顶空气相色谱法快速测定肉及肉制品中乙烯利的残留量

利用乙烯利在碱性水溶液中受热能够快速分解成乙烯的特性,建立了顶空气相色谱法快速测定乙烯利在肉及肉制品中残留量的方法。在样品中添加碱液后恒温加热,吸取顶空瓶中的上层气体,采用石英毛细管色谱柱分离,氢火焰离子化检测器测定。该方法的检测限为0.01mg/kg,回收率为90.9%～96.0%,相对标准偏差为3.5%～8.5%。适用于猪肉、牛肉、鸡肉等肉及肉制品中乙烯利残留量的检测。     

高效液相色谱法同时测定肉制品中的6种食品添加剂

建立了同时测定肉制品中化学性质差异较大的6种常用食品添加剂的高效液相色谱(HPLC)分析方法。根据6种添加剂(苯甲酸(钠)、山梨酸(钾)、糖精钠、安赛蜜、诱惑红和胭脂红)的化学性质,对HPLC分析条件进行了详细的优化。结果表明:以ZORBAX Eclipse Plus C18柱(150mm×4.6mm,5μm)为分析柱,以甲醇和20mmol/L醋酸铵溶液(pH为6.9)为流动相进行梯度洗脱,在235nm波长下进行检测,可以在18min内完成6种添加剂的同时测定。在高、低两个加标浓度下,样品的回收率为80.7%～94.4%,相对标准偏差(n=3)为2.0%～7.1%。结果表明,该方法快速、准确,能够同时分析测定肉制品中上述6种食品添加剂。     

液相色谱-串联质谱法测定肉及肉制品中利谷隆及其代谢产物3,4-二氯苯胺残留

建立了液相色谱-串联质谱分析多种肉及肉制品中利谷隆及其代谢产物3,4-二氯苯胺残留的方法。样品用丙酮-乙腈(5:95, v/v)提取,冷冻去脂,经弗罗里硅土固相萃取柱净化后进行液相色谱-串联质谱检测,采用内标法定量。利谷隆及3,4-二氯苯胺在1～500 μg/L范围内呈良好的线性关系,相关系数(r)均大于0.998,方法的定量限(信噪比(S/N)＞10)为10 μg/kg,检出限(S/N＞3)为5 μg/kg。在各种肉及肉制品基质中添加低、中、高3种不同水平的利谷隆及3,4-二氯苯胺,其回收率范围分别为88.3%～101.2%和91.6%～101.6%,相对标准偏差(RSD)分别为4.8%～13.7%和4.7%～11.8%。结果表明所建立的方法可以满足肉及肉制品中利谷隆和3,4-二氯苯胺残留量的检测需要。     

LC/MS/MS analysis of α‐tocopherol and coenzyme Q10 content in lyophilized royal jelly,beebread and drone homogenate

This study shows the results of application liquid chromatography‐tandem mass spectrometry (LC/MS/MS) for assay of the content of α‐tocopherol and coenzyme Q₁₀ in bee products of animal origin, i.e. royal jelly, beebread and drone homogenate. The biological matrix was removed using extraction with n‐hexane. It was found that drone homogenate is a rich source of coenzyme Q₁₀. It contains only 8 ± 1 µg/g of α‐tocopherol and 20 ± 2 µg/g of coenzyme Q₁₀. The contents of assayed compounds in royal jelly were 16 ± 3 and 8 ± 0.2 µg/g of α‐tocopherol and coenzyme Q₁₀, respectively. Beebread appeared to be the richest of α‐tocopherol. Its level was 80 ± 30 µg/g, while the level of coenzyme Q₁₀ was only 11.5 ± 0.3 µg/g. Copyright © 2016 John Wiley & Sons, Ltd.     

Centurion — a revolutionary irradiator

The facility characteristics for irradiation of red meat and poultry differ significantly from those of medical disposables. This paper presents the results of the market requirement definition which resulted in an innovative conceptual design. The process and the “state of the art tools” used to bring this abstract idea into a proof of concept are presented.     

