Development of gold nanoparticle-based rapid detection kit for melamine in milk products

A reliable and sensitive kit for the rapid detection of melamine (Mel) was developed. The kit is based on gold nanoparticle (Au NP) probe and includes a standard colorimetric card. The Au NPs were prepared by sodium borohydride reduction and characterized by transmission electron microscopy, which revealed particle sizes of approximately 5 nm. The performance of the kit in terms of aggregation kinetics, cross-reactivity, anti-interference, and sample pretreatment was investigated. The standard colorimetric card was then fabricated by chromatic aberration of a series of standard Mel-spiked milk reacts with the 5 nm Au NPs. The working range of the kit is 1-120 mg/L, and its performance is visibly more rapid and reliable by comparison with the standard colorimetric card. As low as 1 mg/L of Mel levels in milk can be determined, with the assay taking only about 10 min, including sample pretreatment. The kit can be stored for a year at room temperature. Samples were also detected by the kit, yielding results close to those obtained by high-performance liquid chromatography/mass spectrometry. Thus, the kit is applicable to qualitative and semiquantitative field detection, as well as naked-eye screening without the aid of any instrumentation.     

原位合成纳米金/石墨烯修饰玻碳电极检测水和土壤中痕量铅

为提高痕量铅的检测精度,提出了一种简单、可控的一步还原法在裸玻碳电极表面原位合成纳米金/石墨烯材料的方法,并通过循环伏安法(cyclic voltammetry,CV)对修饰电极进行电化学表征。利用修饰后的电极对醋酸-醋酸钠缓冲溶液中的铅离子(Pb(Ⅱ))标准样品进行检测,并对检测条件进行了优化。优化条件下的试验结果表明,在pH值为4.5的醋酸-醋酸钠缓冲溶液中,Pb(Ⅱ)的溶出峰为-0.08 V,在1～90μg/L范围内Pb(Ⅱ)的溶出峰电流与Pb(Ⅱ)浓度之间呈现良好的线性关系(R~2=0.985),最小检测下限为0.27μg/L。在优化后的条件下采用该电极测定了实际水样与土壤中的Pb(Ⅱ)含量,加标回收率区间分别为93.75%～109.20%和93.82%～109.9%,相对标准偏差均小于7%,可以用于对实际水样与土壤样本的检测。     

High pressure liquid chromatographic determination of aflatoxins in peanut butter using a silica gel-packed flowcell for fluorescence detection

A high pressure liquid chromatographic method has been developed for determining aflatoxins B1, B2, G1, and G2 in peanut butter. The method is based on extraction with acidified aqueous methanol, partition of the aflatoxin into methylene chloride, and purification of the extract on a 2 g silica gel column. The extracted aflatoxins are resolved on a microparticulate (10 micrometer) porous silica gel column in ca 10 min with a water-washed chloroform-cyclohexane-acetonitrile solvent that contains 2% isopropanol. The fluorescence detection system determines aflatoxins B1, B2, G1, and G2 at low levels, i.e., 0.25 ppb B1, 0.5 ppb G1, and 0.2 ppb B2 and G2. Multiple assays of 5 samples of naturally contaminated peanut butters containing total aflatoxins (B1 + B2 + G1 + G2) at levels of 1, 2, 3, 9, and 17 ppb gave intralaboratory coefficients of variation of 7, 4, 4, 11, and 3%, respectively. Samples spiked at levels of 5, 9, and 17 ppb total aflatoxins showed recoveries of 79, 81, and 81%, respectively.     

豆粕中三聚氰胺显微近红外成像检测的扫描条件优化

为了确定豆粕中三聚氰胺显微近红外成像检测的最佳扫描条件,该文研究了扫描条件对显微近红外光谱图像质量、采集效率和豆粕中三聚氰胺检测效果的影响。针对不同光谱分辨率和扫描次数对光谱图像均方根噪声（RMS）的影响进行了单因素方差分析试验,对干涉仪动镜移动速度（1、2.2 cm/s）、空间分辨率（25、50 μm）、光谱分辨率（8、16、32 cm-1）和扫描次数（4、8、16次）进行了多因素正交试验方差分析,结果得出光谱分辨率对RMS有显著性影响,而且采用不同扫描条件时显微近红外图像采集时间相差很大。根据图像质量、采集效率和豆粕中三聚氰胺检测效果分别得出优选扫描条件,综合考虑上述3个方面,最终推荐采用的扫描条件为空间分辨率为25 μm,干涉仪动镜移动速度为1 cm/s,光谱分辨率为32 cm-1,扫描次数为4次。该研究同时表明显微近红外成像技术可应用于豆粕中三聚氰胺的检测。     

