顺序注射HG-AFS法测定富硒农产品中无机硒和有机硒

本文建立了顺序注射氢化物发生原子荧光法测定硒的分析方法.探讨了富硒农产品中无机硒和有机硒的分离及提取方法.优化了仪器的工作条件,考察了KBH4浓度和酸介质浓度对硒原子荧光强度的影响.方法的线性范围为1～100μg/L,检出限为0.02μg/L,无机硒的回收率为95.0%～104.0%.     

An optimized digestion method coupled to electrochemical sensor for the determination of Cd, Cu, Pb and Hg in fish by square wave anodic stripping voltammetry

An optimized digestion method coupled to electrochemical detection to monitor lead, copper, cadmium and mercury in fish tissues was developed. Square wave anodic stripping voltammetry (SWASV) coupled to disposable screen-printed electrodes (SPEs) was employed as fast and sensitive electroanalytical method for heavy metals detection. Different approaches in digestion protocols were assessed. The study was focused on Atlantic hake fillets because of their wide diffusion in the human nutrition. Best results were obtained by digesting fish tissue with hydrogen peroxide/hydrochloric acid mixture coupled to solid phase (SP) purification of the digested material. This combined treatment allowed quantitative extraction from fish tissue (muscle) of the target analytes, with fast execution times, high sensitivity and avoiding organic residues eventually affecting electrochemical measurements. Finally, the method has been validated with reference standard materials such as dogfish muscle (DORM-2) and mussel tissues (NIST 2977).     

Simultaneous residue monitoring of four tetracycline antibiotics in fish muscle by in-tube solid-phase microextraction coupled with high-performance liquid chromatography

An on-line simple and rapid method for the simultaneous determination of tetracycline (TC), oxytetracycline (OTC), chlortetracycline (CTC) and doxycycline (DC) residues in fish muscle was developed by coupling in-tube solid-phase microextraction (SPME) to high-performance liquid chromatography (HPLC) with a photodiode array detector. Biocompatible poly (methacrylic acid-ethylene glycol dimethacrylate) monolithic capillary was selected as the extraction medium, and no precipitating protein and removing fat steps were required prior to extraction. In order to optimize the extraction of these compounds, several in-tube SPME parameters were investigated. Simply performed by extracting with 0.01 M EDTA-MacIlvaine buffer solution (pH 4.0) and centrifugation, the sample then could be directly injected into the device for extraction. The limits of detection of tetracycline, oxytetracycline, chlortetracycline and doxycycline were calculated to be 22, 16, 30 and 21 ng/g, respectively. The calibration curves showed linearity in the range of 100-10,000 ng/g with a linear coefficient R² value above 0.9980. Excellent method reproducibility was found by intra- and inter-day precisions, yielding the R.S.D.s less than 4.22% and 5.71%, respectively.     

可见-近红外光谱分析技术对鱼油掺假定量快速无损检测方法研究

对掺入不同含量大豆油和菜籽油的鱼油进行鱼油掺假含量的可见-近红外光谱(Vis-NIR)研究。向3个不同品牌鱼油中分别掺入不同比例的大豆油,另外3个不同品牌中分别掺入不同比例的菜籽油,共获得300个样本。对所采集样本的光谱数据分别采用原始光谱,以及平滑,变量标准化(SNV),多元散射校正(MSC),一阶求导和二阶求导等预处理算法进行处理后,建立偏最小二乘回归(PLSR)模型。基于全波段光谱的鱼油中大豆油和菜籽油掺假含量预测的最优模型分别为全波段PLSR模型和MSC-PLSR模型,其预测相关系数(R_p)分别达到0.938 6和0.959 3。进一步采用连续投影算法(SPA)分析鱼油中大豆油和菜籽油掺假样品的光谱,并分别获得了11个和15个光谱特征波长变量。基于特征变量的PLSR模型的R_p分别为0.941 2和0.932 6。试验研究表明, 可以采用Vis-NIR技术实现对鱼油掺假物含量的检测。     

Effect of high pressure processing on the preservation of frozen and re-thawed sliced cod (Gadus morhua) and salmon (Salmo salar) fillets

Cod and salmon are both widely found in the seafood market, but those products are easily spoiled. This work reports on the investigation of the effects of three moderate pressure values (150, 300 and 450?MPa) applied for 5?min at 20°C on crude sliced cod and salmon fillets. It was found that high pressure processing (HPP) significantly reduced the microbial load during refrigerated storage for up to 14 days. As expected, the most effective treatment was 450?MPa because it inhibited microbial growth. This process affected the hardness, lightness, lipid oxidation, protein denaturation and oxidation. The fish muscle composition (lipid amount and protein profile) played a main role in the changes promoted by pressure. HPP permits the shelf life of the raw product at 4°C to be increased with minimal changes in the organoleptic characteristics and to enable crude consumption.     