Optimization and validation of high-performance liquid chromatography using modified QuEChERS to determine anthelmintic drugs in mutton

The aim of this study was to rapidly determine the presence of anthelmintic drugs in sheep meat using the optimized high-performance liquid chromatography-ultraviolet (HPLC-UV) method with modified QuEChERS (quick, easy, cheap, effective, rugged, safe) technology. Fifty fresh sheep meat samples from different slaughterhouses were collected. A double extraction procedure (QuEChERS/HPLC-UV technology) was used to extract the target analytes. A multilevel calibration curve from 1 to 1000 g/kg was used to establish instrument linearity for rafoxanide, albendazole, and closantel, whereas 0.1–100 μg/kg was used for ivermectin, levamisole, and oxyclozanide to find the lowest concentration, maximum residue limit (MRL), and occupied range for targeted analytes. The concentration levels were used to investigate the linearity, whereas several certified reference materials were applied to determine accuracy. The process was linear for all combinations, from the limit of quantification (LOQ) to the maximum concentration. The LOQ was established at 0.5 μg/kg for ivermectin, levamisole, and oxyclozanide and 10 μg/kg for rafoxanide, albendazole, and closantel. Recovery values were 70%–120%, and repeatability/reproducibility stated in relative standard deviation was obtained at less than 20%. QuEChERS method revealed that most meat samples contained anthelmintic drug residues, of which the majority exceeded the MRLs. Thus, the drugs should be used correctly in animals to avoid residues in food for human consumption.     

Effect of Traditional Cooking and Sous Vide Heat Treatment,Cold Storage Time and Muscle on Physicochemical and Sensory Properties of Beef Meat

Consumers are avoiding the consumption of highly processed foods, aware of the negative effects of the additives or high temperatures used on the biological value of the food. This causes an interest in ways of minimal processing or low-temperature cooking procedures. However, to achieve the desired organoleptic quality, it is necessary to know the relationship between the parameters of the treatments and the type of raw material. The purpose of this study was to investigate the complex effects of traditional cooking and sous vide heat treatment, cold storage time and muscle on the physicochemical and sensory properties of beef. The study material consisted of samples of musculus longissimus thoracis and musculus semitendinosus obtained from beef half-carcasses. The muscles were subjected to traditional cooking in water at 95 °C until the temperature inside the piece reached 65 °C and sous vide treatment at 65 °C for 2 h. The study was performed after 2 and 21 days of cold storage. Instrumental evaluation of texture parameters, color and sensory evaluation of meat was carried out. Meat stored for 21 days was characterized by more favorable TPA test (Texture Profile Analysis) results compared to meat evaluated 48 h post mortem. The study also showed positive effects of sous vide heat treatment on texture parameters and sensory properties (especially on tenderness and palatability), as well as differences in the formation of quality traits between muscles. Given the trends associated with energy-saving technologies, it is desirable to seek the optimal combination of temperature and time of fixation treatments at an acceptable level of quality. The use of low-temperature cooking for as little as 2 h, yields positive results in sensory evaluation of juiciness, tenderness, or palatability.     

Rapid detection of doxycycline content in duck meat by using silver nanoparticles and alkylphenols polyoxyethylene enhanced fluorescence of europium complex

Doxycycline can coordinate with europium (III) to form europium (III)-doxycycline complex, which can emit the fluorescence characteristic peak of europium (III) at 617 nm in alkaline solution, and the experiment proved that the fluorescence intensity could be further enhanced in the presence of silver nanoparticles and surfactant alkylphenols polyoxyethylene. So this method was applied to detect doxycycline content in duck meat in this research. First, 390 and 617 nm were selected as the optimum excitation wavelength and optimum emission wavelength by three-dimensional fluorescence spectrometry, respectively. Second, the experimental conditions were optimized through single factor experiment. Lastly, the samples of doxycycline concentration range of 0.05–12 mg/L were analyzed under the optimum experimental conditions. A good linear relationship between the doxycycline concentration and the fluorescence intensity was obtained, and the determination coefficient and the root mean squared error of prediction were 0.9982 and 0.4363 mg/L, respectively. This research showed that it was feasible to achieve the rapid detection of doxycycline content in duck meat by using silver nanoparticles and alkylphenols polyoxyethylene enhanced the fluorescence of europium complex.     