制冷系统不同表面能微通道的流动沸腾传热特性试验

为了研究微通道壁面特性对流动沸腾传热的影响,该文以具有不同表面能的微通道为研究对象,制冷剂R141b为试验工质,在不同热流密度、质量流率下对微通道内的沸腾传热特性进行了试验探究。结果表明:在该试验工况下,质量流率的增加有利于沸腾传热,但微通道内过冷段长度也相应增加;在微通道饱和沸腾区传热系数较稳定,但沿工质流动方向有缓慢降低的趋势;相比于表面能为23.93 m N/m的3#的微通道,表面能为60.03和49.54 m N/m的1#和2#微通道沸腾传热系数分别提高18.42%和9.28%;根据试验值与关联式预测值的对比情况,对Lazarek关联式进行修正,拟合得到能很好预测该试验各工况下的传热关联式,平均绝对误差为9.76%。该研究为微通道换热器的设计提供了参考。     

Single and mixture toxicity of gold nanoparticles and gold(III) to Enchytraeus buchholzi (Oligochaeta)

The ecotoxicity of gold nanoparticles (Au-NPs), gold(III) and their mixtures was assessed in the potworm Enchytraeus buchholzi after 14-day bioassays. The worms were exposed at 20 °C in OECD artificial soil to 0, 9.37, 18.7, 28.1 and 37.5 mg/kg Au-NPs or Au(III) and 0, 9.37 + 9.37, 18.7 + 18.7, 28.1 + 28.1, 37.5 + 37.5 mg Au-NPs + Au(III)/kg. The results indicated that the range of Au-NPs concentrations used in the present study was not deleterious to the survival and reproduction of E. buchholzi. Au(III) showed no significant effect on survival but was significantly deleterious to reproduction in the highest treatment (p ≤ 0.01). A 14-day EC50_Au(III) = 35.5 mg/kg was estimated for effects on reproduction. Au-NPs/Au(III) mixtures essentially caused the same effects as Au(III) except for 18.7 mg Au(III)/kg vs. 18.7 + 18.7 mg Au-NPs + Au(III)/kg where the mixture treatment was significantly more toxic to reproduction (p < 0.02). Mixture results suggested a seemingly additive effect between Au-NPs and Au(III), although the conventional toxic unit approach could not be used to ascertain this conclusively because of the lack of Au-NPs toxicity. The order of toxicity between Au-NPs, Au(III) and their mixtures was Au-NPs = Au(III) = Au-NPs/Au(III) for survival and Au-NPs < Au(III) ≤ Au-NPs/Au(III) for reproduction.     

太阳能与生物质能联合驱动吸附制冷系统的适配性分析

针对生物质能作为辅助能源用于太阳能吸附制冷系统供冷的适配性,以已搭建的太阳能与生物质能联合驱动吸附式制冷试验台为研究对象,试验研究了双热源联合运行供能耦合的可能性。采用MATLAB软件动态模拟了双热源串、并联运行工况,并借助非线性最小二乘法对数据进行处理、分析。结果表明:串联运行时,按照模式2工况循环流动,可较好地实现系统热量的传递;并联运行时,通过对太阳能与生物质能联合供能的适配性研究,结合系统末端供冷需求和经济运行模式分析,得出太阳能与生物质能联合供能的最佳回水流量分配比值范围为0.5~0.6,提出适宜于双热源联合供能3种经济运行模式。研究结果可为改善制冷系统性能的稳定性、实现太阳能与生物质能的有效结合提供参考。     

Development of an immunochromatographic strip test for rapid detection of melamine in raw milk, milk products and animal feed

