河水中兽药多残留分析时亲水亲脂平衡柱的基质效应和保留效果

基质效应是液相色谱-质谱联用(LC-MS)定量分析中的重要干扰因素。以反渗透水为空白对照进行LC-MS/MS检测,在500倍浓缩条件下考察了33种兽药分别经Waters、Supelco和CNW等3种亲水亲脂平衡(hydrophilic-lipophilic balance, HLB)固相萃取柱富集后的基质效应及其保留效果。结果表明,以反渗透水为基质时3种HLB柱均表现出外源性基质效应,对大部分喹诺酮类和四环素类兽药呈现促进效应,有两种HLB柱对雌激素类兽药等呈现抑制效应,对磺胺类兽药的基质效应不显著,有一种HLB柱对氯霉素类兽药呈现抑制效应;以河水为基质时,由于外源性杂质与内源性杂质共同作用,对大部分喹诺酮类和四环素类兽药呈现促进效应,对氯霉素类和雌激素类兽药呈现抑制效应,对磺胺类兽药基质效应不显著。与外标法相比较,基质匹配标准校正法可有效消除基质效应对检测结果的影响。在50 ng/L和200 ng/L两个加标水平下,Waters、Supelco和CNW 3种HLB柱对河水中33种目标兽药的校正后的回收率分别为40.3%~146.0%、37.8%~104.2%和52.9%~150.1%; RSD(n=4)为0.2%~14.6%。相同实验条件下3种HLB柱的外源性基质效应不容忽视。而采用基质匹配标准校正法克服目标物基质效应,保留效果无显著差异,富集效果良好,为河水样品中兽药多残留分析方法中固相萃取柱的选择提供了科学依据。     

Coordinates with Non-Singular Curvature for a Time Dependent Black Hole Horizon

A naive introduction of a dependency of the mass of a black hole on the Schwarzschild time coordinate results in singular behavior of curvature invariants at the horizon, violating expectations from complementarity. If instead a temporal dependence is introduced in terms of a coordinate akin to the river time representation, the Ricci scalar is nowhere singular away from the origin. It is found that for a shrinking mass scale due to evaporation, the null radial geodesics that generate the horizon are slightly displaced from the coordinate singularity. In addition, a changing horizon scale significantly alters the form of the coordinate singularity in diagonal (orthogonal) metric coordinates representing the space-time. A Penrose diagram describing the growth and evaporation of an example black hole is constructed to examine the evolution of the coordinate singularity.     

FLUCTUATIONS AND FUTURE TREND OF CLIMATE, GLACIERS AND DISCHARGE OF ■R■MQI RIVER IN XINJIANG

Based on the analyses of various data available of the rümqi River, Xinjiang, it is found that the warming trend of the climate in recent years is mainly accompanied by the decrease in precipitation, discharge, and glacial mass balance. Since the Little Ice Age, the temperature has increased by 0.5—1.0℃, while the precipitation, glacial volume and annual discharge have decreased by 50 mm, 41% and 11%, respectively. It is possible that the trend would last for the next 10—15 years.     

流域可持续发展系统的协调控制

流域可持续发展是以流域作为特殊区域的一种可持续发展模式,本将流域可持续发展视为一个整体,提出了“流域可持续发展系统”的研究框架,讨论了流域可持续发展系统协调控制的指导原则和协调控制的主要内容,详细研究分析了流域可持续发展系统在技术层次上协调控制的技术路线。     

“双溪堆积体”的成因及其主要工程地质特征

双溪堆积体”是大宁河上游广泛发育的、钙质胶结的碎石土堆积体,其成因与大宁河流域新近系不同时期发育的崩塌、滑坡和泥石流有密切的关系。在大宁河沿岸的双溪、中坝、神基坪一带,志留系泥岩粉砂岩等易风化软弱碎屑岩构成斜坡下部相对较缓的部位,二叠系或三叠系相对坚硬的灰岩则形成斜坡上部高陡的崖坡,坡脚则广泛分布着这种钙质胶结的“双溪堆积体”。     

非牛顿体不稳定流的研究

本文通过试验和分析研究了非牛顿体明渠不稳定流的机理,阐明了不稳定流的产生和发展是由于流体具有屈服应力,利用这一机理,解释了高含沙洪水的波动和“浆河”现象、冰川流和泥流的不稳定流和泥石流的阵流现象。     

