Sol-Gel Method for the Preparation of Solid-Phase Microextraction Fibers

ABSTRACT

A novel sol-gel method is applied for the preparation of solid-phase microextraction (SPME) fibers. Scanning electron microscopy experiments suggested a porous structure for the poly(dimethylsiloxane) (PDMS) coating. SPME-GC analysis provided evidence that the sol-gel fibers have some advantages, such as high thermal stability, efficient extraction rates, high velocities of mass transfer, and spacious range of application.     

金纳米棒非聚集比色法测定多巴胺

基于在金纳米棒(AuNRs)-Ag⁺-多巴胺(DA)体系中,DA快速将Ag⁺还原为Ag,Ag包裹在AuNRs表面形成核壳状纳米棒(Au@AgNRs),改变了AuNRs周围的电介质环境,导致其纵横比减小、纵向等离子体共振吸收波长带(LPAB)蓝移,同时伴随着溶液的颜色发生显著的变化, 藉此开发了一种快速测定DA的比色法. 方法已成功应用于血清中DA的测定,其结果与荧光法相吻合. 此外,探讨了比色法测定DA的机理.     

An Efficient Solid-Phase Method for the Preparation of Diaryl Carbazones

The preparation of diaryl carbazones on solid-phase is reported for the first time. Using Fe(NO₃)₃.9H₂O as oxidant, seven diaryl carbazones have been synthesized under mild conditions in excellent yields. The method is convenient and efficient.     

A Simplex Optimized Colorimetric Method for Formaldehyde

Abstract

The development of a rapid and precise method for analyzing formaldehyde is described. By using an experiment design technique known as simplex optimization, the sensitivity for this procedure was maximized. The analysis requires under 2 minutes of the analyst's time per sample and gives an average coefficient of variation of 1.3 percent. The average sensitivity is 0.294 A/μg/ml and as little as 0.018 μg/ml can be detected with 90 percent confidence if triplicate analyses are performed.     

UPLC–TOF–MS Method for Simultaneous Quantification of Steroid Hormones in Tissue Homogenates of Zebrafish with Solid-Phase Extraction

The quantification of steroid hormones of individual zebrafish (Danio rerio) provides perspective to understand endogenous hormone function. A UPLC–TOF–MS method was developed to provide a reproducible, sensitive, and efficient assay to determine the concentration of steroid hormones, including cortisol, testosterone, androstenedione, 11-deoxycortisol, 11-deoxycorticosterone, and 17-hydroxyprogesterone in whole-body homogenates of each zebrafish. Solid-phase extraction was used to sample matrix clean-up and acquired a recovery from 89.7% to 107.9%. The analytes were separated on an Aquity BEH C18 column using gradient elution. Mass spectrometric analysis was performed by single reaction monitoring (SRM) using positive electrospray ionization mode. The total running time was 6 min, which was greatly shortened compared with a previously reported method. The developed method exhibited excellent linearity for all the analytes, with regression coefficients higher than 0.99. The limit of detection varied between 0.1 and 0.5 ng/L and the limit of quantification was 0.5–1.7 ng/L for all analytes. The precision of the method was assessed on replicate measurements and was found to be in the ranges of 1.9 % to 6.6% and 4.3% to 8.6%, for intra- and inter-day analysis, respectively. This method was validated according to FDA guidance and applied to determine steroid hormone levels in the tissue homogenate of zebrafish acutely treated with caffeine and ethanol.     

Molecularly Imprinted Polymers Modified by Deep Eutectic Solvents and Ionic Liquids with Two Templates for the Simultaneous Solid-Phase Extraction of Fucoidan and Laminarin from Marine Kelp

Molecularly imprinted polymers modified by deep eutectic solvents and ionic liquids (ILs) were prepared as packing materials for the solid-phase extraction (SPE) of fucoidan and laminarin. The prepared materials were characterized by field emission scanning electron microscopy and Fourier transform infrared spectroscopy. The polymers modified by the deep eutectic solvent prepared by choline chloride and urea had the best extraction efficiencies for fucoidan and laminarin (95.5% and 87.6%, respectively) from marine kelp. The relative standard deviations for intraday and interday determination were less than 4.23%. The molecularly imprinted polymers modified by deep eutectic solvents and ILs showed outstanding applications for SPE and may offer novel sample pretreatment for other analytes.     