A simple, rapid and sensitive immunogold chromatographic strip test based on a monoclonal antibody was developed for the detection of melamine (MEL) residues in raw milk, milk products and animal feed. The limit of detection was estimated to be 0.05 μg/mL in raw milk, since the detection test line on the strip test completely disappeared at this concentration. The limit of detection was 2 μg/mL (or 2 μg/g) for milk drinks, yogurt, condensed milk, cheese, and animal feed and 1 μg/g for milk powder. Sample pretreatment was simple and rapid, and the results can be obtained within 3-10 min. A parallel analysis of MEL in 52 blind raw milk samples conducted by gas chromatography-mass spectrometry showed comparable results to those obtained from the strip test. The results demonstrate that the developed method is suitable for the onsite determination of MEL residues in a large number of samples.     

虾夷扇贝海上转运系统改进设计与试验

针对目前虾夷扇贝(Patinopecten yessoensis)海上转运系统作业装备落后及作业方式不合理,致使作业效率低、用工人数多、以及扇贝缩边死亡与碎贝现象严重等问题,通过对獐子岛虾夷扇贝海上转运系统的调研,提出了一种转运方案,并对转运装备进行优化设计。通过海上生产对比试验,得出以下结论:为虾夷扇贝采捕船配备甲板拣贝作业系统与可折叠式装贝笼箱,优化了采捕船拣贝、装箱、装卸舱等作业模式,使劳动强度大幅降低,且用工人数减少2人/艘,作业时间缩短了约0.6 h;运输船采用可折叠式装贝笼箱代替原转运笼箱,使笼箱装卸流程更加合理高效,且作业时间缩短了约0.52 h;采用改造后虾夷扇贝转运系统运输,扇贝缩边死亡率与碎贝率显著降低,其中扇贝平均缩边死亡率约为1.92%,且5个月试验扇贝缩边死亡率无显著差异(P0.05),与原转运系统相比显著降低(P0.05),降低了约1.43%;改造后平均碎贝率约为0.84%,且5个月试验碎贝率无显著差异(P0.05),较原转运系统显著降低(P0.05),降低了约1.99%;改造后的虾夷扇贝海上转运系统经济效果显著,每年可节省费用约2 853.6万元。由此说明,改造后的虾夷扇贝海上转运系统具有高效、高收益等特点,推广应用前景广阔。     

Effect of humic acid on the sedimentation and transport of nanoparticles silica in water-saturated porous media

Journal of Soils and Sediments - Nano silicon particles (nSiO2) is one of the most widely used industrial engineered nanomaterials (ENMs). The extensive applications of nSiO2 may pose potential...     

果园喷雾机器人靶标探测与追踪系统

针对风送喷雾装备不间断无差别喷施造成的过量用药和雾滴脱靶严重的问题,该研究设计一种果园喷雾机器人靶标探测与追踪系统,随果树对象位置变化实时调整喷雾角度实现精准对靶。该系统采用激光雷达扫描获取作业范围内果树的点云数据,确定靶标区域,然后通过点云分割、滤波等处理获得目标靶点,并根据目标靶点位置确定对应喷雾仰角;构建喷雾机构目标仰角与编码器脉冲数的数学模型,以及目标仰角与电动推杆行程的数学模型,设计喷雾机构仰角的测控方法。实际果树冠层靶点探测试验表明,随机选取的3棵果树目标靶点主要集中在距地2.0～3.5m范围内,系统可以依据冠层形状计算靶点并调节喷雾仰角,最小喷雾仰角为47.8°,最大喷雾仰角为51.4°,连续目标靶点之间喷雾仰角最大调节时间为0.06 s,可满足对靶的时效需求。该系统能够适应不同形态果树中下部对靶施药需求,为后续开展果园精准植保研究提供理论基础与技术参考。     

Sensitive silica gel-packed flowcell for fluorometric detection of aflatoxins by high pressure liquid chromatography.

