｅａｇｌｅ犬为窦性心律：３０月龄以下育成犬心律平均为１７３．８次／分，种用犬（５０月龄以上）心率平均为１３１．７次／分；二者经统计学处理，有极显著差异。Ｐ波间期平均为０．０５１±０．０１３Ｓｅｃ。Ｐ波振幅平均０．０６１ｍｖ，Ｐ波直立在导联中占９２．６％，在ａＶＲ导联中Ｐ波倒置率９８．７５％；ＱＲＳ波间期均值为：０．０２７±０．００５Ｓｅｃ。在Ⅱ导联中范围为０．０２－０．０４Ｓ－ｅｃ。在各导联中，Ⅰ导联以ｒ波为主（５１．８５％），Ⅱ导联以Ｒｓ波多见（５０％），Ｑｒ波和ｑｒ波在ａＶＲ导联中出现较多（３８．８９％，３１．４８％）。Ｔ波在Ⅰ、Ⅱ、Ⅲ、ａｖＦ、Ⅴ１、Ⅴ２、Ⅴ３导联中直立为主，在ａｖＬ导联中倒置多见（８９．２％，７３．１％）。Ｔ波方向与ＱＲＳ波一致。Ｔ波振幅平沟０．１３７ｍｖ。Ｐ－Ｒ间期范围在此０。０７５－０．１４０Ｓｅｃ。在９个导联中，无明显Ｓ－Ｐ段偏移。Ｐ－Ｐ间隔＜０．０１Ｓｅｃ。     

Automated headspace solid‐phase microextraction and on‐fiber derivatization for the determination of clenbuterol in meat products by gas chromatography coupled to mass spectrometry

A method was developed for the determination of clenbuterol in meat using stable‐isotope‐dilution gas chromatography with mass spectrometry coupled with solid‐phase microextraction and on‐fiber derivatization. The samples were first homogenized with hydrochloric acid followed by protein deposition. After headspace solid‐phase microextraction and on‐fiber derivatization, the content of clenbuterol was measured with the aid of stable‐isotope dilution. The condition of solid‐phase microextraction was optimized by central composite design. The relative standard deviations, limit of detection, and recoveries for clenbuterol were 4.2–9.2%, 0.48 μg/kg, and 96–104%, respectively. The proposed method was satisfactory for analysis of real samples as compared with the Chinese standard method.     

猪肉中二甲胺四环素的反相-高效液相色谱测定

建立了一种测定猪肉中二甲胺四环素的反相-高效液相色谱(RP-HPLC)分析方法.目标物经EDTA-Mcllvaine提取,用Oasis HLB固相萃取小柱净化,流动相为甲醇-咪唑缓冲溶液,体积比20:80,荧光检测器检测,外标法定量.平均添加回收率在89.6％～94.0％之间,相对标准偏差(RSD)在3.1％～6.5％...     

Analyses of sulfonamide antibiotics in meat samples by on-line concentration capillary electrochromatography-mass spectrometry

In this work, a series of poly(divinylbenzene-alkyl methacrylate) monolithic stationary phases, which were prepared by single step in situ polymerization of divinylbenzene and various alkyl methacrylates (butyl-, octyl-, lauryl- or stearyl methacrylate), were developed as separation columns of nine common sulfonamide antibiotics for capillary electrochromatography (CEC) coupled to mass spectrometry (MS). Results indicated that the sulfonamide's retention became weak with increased carbon chain length of alkyl methacrylate monomer (for example, t(R)=68 min and 21 min for butyl- and lauryl methacrylate, respectively). Among them, the poly(divinylbenzene-octyl methacrylate) (poly(DVB-OMA)) monolith was regarded as the optimal separation column as this provided better resolution within the shortest retention time. Moreover, the cross-sectional roughness of the monolithic column-end, that was used to couple to the ESI interface, strongly influenced the electrospray stability in the CEC-MS. Before the column was connected to the ESI-MS, a simple polishing was done to reduce the roughness of the column end that resulted to a great improvement in the signal stability. The relative standard deviations (RSDs) of the peak areas for the unpolished and polished ends of the poly(DVB-OMA) columns (n=5) were in the range of 46.1-60.2% and 8.9-16.4%, respectively. Furthermore, optimization of the mobile phase composition and the gradient elution strategy successfully determined the sulfonamide antibiotics in meat samples with as low as 10 μg/L level.     