Solid-Phase Spectrophotometry as an Efficient Method for the Determination of Heavy Metals in Foodstuffs

The complexation of some toxic elements with acid and basic dyes in the solid phase was studied. The results were used for the development of new procedures for determining trace metals in foodstuffs and potable water.     

Automated Colorimetric Method for Total Cyanide in Water and Wastewater

Abstract

An automated benzidine-pyridine method for the analysis of total cyanide is described. Cyanides are converted to cyanogen bromide by the reaction with bromine water. Cyanogen bromide reacts with benzidine in a dilute pyridine medium to form an intense red color directly proportional to the cyanide concentration. Cyanide often is found complexed with metals. Complex iron cyanides such as ferrocyanide or ferricyanide are difficult to decompose, but the conversion is hastened with mercuric chloride and magnesium chloride in a modified Serfass distillation.¹

Hydrogen cyanide is readily formed and absorbed in sodium hydroxide.     

Preparation of Ion Exchange Films for Solid-Phase Spectrophotometry and Solid-Phase Fluorometry

ABSTRACT

Atomic spectroscopy has dominated the field of trace inorganic analysis because of its high sensitivity and selectivity. The advantages gained by the atomic spectroscopies come with the disadvantage of expensive and often complicated instrumentation. Solid-phase spectroscopy, in which the analyte is preconcentrated on a solid medium followed by conventional spectrophotometry or fluorometry, requires less expensive instrumentation and has considerable sensitivity and selectivity. The sensitivity gains come from preconcentration and the use of chromophore (or fluorophore) developers and the selectivity is. achieved by use of ion exchange conditions that favor the analyte in combination with speciative chromophores. Little work has been done to optimize the ion exchange medium (IEM) associated with these techniques. In this paper we present a method for making ion exchange polymer films which considerably simplify the solid-phase spectroscopic techniques. They are mechanically sturdy and optically transparent in the ultraviolet and visible portion of the spectrum, which makes them suitable for spectrophotometry and fluorometry.     

A Sensitive Colorimetric Method for the Determination of Arsenic in Environmental and Biological Samples

Results of a thorough study and application of leucocrystal violet for the determination of arsenic in parts per million (ppm) levels in environmental and biological samples is described here. The proposed method is based on the reaction of arsenic with potassium iodate to liberate iodine. The liberated iodine selectively oxidises leucocrystal violet to form crystal violet dye in the presence of sodium hydroxide. The dye formed shows maximum absorbance at 592 nm. The detection limit of arsenic is 0.002 μgmL^?1 and the method obeys Beer's law over the concentration range of 0.1 μg - 1.0 μg of per 25 mL of final solution (0.004–0.04 ppm). The molar absorptivity was found to be 1.49 × 10⁶ L mol^?1 cm^?1. The proposed method was successfully applied for the determination of arsenic in various environmental and biological samples. The results are in good agreement with the standard reported method.     

基于液体阵列比色传感器鉴别不同茶叶的新方法

基于茶多酚与三价铁的络合性以及对氧化铈的还原性,构建了交叉响应的液体阵列传感器,为茶叶种类的区分提供了一种新方法.利用水热法合成了硅酸锌空心微球和纳米棒作为三价铁的吸附剂,同时合成了可被茶多酚还原的纳米氧化铈,以硅酸锌-硫氰酸铁和氧化铈共同构建3×3阵列.对5种茶多酚和14种茶叶进行了检测,每个样本做5次平行实验,通过聚类分析(HCA)和主成份分析(PCA)方法对反应前后的图谱进行了分析.结果表明,该阵列能够将结构类似的茶多酚化合物准确区分,并且平行样本之间稳定性较好;同时对不同品种的茶叶样本区分效果良好,结合反应前后的差谱图可以实现对茶叶的定性分析.该方法在茶叶品质和食品质量的快速可视化检测方面具有潜在应用价值.     