Aflatoxins B1, B2, G1, and G2 were quantitatively detected by high pressure liquid chromatography on a 5 micronm Lichrosorb column, using a Lichrosorb-packed flowcell in the fluorometric detector. The relationship between peak height and the amount injected was linear only up to about 2 ng but showed a linear loglog relationship. Methods for constructing and packing the flowcell are given. A guard column and venting valve were used to minimize deterioration of the analytical column and the adsorbent-packed flowcell. The method was applied to a peanut butter extract, although with the cleanup procedure used, the life expectancy of the flowcell is limited.     

荧光猝灭法检测猕猴桃中氯吡脲的净化剂配方优化研究

为了寻求检测猕猴桃中氯吡脲时样品预处理的净化剂配方最佳组合,以N-丙基乙二胺(PSA)、弗罗里硅土(Florisil)、烷基-硅胶(C₁₈)为净化剂,采用Design-Expert中的混料设计研究3种净化剂的不同组合对猕猴桃中杂质和氯吡脲的影响,建立净化率和保留率与净化剂配比的回归模型,优化最佳工艺参数。结果表明,建立的净化率和保留率的二次多项回归模型均显著(p <0.05),可用于净化剂对猕猴桃中氯吡脲影响的预测和分析;净化剂的最优配方为PSA (32%)、Florisil (25%)、 C₁₈(44%)。在该配方下,对含有不同浓度氯吡脲的猕猴桃提取液进行净化处理,净化率和保留率最低分别可达89.02%、 92.48%。该配方可用于猕猴桃样品的净化处理,对提高猕猴桃中氯吡脲残留量的检测水平具有重要意义。     

玉米赤霉烯酮化学发光免疫分析检测系统设计

为了保障粮食安全,该研究根据玉米赤霉烯酮抗原抗体反应,以及辣根过氧化物酶催化鲁米诺过氧化氢反应产生化学发光,设计一款应用于粮食行业的玉米赤霉烯酮检测系统。采用侧窗型高精度光电倍增管MD983以及16位AD转换芯片,实现化学发光强度信号的准确测量;步进电机驱动旋转精密转台,通过优化步进电机的S型脉冲驱动控制曲线参数,完成转台的高精度定位控制,实现光电倍增管的测试窗口和化学发光孔精确对准;通过精密直线导轨滑台驱动加样器的进给,实现反应液微米量级的准确微量加样。利用竞争性免疫分析方法,使得赤霉烯酮毒素为0 μg/kg情况下,化学发光反应具有最大发光量,解决真菌毒素低浓度情况下的检测精度难题。经过试验验证,系统检出限为0.1 μg/kg,样品加标回收率在90%以上,标准曲线决定系数为0.996 5,系统检测玉米赤霉烯酮的线性范围为0~60 μg/kg。研究表明建立的玉米赤霉烯酮检测系统满足国家粮食行业对于粮食中玉米赤霉烯酮含量检测要求,为真菌毒素检测仪器的国产化提供参考。     

小麦播种量电容法检测系统设计与试验

为实现小麦播种机播种量的精准检测,该文基于电容法设计了一套用于小麦播种量检测的系统,由检测分辨率和排种轮转速与采样频率约束关系确定传感器结构尺寸,建立了种子数量与电容变化量之间的线性关系。在采样周期为15 ms、排种轮转数20 r/min条件下,基于时间窗口建立了小麦播种量实时检测最小二乘回归模型。为了使检测系统适用于不同的排种轮转速,提出了一种通过改变采样周期的检测方法,即排种轮速度每增加5 r/min时,采样周期相应减少0.4ms,则上述建立的最小二乘回归模型仍适用,对不同的排种轮转速均具有较高的检测精度,相对误差介于-2.26%~2.17%之间。本文所设计的检测系统为实现小麦播种量的精准检测提供了一种有效途径,具有较好的实用性和经济性。     

Development of a lateral flow colloidal gold immunoassay strip for the rapid detection of olaquindox residues

A rapid immunochromatographic lateral flow test strip of competitive format has been developed for the specific determination of olaquindox (OLA) residues in pig urine and muscle tissues. The sensitivity of the test strip was found to be 1.58 ± 0.27 μg/kg and 1.70 ± 0.26 μg/kg of OLA in pig urine and muscle tissues, and the lower detection limit was 0.27 ± 0.08 μg/kg and 0.31 ± 0.07 μg/kg respectively. For negative pig urine and muscle samples spiked with 4, 12, and 36 μg/kg, the recovery range was 83.0-94.0% and 78.8-87.4% and the coefficient of variation scope [CV (%)] was 3.17-7.41% and 4.66-7.64% respectively. Parallel analysis of OLA samples from pig urine and muscle tissue showed comparable results from the test strip and HPLC. Each test requires 5-8 min, and the test strip can provide a useful screening method for quantitative, semiquantitative, or qualitative detection of OLA residues.     

