Fractionation of Volatile Constituents fromCurcumaRhizome by Preparative Gas Chromatography

A preparative gas chromatography (pGC) method was developed for the separation of volatile components from the methanol extract ofCurcumarhizome. The compounds were separated on a stainless steel column packed with 10% OV-101 (3 m × 6 mm, i.d.), and then, the effluent was split into two gas flows. One percent of the effluent passed to the flame ionization detector (FID) for detection and the remaining 99% were directed to the fraction collector. Five volatile compounds were collected from the methanol extract ofCurcumarhizome (5 g/mL) after 83 single injections (20 uL) with the yield of 5.1–46.2 mg. Furthermore, the structures of the obtained compounds were identified asβ-elemene, curzerene, curzerenone, curcumenol, and curcumenone by MS and NMR spectra, respectively.

Determination of Low Levels of Lead in Beer Using Solid-Phase Extraction and Detection by Flame Atomic Absorption Spectrometry

In this study, a method for the determination of low concentrations of lead in beer samples using solid-phase extraction with a flow injection analysis system and detection by flame atomic absorption spectrometry (FAAS) was developed.Moringa oleiferaseeds were used as a biosorbent material. Chemical and flow variables of the online preconcentration system, such as sample pH, preconcentration flow rate, eluent flow rate, eluent concentration, particle size, and sorbent mass, were studied. The optimum extraction conditions were obtained using a sample pH of 6.0, sample flow rate of 6.0 mL min−1, 63.0 mg of sorbent mass, and 2.0 mol L−1HNO3at a flow rate of 2.0 mL min−1as the eluent. With the optimized conditions, the preconcentration factor, precision, detection limit, consumption index, and sample throughput were estimated as 93, 0.3% (10.0 μg L−1,n=7), 7.5 μg L−1, 0.11 mL, and 23 samples per hour, respectively. The method developed was successfully applied to beer samples and recovery tests, with recovery ranging from 80% to 100%.

A Simple Automated Method for the Determination of Nitrate and Nitrite in Infant Formula and Milk Powder Using Sequential Injection Analysis

A fast and efficient automated method using a sequential injection analysis (SIA) system, based on the Griess, reaction was developed for the determination of nitrate and nitrite in infant formulas and milk powder. The system enables to mix a measured amount of sample (previously constituted in the liquid form and deproteinized) with the chromogenic reagent to produce a colored substance whose absorbance was recorded. For nitrate determination, an on-line prereduction step was added by passing the sample through a Cd minicolumn. The system was controlled from a PC by means of a user-friendly program. Figures of merit include linearity (r2> 0.999 for both analytes), limits of detection (0.32 mg kg-1NO3-N, and 0.05 mg kg-1NO2-N), and precision (sr%) 0.8–3.0. Results were statistically in good agreement with those obtained with the reference ISO-IDF method. The sampling frequency was 30 hour-1(nitrate) and 80 hour-1(nitrite) when performed separately.

An Environmental Friendly Procedure for Photometric Determination of Hypochlorite in Tap Water Employing a Miniaturized Multicommuted Flow Analysis Setup

A photometric procedure for the determination ofClO-in tap water employing a miniaturized multicommuted flow analysis setup and an LED-based photometer is described. The analytical procedure was implemented using leucocrystal violet (LCV; 4,4′,4′′-methylidynetris (N,N-dimethylaniline), C25H31N3) as a chromogenic reagent. Solenoid micropumps employed for solutions propelling were assembled together with the photometer in order to compose a compact unit of small dimensions. After control variables optimization, the system was applied for the determination ofClO-in samples of tap water, and aiming accuracy assessment samples were also analyzed using an independent method. Applying the pairedt-test between results obtained using both methods, no significant difference at the 95% confidence level was observed. Other useful features include low reagent consumption, 2.4 μg of LCV per determination, a linear response ranging from 0.02 up to 2.0 mg L−1 ClO-, a relative standard deviation of 1.0% (n=11) for samples containing 0.2 mg L−1 ClO-, a detection limit of 6.0 μg L−1 ClO-, a sampling throughput of 84 determinations per hour, and a waste generation of 432 μL per determination.

A LabVIEW-Based Virtual Instrument System for Laser-Induced Fluorescence Spectroscopy

We report the design and operation of a Virtual Instrument (VI) system based on LabVIEW 2009 for laser-induced fluorescence experiments. This system achieves synchronous control of equipment and acquisition of real-time fluorescence data communicating with a single computer via GPIB, USB, RS232, and parallel ports. The reported VI system can also accomplish data display, saving, and analysis, and printing the results. The VI system performs sequences of operations automatically, and this system has been successfully applied to obtain the excitation and dispersion spectra ofα-methylnaphthalene. The reported VI system opens up new possibilities for researchers and increases the efficiency and precision of experiments. The design and operation of the VI system are described in detail in this paper, and the advantages that this system can provide are highlighted.