手机数码比色法测定土壤中总磷含量

基于在酸性介质中,磷酸二氢钾(KH2PO4)与钼酸钠及抗坏血酸作用,生成蓝色的络合物,溶液的颜色随着KH2PO4浓度的增加而逐渐变浅,并呈现一定颜色梯度的原理,提出了使用手机数码比色法测定土壤中总磷含量的分析新方法。方法的相对标准偏差(RSD)为1.2%,对样品进行加标回收实验,加标回收率在102%~103%。方法方便快捷,成本低,适合现场分析,是一种农民自行测定土壤中总磷含量的新方法。     

化学比色原理的甲醛气体检测仪校准方法

提出化学比色原理甲醛气体检测仪的一种校准方法。因为气泡吸收管的吸收效率不恒定及甲醛气体的溶解度受标准气体分压及温度影响,JJG 1022–2007不适用于检定化学比色原理甲醛气体检测仪。建立了以水中甲醛标准物质校准仪器零点漂移、灵敏度、线性误差、示值重复性及稳定性的方法。方法准确可靠,可实现计量校准和量值溯源。     

Method for the Analysis of Solutions Based on the Principle of Solid-Phase Separation and Determination of Ions

Results of investigations on the development of a method of ion analysis are reported. The method is based on the principle of the internal-diffusion ion-exchange separation of a test mixture followed by the detection of ions using the macroscopic field phenomenon in multicomponent ion exchange. The potentiograms obtained exhibit well-resolved peaks that correspond to the injected alkali metal cations. The performance characteristics of the proposed method are estimated.     

手机数码比色法测定土壤中总磷含量

基于在酸性介质中,磷酸二氢钾(KH2PO4)与钼酸钠及抗坏血酸作用,生成蓝色的络合物,溶液的颜色随着KH2PO4浓度的增加而逐渐变浅,并呈现一定颜色梯度的原理,提出了使用手机数码比色法测定土壤中总磷含量的分析新方法。方法的相对标准偏差(RSD)为1.2%,对样品进行加标回收实验,加标回收率在102%¹03%。方法方便快捷,成本低,适合现场分析,是一种农民自行测定土壤中总磷含量的新方法。     

A Solid-Phase Microcolumn Extraction Method for the Analysis of Acetic Acid and Furfural Emitted from Paper

A rapid non-destructive sampling technique for the analysis of volatile organic compounds emitted from paper sheets is presented. A capillary, which is connected to an adsorbent-packed microcolumn, is inserted between two sheets at the centre of a paper stack placed in a bag made of polyethylene terephthalate/aluminium/polyethylene. The other end of the microcolumn is connected to a gas-tight syringe and an appropriate volume (5 mL) of the gaseous phase is aspirated. The loaded microcolumn is transferred into a modified split/splitless inlet of the GC-FID for desorption and analysis. The method has been successfully applied to the analysis of acetic acid and furfural in artificially aged paper sheets and naturally aged old books. The method shows good repeatability with limits of quantification for acetic acid and furfural of 0.1 and 0.04 ng mL^?1 respectively in the gas phase.     

LC–MS Method for the Quantification of Clonazepam in Rat Plasma

A sensitive and specific high-performance liquid chromatography–tandem mass spectrometry method has been developed and validated for the determination of clonazepam in rat plasma. Clonazepam and internal standard diazepam were extracted from plasma samples by a single-step protein precipitation. The chromatographic separation was performed on a Dikma ODS-C18 reversed-phase column at 40 °C. The mobile phase composed of a premix of solvent A (0.1% formic acid–4 mM ammonium acetate–water)–solvent B (acetonitrile) (13:87, v/v) at a flow-rate of 0.7 mL min⁻¹. Positive electrospray ionization was utilized as the ionization source. Clonazepam and the internal standard were determined using multiple reaction monitoring of precursor → product ion transitions at m/z 316.0 → 270.0 and m/z 285.1 → 193.2, respectively. The lower limit of quantification was 0.25 ng mL⁻¹ using 50 μL plasma samples and the linear calibration range was from 0.25 to 128 ng mL⁻¹. The within- and between-batch RSDs were lower than 15% and the relative recoveries of clonazepam ranged from 97.4 to 104.7%. The mean extraction recoveries of clonazepam and IS were 79.7 and 77.6%, respectively. The method has been successfully applied to the pharmacokinetic studies in rat after oral administration of clonazepam.

     

固相有机合成中的连接基团

介绍了固相有机合成中的连接基团,特别是带有隔离单元的连接基团、无痕迹连接基团、安全拉手型连接基团和复合型连接基团的基本概念、发展近况以及它们的应用.