Determination of volatile nitrosamines in meat products by microwave-assisted extraction and dispersive liquid-liquid microextraction coupled to gas chromatography-mass spectrometry

Microwave-assisted extraction (MAE) and dispersive liquid-liquid microextraction (DLLME) coupled with gas chromatography-mass spectrometry (GC-MS) were evaluated for use in the extraction and preconcentration of volatile nitrosamines in meat products. Parameters affecting MAE, such as the extraction solvent used, and DLLME, including the nature and volume of the extracting and disperser solvents, extraction time, salt addition and centrifugation time, were optimized. In the MAE method, 0.25g of sample mass was extracted in 10mL NaOH (0.05M) in a closed-vessel system. For DLLME, 1.5mL of methanol (disperser solvent) containing 20μL of carbon tetrachloride (extraction solvent) was rapidly injected by syringe into 5mL of the sample extract solution (previously adjusted to pH 6), thereby forming a cloudy solution. Phase separation was performed by centrifugation, and a volume of 3μL of the sedimented phase was analyzed by GC-MS. The enrichment factors provided by DLLME varied from 220 to 342 for N-nitrosodiethylamine and N-nitrosopiperidine, respectively. The matrix effect was evaluated for different samples, and it was concluded that sample quantification can be carried out by aqueous calibration. Under the optimized conditions, detection limits ranged from 0.003 to 0.014ngmL(-1) for NPIP and NMEA, respectively (0.12-0.56ngg(-1) in the meat products).     

导盲犬和淘汰犬肠道菌群的差异性研究

目的 探究导盲犬和淘汰犬之间肠道菌群的差异,分析两者特征性差异菌群。方法 收集16只导盲犬和10只淘汰犬的新鲜粪便样本,按照犬品种和性别分为拉布拉多雄性导盲犬(GD-ML)和淘汰犬(ED-ML)、拉布拉多雌性导盲犬(GD-FL)和淘汰犬(ED-FL)、金毛雄性导盲犬(GD-MG)和淘汰犬(ED-MG),另外从中随机抽取9只导盲犬和4只淘汰犬分为导盲犬组(GD)和淘汰犬组(ED),共分为4组配对。提取粪便样本总DNA,应用PCR-DGGE技术获得肠道菌群图谱,应用相关软件和统计学方法对每组配对进行差异性分析。结果 聚类分析结果显示,GD和ED,GD-ML和ED-ML,GD-FL、ED-FL和GD-MG均各归为一类,表明导盲犬和淘汰犬之间肠道菌群存在差异。肠道菌群多样性、丰富度和均匀度分析结果显示,每两个配对组之间多样性指数、丰富度指数和均匀度指数存在差异,但差异均无统计学意义。差异性条带测序分析结果显示：与ED相比,GD Megamonas funiformis YIT 11815菌株增多;与ED-ML相比,GD-ML Succinatimonas hippei YIT 12066、Lactobacillus vaginalis DSM 5837、Lactobacillus acidophilus NCFM、Faecalibacterium prausnitzii A2-165菌株增多,Collinsella aerofaciens ATCC 25986和Prevotella copri DSM 18205菌株减少;与ED-FL相比,GD-FL Ruminococcus gnavus AGR2154、Fusobacterium russii ATCC 25533菌株减少;与ED-MG相比,GD-MG Tropheryma whipplei str. Twist菌株增多。结论 本研究发现导盲犬和淘汰犬肠道菌群存在差异,未来对差异菌群的进一步研究可能有助于辅助导盲犬的早期筛选。     

同时测定肉制品中氯化物、亚硝酸盐、硝酸盐

本文应用离子色谱仪,兔肉脯为基质,建立了同时测定肉及肉制品中氯化物、亚硝酸盐和硝酸盐的分析方法.样品绞碎后纯水起声提取,提取液过c18柱除去有机杂质,经0.45μm过滤器直接进行测定.方法操作简单,重现性好,各组分加标回收率为：C1,103.0％; NO2-N,98.0％;NO,-N,94.2％.RSD在0.4％～1.3％（n=6）.方法检出限分别为：C1,0.01 mg/L; NO2-N,0.005 mg/L; NO3-N,0.02 mg/L.