Synthesis and Physical Properties of Estolide Ester Using Saturated Fatty Acid and Ricinoleic Acid

A study was conveyed to produce estolide ester using ricinoleic acid as the backbone. The ricinoleic acid reacted with saturated fatty acid from C8–C18. These reactions were conducted under vacuum at 60°C for 24 h without solvent. The reaction used acid catalyst, sulphuric acid. The new saturate ricinoleic estolide esters show superior low-temperature properties (−52 ± 0.08°C) and high flash point (>300°C). The yield of the neat estolide esters ranged from 52% to 96%. The viscosity range was 51 ± 0.08 to 86 ± 0.01 cp. These new saturated estolide esters were also compared with saturated branched estolide esters.

Rapid and Automated Analytical Methods for Redox Species Based on Potentiometric Flow Injection Analysis Using Potential Buffers

Two analytical methods, which prove the utility of a potentiometric flow injection technique for determining various redox species, based on the use of some redox potential buffers, are reviewed. The first is a potentiometric flow injection method in which a redox couple such as Fe(III)-Fe(II), Fe-Fe(CN), and bromide-bromine and a redox electrode or a combined platinum-bromide ion selective electrode are used. The analytical principle and advantages of the method are discussed, and several examples of its application are reported. Another example is a highly sensitive potentiometric flow injection method, in which a large transient potential change due to bromine or chlorine as an intermediate, generated during the reaction of the oxidative species with an Fe(III)-Fe(II) potential buffer containing bromide or chloride, is utilized. The analytical principle and details of the proposed method are described, and examples of several applications are described. The determination of trace amounts of hydrazine, based on the detection of a transient change in potential caused by the reaction with a Ce(IV)-Ce(III) potential buffer, is also described.

Flow-Injection Preconcentration of Chloramphenicol Using Molecularly Imprinted Polymer for HPLC Determination in Environmental Samples

The residue of antibiotic chloramphenicol (CAP) is important issue for food quality control and also for the environmental monitoring. It is banned for use in food-producing animals and has very limited use in human medicine, because of its severe impact on human health. Determination of trace level of CAP in environmental samples requires a very sensitive analytical method and efficient preconcentration procedure. CAP can be efficiently preconcentrated in flow-injection system using flow-through reactor packed with molecularly imprinted polymer (MIP), but determination of CAP in eluate from MIP requires the application of chromatographic separation, which was made in reversed-phase HPLC system with UV detection. In optimized conditions the limit of detection for 100 mL sample in HPLC with offline preconcentration on MIP was evaluated as 0.66 mg/L. In hyphenated FIA-HPLC system with zone sampling the LOD for developed method was evaluated as 15 ng/L, which indicates the possibility of using it for analysis of environmental samples.

Automatic Discrimination of the Geographical Origins of Milks by Excitation-Emission Fluorescence Spectrometry and Chemometrics

This paper presents the automatic discrimination of geographical origins of milks from Western Yunnan Plateau areas and eastern China by excitation-emission fluorescence spectrometry and chemometrics. Genuine plateau milks (n=60) and milks from eastern China (n=89) are scanned in the regions of 180–300 nm for excitation and 200–800 nm for emission. Different options of data analysis are investigated and compared in terms of their performance in discriminating milks of different geographical origins: (1) two-way partial least squares discriminant analysis (PLSDA) based on excitation and emission spectra, respectively; (2) two-way PLSDA based on fusion of excitation and emission spectra; (3) three-way PLSDA based on excitation-emission matrix spectra. The two-way PLSDA methods with excitation spectra, emission spectra, and fusion of excitation and emission spectra correctly classify 91.3%, 88.6%, and 95.3% of the milk samples, respectively; while the total accuracy of three-way PLSDA is 96.0%. The results demonstrate the two-way data combining excitation and emission spectra are sufficient to characterize and identify the plateau milks. Considering both model accuracy and the analytical time required, two-way PLS-DA with fusion of excitation and emission spectra is recommended as a reliable and quick method to discriminate plateau milks from ordinary milks.

Design of a Flow-Through Voltammetric Sensor Based on an Antimony-Modified Silver Electrode for Determining Lithol Rubine B in Cosmetics

Lithol Rubine B (LRB; the disodium salt of 3-hydroxy-4-[(4-methyl-2-sulfophenyl) azo]-2-naphthalenecarboxylic acid) was detected using high-performance liquid chromatography with an electrochemical (antimony film on silver) detector (HPLC-ECD). For direct current (DC) mode, with the current at a constant potential, and measurements with suitable experimental parameters, a linear concentration from 0.125 to 1.80 μg/mL was found. The detection limit of our method was approximately 2.0 ng/mL. An antimony-modified silver detector was used to demonstrate that LRB is electrochemically reduced in acidic media and to analyze commercial cosmetics to determine their LRB content. Findings using HPLC-ECD and HPLC with an ultraviolet detector were comparable.