Portable surface plasmon resonance immunosensor for the detection of fluoroquinolone antibiotic residues in milk

An inexpensive and portable surface plasmon resonance (SPR) sensor, SPReeta Evaluation Kit SPR3, has been used to develop a biosensor for the determination of fluoroquinolone antibiotics (FQs) and to demonstrate its performance analyzing FQ residues in milk samples. The SPReeta three-channel gold chips were activated with a mixed self-assembled monolayer (m-SAM) and functionalized with a FQ haptenized protein. Binding of the antibody produced a concentration-dependent increase of the SPR signal as a result of the change in the refraction index. Similarly, the presence of the FQ produced a dose-dependent decrease of the response, which allowed a good limit of detection (LOD) to be obtained (1.0 ± 0.4 μg L(-1) for enrofloxacin in buffer). The response was reproducible in all three channels, on different injections and days, and also between chips. Milk samples could be analyzed after a simple sample treatment involving fat removal by centrifugation and dilution with water. Under these conditions calibration curves were obtained showing that FQ residues can be analyzed in milk samples with an IC(50) value of 26.4 ± 7.2 μg L(-1) and a LOD of 2.0 ± 0.2 μg L(-1) (for enrofloxacin), far below the European Union regulations for this antibiotic family in this matrix. Finally, the paper also demonstrates that the biosensor is able to selectively detect the presence of FQs in milk samples, even in the presence of other antibiotics. Enrofloxacin, ciprofloxacin, and norfloxacin residues were detected in blind samples supplied by Nestle? Co.     

Marine fish as source of protein supplement in meat

For the past 2 decades, a great deal of research has been done in fish technology, particularly in the area of mechanically deboned minced fish. Minced fish is the edible muscle flesh of fish that has been mechanically separated from the bones and skin. Ideally, the product is prepared from a high quality fish and resembles hamburger meat. In its final form, minced fish is used either as an ingredient or as an extender in seafood or in food products that require further processing. On the basis of technological advancements, the National Marine Fisheries Service of the U.S. Department of Commerce and the National Fisheries Institute jointly petitioned the U.S. Department of Agriculture in 1980 to add minced fish at a level of 15% in the meat formulation of frankfurters. This paper explores certain aspects of processing, production, acceptance, and hazard assessment of minced fish ingredients as possible protein supplements in meat and poultry food products relative to this request.     

Effect of plant phenolics on protein and lipid oxidation in cooked pork meat patties

Rapeseed and pine bark are rich sources of phenolic compounds that have in previous studies been shown to exhibit antioxidant and anti-inflammatory properties. In this study, the antioxidant effect of rapeseed and pine bark phenolics in inhibiting the oxidation of lipids and proteins in meat was tested as a possible functional food application. The cooked pork meat with added plant material was oxidized for 9 days at 5 degrees C under light. The suitable level of plant material addition was first screened by following lipid oxidation only. For further investigations plant materials were added at a level preventing lipid oxidation by >80%. The oxidation was followed by measuring the formation of hexanal by headspace gas chromatography and the formation of protein carbonyls by converting them to 2,4-dinitrophenylhydrazones and measured by spectrophotometer. It was shown that rapeseed and pine bark were excellent antioxidants toward protein oxidation (inhibitions between 42 and 64%). These results indicate that rapeseed and pine bark could be potential sources of antioxidants in meat products.     

Spectrofluorometric determination of histamine in fish and meat products

A method has been developed for spectrofluorometric determination of histamine in fish and meat products. After a perchloric extract is obtained from samples, histamine is extracted with n-butanol and transferred to hydrochloric acid. Finally, histamine is subjected to a condensation reaction with o-phthalaldehyde (OPT). The method was tested for lack of interference from other amines. Precision of the method in fish products was 6.60% CV; recovery was 96.50%. In meat products, precision was 5.42% CV; recovery was 96.20%. By analysis of variance (P = 0.05), no significant statistical differences were found for recovery values vs histamine content in both foods.     

