DMSO辅助浓缩气相色谱-质谱联用仪测定水产品中6种丁香酚类化合物

建立了水产品中6种丁香酚类化合物的二甲亚砜(DMSO)辅助浓缩-气相色谱-质谱联用仪(GC-MS)测定方法。试样加入无水硫酸钠后,以乙腈为提取溶剂,乙腈饱和的正己烷脱脂,乙腈层加入二甲亚砜(DMSO)辅助氮吹浓缩至近干;采用DB-1701色谱柱进行分离,并用质谱进行检测。6种化合物在20~1000 μg/L内呈良好的线性关系(相关系数大于0.999);在四种基质中的加标水平分别为0.02、0.04、0.10 mg/kg时,6种化合物平均加标回收率为64.8%~110.9%,相对标准偏差均不大于15%(n=6);方法定量限为0.02 mg/kg。该方法灵敏、准确度高、快速、线性范围宽、选择性好、前处理简单,并解决了目前文献方法中仅直接氮吹浓缩对回收率影响很大的关键问题,适用于水产品中丁香酚类化合物的准确定性定量检测,可用于水产品中该类麻醉剂的摸底监测。     

全自动橡塑材料磨样试验机的研制

为提升橡塑材料试样的精确度和制样效率,研制了全自动橡塑材料磨样试验机。该试验机由软件控制系统、磨削系统和安全防护系统组成,实现了试样的自动打磨。验证结果表明：与传统砂轮磨样机的手动打磨法相比,该试验机的自动打磨法的试样准确度和精密度显著提高,制样效率可提高1.5倍以上。     

Real-time recombinase-aided amplification with improved propidium monoazide for the rapid detection of viable Escherichia coli O157:H7 in milk

Escherichia coli O157:H7, the causative agent of thrombotic thrombocytopenic purpura and hemolytic uremic syndrome in humans, generates a effective harm to community health because of its high pathogenicity. A real-time recombinase-aided amplification (rRAA) is an emerging method for nucleic acid detection. However, genomic DNA of bacteria could exist in food and the environment for a long time after death and could be amplified by rRAA assay, resulting in false-positive signal; thus, developing a fast and sensitive method is necessary to detect viable foodborne pathogens in food products. In our research, rRAA assay coupled with an enhanced nucleic acid binding dye named improved propidium monoazide (PMAxx) was established and applied in viable E. coli O157:H7 identification in skim milk. The PMAxx could eliminate interference from dead bacteria by permeating impaired membranes and covalently linking to DNA to prevent DNA amplification. The PMAxx-rRAA assay was performed with high sensitivity and good specificity. The PMAxx-rRAA assay could detect as low as 5.4 × 10⁰ cfu/mL of viable E. coli O157:H7 in pure culture, and 7.9 × 10⁰ cfu/mL of viable E. coli O157:H7 in skim milk. In addition, the PMAxx-rRAA assay was performed in the presence of a high concentration of dead bacteria or nontarget bacteria in skim milk to verify the capacity to resist interference from dead bacteria and nontarget bacteria. Therefore, the established PMAxx-rRAA assay is a valuable tool for the identification of viable E. coli O157:H7 in complex food matrix.     

超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法快速检测茶叶中草甘膦、草铵膦及其代谢物残留

摘 要：目的 建立一种非衍生化处理, 直接测定茶叶中草甘膦、草铵膦及代谢物的的快速分析方法。方法 茶叶样品经酸化的同体积甲醇-水进行提取, 经Oasis PRiME HLB 固相萃取柱通过式净化, 并通过超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法对样品进行测定。结果 茶叶中草甘膦、草铵膦及代谢物在1.0~50 ng/mL的范围内, 线性关系良好(r2＞0.999), 平均回收率在83.7%~92.2%之间, 相对标准偏差低于10%, 检出限为0.01 mg/kg, 定量限为0.05 mg/kg。结论 此方法前处理简便快速, 且准确性好、灵敏度高, 可实现茶叶中草甘膦、草铵膦及其代谢物的快速筛查。     

贻贝中微塑料检测的消解方法比较

目的 比较贻贝中微塑料(microplastics, MPs)检测常用的酸消解、碱消解、氧化消解和酶消解等方法,推荐适用于贝类中微塑料检测的通用型消解方式。方法 以常用的指示性双壳贝类贻贝作为研究对象,确定食品样品检测通用的消解条件。在这些条件下对聚苯乙烯(polystyrene, PS)、聚丙烯(polypropylene, PP)、聚碳酸酯(polycarbonate, PC)、聚乙烯(polyethylene, PE)、聚对苯二甲酸乙二醇酯(polyethylene terephthalate, PET)、聚酰胺6 (polyamide, PA6)和聚酰胺66 (polyamide, PA66) 7种微塑料进行消解,考察不同条件下微塑料粒子消解前后重量、红外光谱、粒径分布和形貌特征的变化。结果 采用不同的消解方式对不同的微塑料影响不同,其中重量受影响较大的是PA6和PA66,在硝酸-高氯酸混合溶液和高氯酸-双氧水混合溶液中完全溶解损失,PC和PET在氢氧化钾溶液中损失严重。通过结构表征, PE、PA6和PC的粒径增加, PC的形貌结构发生彻底改变。结论 对微塑料含量甚微的双壳贝类...     