基于光谱技术的原料肉新鲜度指标在线检测系统开发及试验

为了实现原料肉新鲜度参数的无损在线实时评估,基于双波段可见/近红外反射光谱（350~1 100和1 000~2 500 nm）技术建立了原料肉新鲜度主要指标的在线检测系统。研究设计了装置的光源单元、光谱采集单元、控制单元和驱动单元,优化设计了光源固定支架和安放角度,编写了相应的控制程序,开发了实验室用和便于在不同生产线应用的两套在线检测系统。首先,对试验参数（传送带速度和样品到透镜入光口距离）进行了优化研究,通过光谱相似度比较和显著性分析,确定传送带速度是275 mm·s-1、距离是12 cm时能够获得更加稳定的光谱信号。然后,基于该试验参数,分别在静止和在线条件下采集了贮藏时间为1~13 d共50个猪肉样本的反射光谱,并利用抛物线拟合法对双波段光谱进行融合,以获取整条覆盖可见及近红外区域的完整光谱。为了使两个波段范围内的光谱数据点权重相同,在整个波段范围内均匀分布,借助三次样条插值法将所有光谱数据点以2 nm为间隔进行重新排布。采用窗口移动多项式最小二乘拟合法对光谱作平滑处理,采用标准正态变量变换对每条光谱进行标准化预处理,分别建立了静止和在线条件下新鲜度主要表征指标-颜色（L*,a*和b*）、pH和挥发性盐基氮的预测模型,以此验证所搭建系统的可靠性。经过对比分析,发现在线条件下的建模结果不如静止状态下的建模结果,这可能与在线采集时光谱存在漂移现象有关。进一步尝试利用一阶导数处理来消除基线漂移强化谱带特征,并对一阶导数和标准化处理顺序对建模结果的影响进行了探讨。结果发现先经过一阶导数再经过标准化处理,能更好地消除外部干扰造成的影响,建模结果更佳。在该处理方式下,基于第一波段光谱建立了颜色参数（L*,a*,b*）的预测模型,基于双波段光谱建立了pH和挥发性盐基氮的在线检测模型,预测相关系数分别为0.955 3,0.924 7,0.955 1,0.961 5和0.966 8。最后,为了验证模型的适用性,基于开发的便于在不同生产线应用的在线检测系统,利用独立的20个样本对在线模型进行外部验证,对颜色参数（L*,a*,b*）,pH和挥发性盐基氮的预测相关系数分别为0.918 9,0.914 1,0.947 7,0.950 4和0.960 6。研究结果表明,该系统通过双波段光谱的实时采集和融合,可以获取更多反应样本内部信息的光学信号,具有更强的检测能力。结合设计的光路等其他硬件单元,可以同时获取样本表面更大区域的反射光谱信息,从而实现对原料肉新鲜度主要表征参数的无损、在线、实时评估。该系统便于组装和拆卸,可以适应不同企业生产线的实际需要,具有较强的实用价值和较好的市场前景。     

Mechanistic aspects of electrochemical hydride generation for cadmium

A reversed-phase chromatographic method has been developed and optimised in order to detect and quantitate soybean proteins in commercial heat-processed meat products. The optimised conditions consisted of a linear binary gradient tetrahydrofurane-water-0.05% trifluoroacetic acid at a flow rate of 1 mL/min. Meat products were defatted with acetone and soybean proteins were extracted with a buffered solution at pH 9.60. The injection of this extract into the chromatographic system enabled the detection of soybean proteins in heat-processed meat products in about 12 min. The method enabled the detection and quantitation of additions of 0.38% (w/w) and 0.63% (w/w), respectively, of soybean proteins (related to 10 g of initial product). The method has been proven to be precise with relative standard deviations (R.S.D.) for repeatability, intermediate precision, and internal reproducibility lower to 7.0%. Recoveries obtained for spiked meat products were close to 100% and no matrix interferences were observed. The application of the method to commercial heat-processed meat products in whose formulation soybean proteins were present yielded soybean protein contents ranging from 0.90% to 1.54%, below the maximum levels established by regulations.