Identification of O,O-dialkyl-S-methylphosphorodithioate residues in fish

O,O-Dialkyl-S-methylphosphorodithioates were found in Mississippi River buffalo fish caught near several chemical plants and oil refineries in Hartford and Wood River, IL. These chemicals, which have not been previously recognized as environmental or food contaminants, were identified and quantitated by a procedure similar to the AOAC multiresidue method for organochlorine and organophosphorus pesticides, using gas chromatography (GC) with flame photometric detection (FPD). The key to their identification was a GC/FPD retention time pattern that was virtually the same as that for the diazomethane reaction products of a commercial zinc dialkyl dithiophosphate motor oil additive. GC/mass spectrometry (MS) showed that the compound producing the largest GC/FPD peak contained butoxy groups. The identification of this compound as O,O-di(2-methylpropyl)-S-methyl-phosphorodithioate (Compound C) was confirmed by GC/MS analysis by comparison with the authentic material. The buffalo fish contained 0.15 ppm Compound C and 0.5 ppm total O,O-dialkyl-S-methylphosphorodithioates. Subsequent analyses of fish from other areas showed that these contaminants were not limited to the Hartford-Wood River area. Lower residue levels of Compound C, ranging from 0.01 to 0.05 ppm, were found in fish from the Mississippi River at Sauget, IL, and from the Delaware River and Newark Bay in NJ.     

Liquid chromatographic determination of chloramphenicol residues in meat: interlaboratory study

A liquid chromatographic (LC) method for the determination of chloramphenicol (CAP) residues in meat at the 10 microgram/kg level was tested in an interlaboratory study. The method used, based on aqueous extraction and sample cleanup with a cartridge containing Extrelut, was published earlier. A prestudy to familiarize collaborators with the method was performed before the actual interlaboratory precision study. The meat samples used in the precision study were prepared by diluting dosed chicken and pig muscle tissues with blank tissues from other species. Fourteen laboratories received 20 meat samples; 13 laboratories actually participated in the study. Two blank samples and 2 positive samples each of pig, calf, chicken, lamb, and cow meat were tested. The chloramphenicol concentrations in the positive samples ranged from 6.5 to 21 micrograms/kg. The overall mean reproducibility coefficient of variation was 17.9% after the results per laboratory were corrected for the mean recovery obtained within each sample series. The overall mean recovery was 55.1% with a coefficient of variation of 18.0% at the 10 micrograms/kg level. The limit of detection, based on chromatograms of blank samples, was estimated to be 1.5 micrograms/kg of chloramphenicol. No false positives or false negatives were observed in the concentration range tested; only 2 false positive results above the detection limit (1.7 and 6 micrograms/kg) on a total number of 60 blank analyses (3.3%) were observed.     

Effect of proteolytic squid protein hydrolysate on the state of water and dehydration-induced denaturation of lizard fish myofibrillar protein

With the goal of preparing low-cost functional food, squid protein hydrolysate (SPH) was extracted from four squid species by protease treatment. Peptides are the major components (approximately 84-88%) of the SPH. The stabilization effects of 5% SPH (dried weight/wet weight) on the state of water and the denaturation of frozen lizard fish Saurida wanieso myofibrillar protein (Mf) were evaluated on the basis of desorption isotherm curves with respect to Ca2+-ATPase inactivation and the presence of unfrozen water, which was determined using differential scanning calorimetry during dehydration, and the effects were compared with those of sodium glutamate. The Mf with SPH was found to contain higher levels of monolayer and multilayer sorption water, resulting in decreased water activity and Ca2+-ATPase inactivation. The amount of unfrozen water in Mf with SPH increased significantly, suggesting that the peptides of SPH stabilized water molecules on the hydration sphere of Mf, which maintained the structural stability of Mf, and therefore suppressed dehydration-induced denaturation. The effect by SPH was less than that by sodium glutamate.     

