超分子溶剂直提测定水中的多环芳烃

超分子溶剂是两亲化合物通过分子间有序的自组装过程形成的具有纳米结构的胶束聚集体,是一种高效提取溶剂。该文以高效液相色谱-荧光检测法为测试手段,系统地对超分子溶剂组成及用量进行了优化,发展了一种直接提取、快速测定水中多环芳烃的方法,并进行了方法学验证及实际样品检测。结果表明,采用四氢呋喃和1-辛醇制备的超分子溶剂对4种多环芳烃的回收率为89.08%~102.47%,相对标准偏差(RSD,n=5)为1.38%~3.92%。4种多环芳烃在一定范围内线性关系良好(相关系数R~20.999),检出限为1.26~9.23 ng/L。该方法前处理过程简单,有利于实现快速分析;溶剂使用量少,符合绿色化学的发展趋势,具有一定的推广价值。     

A Fluorescent Zirconium‐Based Metal‐Organic Framework for Selective Detection of Nitro Explosives and Metal Ions

In this work, a new porous Zr‐based metal‐organic framework (MOF ) with a large Brunner‐Emmet‐Teller (BET ) surface area was prepared by the solvothermal method using 4,4’‐(naphthalene‐1,4‐diyl)dibenzoic acid (NDDA ) as the organic ligand, and the luminescent detection performance was studied systematically. The experiments combing with computations indicate that the as‐synthesized material can sensitively and selectively detect nitro explosives and metal ions, especially for 2,4,6‐trinitrophenol (TNP ) and Fe³⁺, due to the possible electron transfer from inorganic moieties to organic moieties with naphthalene part. Interestingly, owing to its high porosity and large surface area, this Zr‐MOF showed quick luminescent response time (in 1 min) for TNP and Fe³⁺. The results obtained may provide useful information for the design of MOFs with the large permanent porosity in sensing applications for large molecules in the future.     

HPLC method for determination of moxifloxacin in plasma and its application in pharmacokinetic analysis

Moxifloxacin is a representative of the fourth generation of fluoroquinolones. It possesses bacteriostatic activity against Gram-positive and Gram-negative bacteria. A simple and fast high performance liquid chromatography-ultraviolet detection (HPLC-UV) method was developed for moxifloxacin analysis. The separation was performed on C18 column. The mobile phase was a mixture of acetonitrile and 0.4% triethylamine solution. The regression curve was linear over the range 0.2–10.0?µg/mL. The validation parameters obey the European Medicine Agency limits. The in vivo study confirmed the practical application of the method.     

Effect of ultraviolet absorption reagent for determination of piperidinium ionic liquid cations by ion pair chromatography with indirect ultraviolet detection

Indirect ultraviolet detection method is a simple and effective method for the determination of ionic liquid cations without ultraviolet absorption group. This paper focused on the influence of different background ultraviolet absorption reagents on the determination of piperidinium ionic liquid cations by ion pair chromatography with indirect ultraviolet detection. Ultraviolet absorption reagents are divided into cationic (4-aminophenol hydrochloride, 1-ethyl-3-methylimidazolium tetrafluoroborate, and N-ethylpyridinium tetrafluoroborate), anionic (potassium biphthalate and 5-sulfosalicylic acid), and amphiprotic (p-aminobenzoic acid). The results showed that piperidinium cations can be separated and detected by cationic and anionic ultraviolet absorption reagents. In general, the cationic ultraviolet absorption reagents have the best effect for separation and detection of the piperidinium cations by ion pair chromatography with indirect ultraviolet detection.     

稳健残差控制图的构建及在金融时序中的应用

对于呈现自相关和波动族聚性并存的受控过程,通常采用残差控制图对其进行监控。但异常点的存在会对自相关或波动族聚性模型的拟合产生重要影响,使得基于该模型的残差并非独立同分布导致常规残差控制图监控失效。为解决这类问题,本文提出稳健残差控制图。即建立稳健的ARMA模型解决自相关问题从而得到无自相关的残差序列,用稳健的GARCH模型来构建控制图的上下限。模拟和实证研究表明,本文提出的稳健残差控制图具有很好的抗异常点能力并能更好的对金融时间序列的异常现象进行监控。     

Classification of edges using compactly supported shearlets

We analyze the detection and classification of singularities of functions $f={\chi }_S$, where $S?{\mathbb{R}}^d$ and $d=2,3$. It will be shown how the set ?S can be extracted by a continuous shearlet transform associated with compactly supported shearlets. Furthermore, if ?S is a $d?1$ dimensional piecewise smooth manifold with $d=2$ or 3, we will classify smooth and non-smooth components of ?S. This improves previous results given for shearlet systems with a certain band-limited generator, since the estimates we derive are uniform. Moreover, we will show that our bounds are optimal. Along the way, we also obtain novel results on the characterization of wavefront sets in 3 dimensions by compactly supported shearlets. Finally, geometric properties of ?S such as curvature are described in terms of the continuous shearlet transform of f.     