Molecularly-Imprinted Materials for Potentiometric Transduction: Application to the Antibiotic Enrofloxacin

Enrofloxacin (ENR) is an antimicrobial used both in humans and in food producing species. Its control is required in farmed species and their surroundings in order to reduce the prevalence of antibiotic resistant bacteria. Thus, a new biomimetic sensor enrofloxacin is presented. An artificial host was imprinted in specific polymers. These were dispersed in 2-nitrophenyloctyl ether and entrapped in a poly(vinyl chloride) matrix. The potentiometric sensors exhibited a near-Nernstian response. Slopes expressing mV/Δlog([ENR]/M) varied within 48–63. The detection limits ranged from 0.28 to 1.01 µg mL^?1. Sensors were independent from the pH of test solutions within 4–7. Good selectivity was observed toward potassium, calcium, barium, magnesium, glycine, ascorbic acid, creatinine, norfloxacin, ciprofloxacin, and tetracycline. In flowing media, the biomimetic sensors presented good reproducibility (RSD of ± 0.7%), fast response, good sensitivity (47 mV/Δlog([ENR]/M), wide linear range (1.0 × 10^?5–1.0 × 10^?3 M), low detection limit (0.9 µg mL^?1), and a stable baseline for a 5 × 10^?2 M acetate buffer (pH 4.7) carrier. The sensors were used to analyze fish samples. The method offered the advantages of simplicity, accuracy, and automation feasibility. The sensing membrane may contribute to the development of small devices allowing in vivo measurements of enrofloxacin or parent-drugs.     

鱼肉中微囊藻毒素的高效液相色谱法分析

应用反相高效液相色谱法分析了鱼肉中藻毒素的含量。用BDS C18色谱柱,以水（含1％三氟乙酸）：甲醇＝30：70（V／V）溶液为流动相,238nm紫外检测。鱼肉样品用甲醇－水和丙酮混合溶剂提取,经正已烷萃取后,将有机相弃去,水相用固相萃取柱净化后进行高效液相色谱分析。该法检测限为10ng/g,峰面积标准曲线在50－250ng范围内有良好线性关系,平均回收率为85．1％－88．2％。     

A Novel Flow Injection Optical Fiber Biosensor for Hypoxanthine Based on Luminol Electrochemiluminescence

IntroductionIn the food industry,the determination of hy-poxanthine in fish meatcan be regarded as a simplemethod for evaluating fish freshness.When a fishis caught and killed,the breakdown of adenosine-5 - triphosphate( ATP) in the fish meat results inthe release of adenosine- 5 - diphosphate ( ADP) ,and further degradation products are adenosine- 5 -monophosphate( AMP) ,inosine- 5 - monophosphate( IMP) ,inosine( Hx R) ,hypoxanthine( Hx) ,xan-thine( X) and uric acid( UA) . It has be…     

甲苯胺蓝共振光散射法测定纳克级脱氧核糖核酸

研究了吩噻嗪类染料甲苯胺蓝 (TB)与DNA作用的共振光散射光谱 ,在pH 1 0～ 1 1的范围内 ,加入DNA导致甲苯胺蓝共振光散射增强 ,在 35 0nm处 ,存在一共振光散射增强峰 ,其强度与DNA浓度呈线性关系 ,据此建立了一种测定DNA的共振光散射法。对于ctDNA ,方法的线性范围为 0～ 90 0ng·mL-1 ,检出限为6 75ng·mL-1 ,RSD为 3 7% ;对于fsDNA ,方法的线性范围为 0～ 90 0ng·mL-1 ,检出限为 2 99ng·mL-1 ,RSD为 5 6 % .已用于合成样品中DNA的测定     

明胶大分子中的正电子湮没行为

利用正电子湮没寿命谱 ,从分子尺度上对两种分别从深海鱼皮和牛骨提取的明胶大分子的微观结构性能进行了研究 .正电子湮没寿命谱的长寿命组分给出了关于明胶大分子中自由体积空穴的信息 .结果表明 ,鱼明胶大分子中自由体积空穴的尺度与数量均低于骨明胶大分子 .同时 ,用鱼明胶和骨明胶作为成核分散介质的乳剂试验表明 ,鱼明胶可以改善卤化银颗粒的单分散性并抑制晶核的生长和聚结 .由此认为 ,明胶作为保护性胶体的功能与其微结构特征相关 .鱼明胶在控制卤化银颗粒成核与生长中的功能强于骨明胶 .