金沙江下虎跳滑石板滑坡破坏机理及稳定性分析

1996年10月28日发生在金沙江下虎跳峡口的滑石板滑坡,因堵塞金沙江、摧毁公路而引起高度重视。野外调查发现,滑石板滑坡是典型结构面控制的顺层基岩滑坡,层面和两组近于垂直层面的节理将边坡厚层灰岩切割成不同规模的菱形块体,长期的风化作用、重力、降雨、人工开挖公路等因素作用下,这些菱形块体从顺层稳定状态演化为稳定性较差的“悬挂”体,受河谷边坡斜向割切影响,表现为梯级叠次“悬挂”,最外边的“悬挂”体稳定性最差,最容易发生快速滑动。因此,该滑坡每次发生破坏滑动的体积不会很大,但是具有多次重复发生的特点,值得高度注意。     

Heterogeneous immunoassay for soy protein determination using nile blue-doped silica nanoparticles as labels and front-surface long-wavelength fluorimetry

A long-wavelength fluoroimmunoassay for the determination of soy protein is reported for the first time using a conjugate composed of anti-soy protein antibodies bound to nile blue-doped silica nanoparticles (NPs). These NPs have been synthesized by a reverse-micelle microemulsion method and functionalized by using 3-(aminopropyl)triethoxysilane (APS) and 3-(trihydroxysilyl)propyl methylphosphonate (THPMP) to avoid NP aggregation. The tracer has been obtained by linking the functionalized NPs with anti-soy protein antibodies previously oxidised with sodium periodate. The immunoassay has been developed in 96-well microplates using a heterogeneous competitive format with antibody capture. Soy proteins are immobilised onto the wells and bovine serum albumin is added to block the surface, thus minimising non-specific binding. After washing, the microplates can be stored ready to use. At the analysis time, soy protein standards or sample and tracer are added and incubated and, after the corresponding washing and drying steps, the fluorescence is measured onto the solid surface at λ_ex 620 and λ_em 680 nm. The method features a dynamic range of 0.1–10 mg L⁻¹ and a detection limit of 0.05 mg L⁻¹. The precision of the method has been assayed at 0.5 and 5 mg L⁻¹ protein concentrations, obtaining the values of relative standard deviation of 9.6% and 6.1%, respectively. This new immunoassay has been applied to the analysis of food containing soy protein and the results obtained have been compared to those provided by a commercial ELISA kit with no statistically differing results. Also, a recovery study has been performed, providing percentages in the range of 81.5–111.0%.     

Sensitive adsorptive stripping voltammetric method for direct determination of trace concentration of lead in the presence of cupferron in natural water samples

This paper reports the use of an adsorptive voltammetric technique for Pb(II) determination using cupferron as a selective complexing agent. After accumulation of the complex onto a hanging mercury drop electrode, the electrode potential was scanned with differential pulse modulation and the reduction current of lead was observed at about??0.5?V. Under optimum conditions (5?×?10^?4?mol?L^?1 cupferron concentration, 0.1?mol?L^?1 acetate buffer (pH 5.5), adsorption at??50?mV for 30?s) the detection limit was 5.1?×?10^?10?mol?L^?1. The relative standard deviation of five measurements for low lead concentration was 3.1%. The accuracy of the method was tested by analysing certified reference material (SPS-WW1 Waste Water). Finally, the method was successfully applied to the determination of Pb(II) in river water samples without any pretreatments.     

Labeling Microplastics with Fluorescent Dyes for Detection,Recovery, and Degradation Experiments

Staining microplastics (MPs) for fluorescence detection has been widely applied in MP analyses. However, there is a lack of standardized staining procedures and conditions, with different researchers using different dye concentrations, solvents, incubation times, and staining temperatures. Moreover, with the limited types and morphologies of commercially available MPs, a simple and optimized approach to making fluorescent MPs is needed. In this study, 4 different textile dyes, along with Nile red dye for comparison, are used to stain 17 different polymers under various conditions to optimize the staining procedure. The MPs included both virgin and naturally weathered polymers with different sizes and shapes (e.g., fragments, fibers, foams, pellets, beads). We show that the strongest fluorescence intensity occurred with aqueous staining at 70 °C for 3 h with a dye concentration of 5 mg/mL, 55 mg/mL, and 2 µg/mL for iDye dyes, Rit dyes, and Nile red, respectively. Red fluorescent signals are stronger and thus preferred over green ones. The staining procedure did not significantly alter the surface, mass, and chemical characteristics of the particles, based on FTIR and stereomicroscopy. Stained MPs were spiked into freshwater, saltwater, a sediment slurry, and wastewater-activated sludge; even after several days, the recovered particles are still strongly fluoresced. The approach described herein for producing customized fluorescent MPs and quantifying MPs in laboratory-controlled experiments is both straightforward and simple.