Online Flowing Colloidosomes for Sequential Multi‐analyte High‐Throughput SERS Analysis

3D plasmonic colloidosomes are superior SERS sensors owing to their high sensitivity and excellent tolerance to laser misalignment. Herein, we incorporate plasmonic colloidosomes in a microfluidic channel for online SERS detection. Our method resolves the poor signal reproducibility and inter‐sample contamination in the existing online SERS platforms. Our flow system offers rapid and continuous online detection of 20 samples in less than 5 min with excellent signal reproducibility. The isolated colloidosomes prevent cross‐sample and channel contamination, allowing accurate quantification of samples over a concentration range of five orders of magnitude. Our system demonstrates high‐resolution multiplex detection with fully preserved signal and Raman features of individual analytes in a mixture. High‐throughput multi‐assay analysis is performed, which highlights that our system is capable of rapid identification and quantification of a sequence of samples containing various analytes and concentrations.     

Indirect ultraviolet detection of alkaline earth metal ions using an imidazolium ionic liquid as an ultraviolet absorption reagent in ion chromatography

A convenient and versatile method was developed for the separation and detection of alkaline earth metal ions by ion chromatography with indirect UV detection. The chromatographic separation of Mg²⁺, Ca²⁺, and Sr²⁺ was performed on a carboxylic acid base cation exchange column using imidazolium ionic liquid/acid as the mobile phase, in which the imidazolium ionic liquid acted as an UV‐absorption reagent. The effects of imidazolium ionic liquids, detection wavelength, acids in the mobile phase, and column temperature on the retention of Mg²⁺, Ca²⁺, and Sr²⁺ were investigated. The main factors influencing the separation and detection were the background UV absorption reagent and the concentration of hydrogen ion in ion chromatography with indirect UV detection. The successful separation and detection of Mg²⁺, Ca²⁺, and Sr²⁺ within 14 min were achieved using the selected chromatographic conditions, and the detection limits (S /N = 3) were 0.06, 0.12, and 0.23 mg/L, respectively. A new separation and detection method of alkaline earth metal ions by ion chromatography with indirect UV detection was developed, and the application range of ionic liquids was expanded.     

Effective length calibration method for processing the fluorescence signal detected by charge‐coupled device in capillary electrophoresis

A novel method named effective length calibration method has been developed to process the fluorescence signal detected by charge‐coupled device during capillary electrophoresis. The new method treated each pixel as an individual point detector, and effectively binned a large number of pixels into a final electropherogram without losing the narrow detection window defined by a single pixel. Capillary electrophoresis separations of DNA were carried out and detected by charge‐coupled device and conventional detector (photomultiplier tube). Detection properties including signal‐to‐noise ratio, peak width, detection frequency, and tilt of detector were investigated. It was found that the new method achieved much higher signal‐to‐noise ratio and smaller peak width than the conventional detector did. A Detection width of 0.5 μm was easily achieved.     

Synthesis of Cu2O/Ag Composite with Visible Light Photocatalytic Degradation Activity for in situ SERS Analysis

A multifunctional Cu₂O/Ag micro-nanocomposite, which has the characteristics of high catalytic activities under the visible light and high surface-enhanced Raman scattering (SERS) activity, was fabricated via a facile method and employed for the in situ SERS monitoring of the photocatalytic degradation reaction of crystal violet. Through the variation of the AgNO₃ concentration, Ag content on the Cu₂O template can be controllably tuned, which has great influence on the SERS effect. The results indicate that Ag nanoparticles form on the Cu₂O nanoframes to obtain the Cu₂O/Ag nanocomposite, which can act as an excellent bifunctional platform for in situ monitoring of photocatalytic degradation of organic pollutions by SERS.