基于鱼体特征点检测的淡水鱼种类识别

针对传统机器视觉技术对淡水鱼种类进行检测时特征提取过程复杂的问题,该研究提出了基于特征点检测的淡水鱼种类识别方法。以鳊、鳙、草鱼、鲢、鲤5种大宗淡水鱼为对象,构建了淡水鱼特征点检测数据集;以AlexNet模型为基础,通过减小卷积核尺寸、去除局部响应归一化、引入批量归一化、更换损失函数,构建了改进AlexNet模型用于特征点检测;并以特征点为依据提取特征值、构造特征向量,使用Fisher判别分析方法实现了淡水鱼的种类识别。试验结果表明：改进AlexNet模型在测试集上的归一化平均误差的均值为0.0099,阈值δ为0.02和0.03时的失败率F_0.02、F_0.03分别为2.50%和0.83%,具有较好的精准度和误差分布情况;基于该模型和Fisher判别分析的淡水鱼种类识别方法对5种淡水鱼的识别准确率为98.0%,单幅图像的平均识别时间为0.368 s,保证了时效性。由此可知,提出的改进AlexNet模型能实现淡水鱼的特征点检测并具有较高的精度,可为淡水鱼种类识别、尺寸检测、鱼体分割等提供条件,该方法可为淡水鱼自动化分类装置的研发奠定基础。     

Determination of ampicillin residues in fish tissues by liquid chromatography

A liquid chromatographic (LC) method is described for determination of ampicillin residues in fish tissues. The drug is extracted from tissues with methanol, and the extract is evaporated to dryness. This residue is cleaned up by Florisil cartridge chromatography. LC analysis is carried out on a Nucleosil C18 column, and ampicillin is quantitated by ultraviolet detection at 222 nm. Recoveries of ampicillin added to tissues at levels of 0.2 and 0.1 ppm were 73.2 and 61.5%, respectively. The detection limit was 3 ng for ampicillin standard, and 0.03 ppm in tissues.     

Determination of nitrogen and protein content of meat and meat products

Chemical and instrumental methods for determination of nitrogen and protein are reviewed for their mode of action and utility in analysis of meat proteins and products. Although the Kjeldahl digestion method is satisfactory for determining total nitrogen, it is imprecise for determining total protein content. Presence of variable amounts of nonprotein nitrogenous components and of connective tissue proteins such as collagen and elastin produces error if the formula (N X 6.25) is used to calculate crude protein. Such fibrous proteins have higher nitrogen levels (over 18%) than other muscle proteins (about 16%), and a higher than actual protein value will be determined unless a lower conversion factor is used to correct for their content. To determine meat protein content more accurately, a combination of Kjeldahl determination with one or more additional tests to correct for nonprotein and fibrous protein content is recommended. The choice of the additional method(s) is based on the user's requirement for protein characterization, available time, type of meat product, and sample size.     

基于高光谱成像的肉品检测去条带噪声方法

推扫式高光谱成像系统通常因电荷耦合器件（Charge Coupled Device,CCD）各像元响应不一致而产生条带噪声,该研究以猪肉为研究对象,设计一种基于多块标准反射率板进行逐波段逐像素相对辐射定标的去除条带噪声方法。该方法基于最小二乘法,利用不同反射率标准板的反射率值与CCD输出值,采用多项式拟合出接近于各个波段逐像元真实响应函数的拟合响应函数;选取每一波段图像中的任一像元作为参考,将其余像元与参考像元的拟合响应函数做差,作为其余像元的补偿函数,再采用样本的输出值加补偿值以校正样本。分别采用逐波段逐像素相对辐射定标法和传统矩匹配法对猪肉高光谱图像进行处理,并以四阶标准反射率板各反射区均值与参考值的绝对误差评估反射率校正结果。结果表明,逐波段逐像素相对辐射定法在有效去除条带噪声的同时,不会产生新的噪声,同时能够保持原始图像的灰度分布,校正后图像条带系数最大值比原始图像减少63.5%;相比矩匹配法,反射率误差大幅下降,其中条带系数最大波段（200波段）4个反射区的绝对误差为0.003～0.089,随机抽取波段（300波段）4个反射区的绝对误差为0.009～0.083。该研究为消除条带噪声提供了一种可靠方法,同时为提高后续基于推扫式光谱成像的指标空间可视化精度奠定了良好的基础。     