Use of a fractal-like gold nanostructure in surface-enhanced raman spectroscopy for detection of selected food contaminants

The safety of imported seafood products because of the contamination of prohibited substances, including crystal violet (CV) and malachite green (MG), raised a great deal of concern in the United States. In this study, a fractal-like gold nanostructure was developed through a self-assembly process and the feasibility of using surface-enhanced Raman spectroscopy (SERS) coupled with this nanostructure for detection of CV, MG, and their mixture (1:1) was explored. SERS was capable of characterizing and differentiating CV, MG, and their mixture on fractal-like gold nanostructures quickly and accurately. The enhancement factor of the gold nanostructures could reach an impressive level of approximately 4 x 10(7), and the lowest detectable concentration for the dye molecules was at approximately 0.2 ppb level. These results indicate that SERS coupled with fractal-like gold nanostructures holds a great potential as a rapid and ultra-sensitive method for detecting trace amounts of prohibited substances in contaminated food samples.     

获得甘薯×五倍体种间杂种的杂交后代的有效方法

为获得甘薯×五倍体种间杂种的大量杂交后代而进行的实验表明,反交(即以甘薯为父本)或蒙导授粉(五倍体活花粉与甘薯死花粉混授给异不孕群甘薯)显著促进五倍体花粉管生长和增加结实；生长调节剂(NAA+BA)授粉当天及授粉后5 d两次处理能有限地延长子房寿命；反交(或蒙导授粉)结合生长调节剂处理有利于获得大量适龄子房和有效胚珠，将它们置于筛选到的培养基(MS+CH，或MS+BA+GA3)，成苗率较高，是获得五倍体种间杂种同甘薯杂交的后代的有效方法；自交和互交均不结实的五倍体各系同甘薯品种相间种植以进行放任授粉，能在五倍体植株上收获大量杂交种子，是在一定条件下获得五倍体种间杂种同甘薯杂交的后代的有效方法。     

Quantitative liquid chromatographic method using fluorescence detection for determining zearalenone and its metabolites in blood plasma and urine

The liquid chromatographic (LC) method described, suitable for use with both blood plasma and urine, is applicable for determination of zearalenone and alpha-zearalenol at levels as low as 0.5 ng/mL plasma and 5 ng/mL urine. The sample is incubated overnight with beta-glucuronidase to analyze for both conjugated and unconjugated forms of zearalenone. The next day, the sample is acidified with H3PO4, extracted with chloroform, and evaporated to dryness. The residue is dissolved in toluene and loaded onto a silica gel cartridge which is washed with toluene and eluted with toluene-acetone (88 + 12). The eluate is evaporated, and the residue is dissolved in chloroform, extracted with 0.18M NaOH, neutralized with H3PO4, and re-extracted with chloroform. The chloroform extract is evaporated, dissolved in mobile phase for LC, and injected onto a normal phase column under the following chromatographic conditions: mobile phase of water-saturated dichloromethane containing 2% 1-propanol, and fluorescence detector, excitation wave-length 236 nm, and 418 nm cut-off emission filter. Recoveries of zearalenone and its metabolites from blood plasma and urine are 80-89% in the range 2.0-10 ng standard/mL plasma, and 81-90% in the range 10-30 ng standard/mL urine. This method was used to analyze blood and urine samples from a pig fed zearalenone-contaminated feed (5 mg/kg), corresponding to 80 micrograms/kg body weight. Zearalenone was rapidly metabolized to alpha-zearalenol, which appeared in the blood only 30 min after feeding. Almost all zearalenone and alpha-zearalenol was found conjugated with glucuronic acid in both blood plasma and urine.