热裂解-气相色谱-质谱法快速筛查和定量分析乳与乳制品中的4种微塑料

目的建立热裂解-气相色谱-质谱法(pyrolysis-gas chromatography mass spectrometry,PY-GC-MS)快速筛查和定量分析乳与乳制品中的4种微塑料(microplastics,MPs)的方法。方法以聚碳酸酯(polycarbonate,PC)、聚对苯二甲酸乙二醇酯(polyethylene terephthalate,PET)、聚酰胺6 (polyamide 6,PA6)和聚酰胺66(polyamide 66,PA66) 4种微塑料粒子为例,采用红外光谱和粒度分析对微塑料形貌进行表征。考察进样模式、裂解温度对裂解效果的影响,并对4种微塑料的特征定量峰进行比较,最终选择单击式裂解模式,裂解温度600℃,4种微塑料的特征物质分别为双酚A、对苯二甲酸-2-苯甲酰氧基乙酯乙烯酯、己内酰胺和环戊酮。验证裂解方法的稳定性和特异性,利用高温裂解产生的特征碎片离子进行定量分析。结果本方法对4种微塑料检测的线性范围为2～64μg与4～64μg (PET),检出限为0.1～1.2μg,定量限为0.3～4.0μg,平均加标回收率为79.5%～96.0%,精密度为1....     

Current challenges and potential directions towards precision microscale additive manufacturing – Part III: Energy induced deposition and hybrid electrochemical processes

The Part III of the four-part series of articles discusses the challenges and opportunities in microscale additive manufacturing processes, specifically focusing on energy-induced deposition and electrochemical processes. Compared to the direct ink write (DIW) and laser-based processes, the energy-induced deposition methods can fabricate high-resolution, high aspect ratio and complex parts, while the hybrid electrochemical process can be used to fabricate complex parts using a wide range of conductive and photoactive materials. However, the volumetric throughput of these processes is lower than their DIW and laser-based counterparts. The processes that have been explored in this process are Focused-ion Beam Induced Deposition (FIBID), Laser Chemical Vapor Deposition (LCVD), Menicus-confined Electrodeposition (MCED) and Laser-Enabled Electrochemical Printing (LECP). The range of processable materials, feature-size resolution, geometry and volumetric throughput are used as factors to evaluate the current state-of-the-art for these processes. Novel approaches have been proposed in the article to address these challenges associated with microscale AM processes.     

Using genetic algorithm to support clustering-based portfolio optimization by investor information

A clustering-based portfolio optimization scheme that employs a genetic algorithm (GA) based on investor information for active portfolio management is presented. Whereas numerous studies have investigated trading behaviors, investor performance, and portfolio investment strategies, few works have developed investment strategies based on investor information. This study is conducted in two phases. First, a basket of portfolio (i.e., a collection of stocks held in individual portfolios) is developed through a cluster analysis of investor information. A GA is then employed to optimize the weights of the selected stocks. And the optimized portfolio is rebalanced to get excess return. It is concluded that the proposed multistage portfolio optimization scheme for active portfolio management generates superior results than previously proposed methods for the Korean stock market.     

Review of the current methods of analytical traceability allowing determination of the origin of foodstuffs

Modern analytical techniques, in particular molecular biology techniques, can determine the plant or animal species present in a foodstuff. It is actually very difficult to determine the geographical origin of a food. The new European regulation 178/2002, applicable on January 1st, 2005 imposes this requirement for the traceability of food. This article gives a progress report on the physicochemical and microbiological analytical techniques available which make it possible to determine the origin of a food with some precision.     

竹纤维密胺餐具中单体物质界面迁移的机理研究

目的 分析竹纤维密胺复合制品中有害单体物质在材料中扩散系数（Diffusion Coefficient,DC）的影响因素，探索其特定迁移量变化的规律和界面迁移机理。方法 本文以相同原料、不同工艺制成的竹纤维密胺餐具为试验样本，采用液相色谱仪、紫外分光光度计、扫描电子显微镜/能谱仪等方法研究了竹纤维密胺复合制品中三聚氰胺和甲醛残留单体的含量、特定迁移量、材料结构、扩散系数之间的关系和影响。结果 不同工艺制成的样本存在界面结构和残留单体浓度差异是影响单体物质扩散系数的主要内在因素。扩散系数是单体物质界面浓度因素和材料结构因素共同作用后形成的变量。随着浸泡时间的增加，模拟液对材料表面结构造成破坏，会促使扩散系数变大。同时，材料内单体浓度也在发生变化，单体浓度和界面结构共同影响下致使扩散系数增加或减少。结论 竹纤维密胺复合制品在单体物质特定迁移量的试验过程中，由于界面结构的变化，影响了扩散系数，验证了特定迁移量数值上的变化规律，为评价竹纤维密胺制品的安全性提供了参考。