Effects of cooking on concentrations of polychlorinated dibenzo-p-dioxins and related compounds in fish and meat

We investigated the cooking-induced changes in concentrations of polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs), and dioxin-like polychlorinated biphenyls (PCBs) (dioxins) using mackerel and beef. The concentrations of dioxins (29 congeners) were determined by isomer specific analyses and were compared between uncooked and cooked samples. The cooking procedures examined in this study included grilling as a fillet, boiling as a fillet, and boiling as tsumire (small, hand-rolled balls) for mackerel and boiling as a slice, broiling as a slice, and broiling as a hamburger for beef. Three trials were carried out for each cooking method. Generally, concentrations of dioxins were reduced in every cooking trial. When nondetected congener concentrations were assumed to be half the limit of detection for mackerel, the maximum percentage reductions of total concentrations given as 2,3,7,8-tetraCDD equivalents (TEQ) were 31% in grilling as a slice, 14% in boiling as a slice, and 21% in boiling as tsumire under the conditions of this study. In contrast, for beef, the reductions were 42% in boiling as a slice, 42% in broiling as a slice, and 44% in broiling as a hamburger. These results suggest that ordinary cooking processes with heating undoubtedly reduce the dioxin content in animal products, and the reductions estimated should be considered when dioxin intake is evaluated using contamination data for individual food items.     

牛奶抗生素残留快速检测技术进展及应用现状

综述了商品化牛奶中抗生素残留的快速检测方法和试剂盒。主要的检测方法有微生物抑制法和酶联免疫法。微生物抑制法的主要试剂盒有DELVOTEST、CHARM SCIENCE、BRILLIANT BLACK REDUCTION等;以免疫法为基础的主要有β-LACTAMS、DEVLX-PRESS、BETA SCREEN、CHARMⅡASSAY、β-STAR、CHARM-MRL、PENZYM、PARALLUX等。文章列出了这些方法的检测极限,对一些新的检测方法和方向进行了讨论,同时提出了牛奶抗生素残留快速筛选方法的问题和今后的发展方向。     

Survey of residues of organochlorine pesticides in some marketable Egyptian fish

One hundred random samples representing 34 species of marketable fish were collected from 8 Egyptian governorates during the period March 1986 to March 1988 and were analyzed for the presence of some organochlorine pesticides. The results showed the predominance of beta-BHC and lindane at maximum levels of 435.30 and 59.00 micrograms/kg, respectively, for fish samples obtained from Damietta governorate. The corresponding levels of aldrin, and o,p'-DDT were 34.27 and 734.10 micrograms/kg, respectively, for fish from the Red Sea governorate. gamma-Chlordane, p,p'-DDE, and p,p'-DDT were found in fish from Ismailia governorate at respective maximum levels of 36.17, 234.40, and 57.19 microgram/kg. Heptachlor was identified at 8.50 micrograms/kg in Port Said governorate fish and o,p'-DDE at 10.59 micrograms/kg in Suez governorate fish. Mirex, on the other hand, could not be detected in any of the samples investigated.     

干燥方法对即食扇贝柱品质的影响

为深入了解不同干燥方法对即食扇贝柱干燥后品质的影响,以海湾扇贝柱为原料,研究了微波干燥、真空冷冻干燥、自然干燥和烘箱干燥四种方法对即食扇贝柱理化特性和感官品质的影响。结果表明：不同干燥方法所得产品在水分活度、pH值、硬度、咀嚼性和粘聚性方面存在着显著性差异,不同干燥方法对产品的色泽（L*,a*,b*）和弹性影响均不显著;烘箱干燥产品感官品评得分8.82分,其氨基酸总量最高,微波干燥氨基酸总量最低;真空冷冻干燥后产品中必需氨基酸和呈味氨基酸含量最高,自然干燥最低。综合考虑,烘箱干燥是即食扇贝柱最适宜的干燥方法,产品感官品质较高。