Journal of Analytical Methods in Chemistry The latest articles from Hindawi Publishing Corporation © 2015 , Hindawi Publishing Corporation . All rights reserved. Analysis of Reaction between -Lipoic Acid and 2-Chloro-1-methylquinolinium Tetrafluoroborate Used as a Precolumn Derivatization Technique in Chromatographic Determination of -Lipoic Acid Sun, 04 Oct 2015 12:44:16 +0000 The present study offers results of analysis concerning the course of reaction between reduced α-lipoic acid (LA) and 2-chloro-1-methylquinolinium tetrafluoroborate (CMQT). In water environments, the reaction between CMQT and hydrophilic thiols proceeds very rapidly and the resultant products are stable. For the described analysis, optimum reaction conditions, such as concentration of the reducing agent, environment pH, and concentration of the reagent were carefully selected. The spectrophotometric assay was carried out measuring absorbance at  nm (i.e., the spectral band of the obtained reaction product). Furthermore, the calibration curve of lipoic acid was registered. It was concluded that the Lambert-Beer law was observed within the range 1–10 μmol L−1. Later, the reaction between LA and CMQT was used as precolumn derivatization in a chromatographic determination of the lipoic acid in the range 2.5–50 μmol L−1. Practical applicability of the designed methods was evaluated by determining lipoic acid in Revitanerv pharmaceutical preparation which contains 300 mg LA in a single capsule. The error of the determination did not exceed 0.5% in relation to the declared value. Magdalena Godlewska, Angelika Odachowska, Monika Turkowicz, and Joanna Karpinska Copyright © 2015 Magdalena Godlewska et al. All rights reserved. Detection of Gelatin Adulteration in Traditional Chinese Medicine: Analysis of Deer-Horn Glue by Rapid-Resolution Liquid Chromatography-Triple Quadrupole Mass Spectrometry Sun, 04 Oct 2015 11:12:06 +0000 Simultaneous identification of donkey-hide gelatin and bovine-hide gelatin in deer-horn glue was established by rapid-resolution liquid chromatography-triple quadrupole mass spectrometry. Water containing 1% NH4HCO3 was used for sample dissolution and trypsin was used for hydrolysis of the gelatins. After separation by a SB-C18 reversed-phase analytical column, collagen marker peptides were detected by mass spectrometry in positive electrospray ionization mode with multiple reaction monitoring. The method was specific, precise and reliable, and suitable for detection of adulterants derived from donkey-hide gelatin and bovine-hide gelatin in deer-horn glue. Jia Chen, Xian-Long Cheng, Feng Wei, Qian-Qian Zhang, Ming-Hua Li, and Shuang-Cheng Ma Copyright © 2015 Jia Chen et al. All rights reserved. A Virtual Instrument System for Determining Sugar Degree of Honey Sun, 04 Oct 2015 08:55:23 +0000 This study established a LabVIEW-based virtual instrument system to measure optical activity through the communication of conventional optical instrument with computer via RS232 port. This system realized the functions for automatic acquisition, real-time display, data processing, results playback, and so forth. Therefore, it improved accuracy of the measurement results by avoiding the artificial operation, cumbersome data processing, and the artificial error in optical activity measurement. The system was applied to the analysis of the batch inspection on the sugar degree of honey. The results obtained were satisfying. Moreover, it showed advantages such as friendly man-machine dialogue, simple operation, and easily expanded functions. Qijun Wu and Xun Gong Copyright © 2015 Qijun Wu and Xun Gong. All rights reserved. Protective Effects of Intralipid and Caffeic Acid Phenethyl Ester on Nephrotoxicity Caused by Dichlorvos in Rats Sun, 04 Oct 2015 08:01:53 +0000 The protective effects of Caffeic Acid Phenethyl Ester (CAPE) and intralipid (IL) on nephrotoxicity caused by acute Dichlorvos (D) toxicity were investigated in this study. Forty-eight Wistar Albino rats were divided into 7 groups as follows: Control, D, CAPE, intralipid, D + CAPE, D + IL, and D + CAPE + IL. When compared to D group, the oxidative stress index (OSI) values were significantly lower in Control, CAPE, and D + IL + CAPE groups. When compared to D + IL + CAPE group, the TOS and OSI values were significantly higher in D group (). When mitotic cell counts were assessed in the renal tissues, it was found that mitotic cell count was significantly higher in the D group while it was lower in the D + CAPE, D + IL, and D + IL + CAPE groups when compared to the control group (). Also, immune reactivity showed increased apoptosis in D group and low profile of apoptosis in the D + CAPE group when compared to the Control group. The apoptosis level was significantly lower in D + IL + CAPE compared to D group () in the kidneys. As a result, we concluded that Dichlorvos can be used either alone or in combination with CAPE and IL as supportive therapy or as facilitator for the therapeutic effect of the routine treatment in the patients presenting with pesticide poisoning. Muhammet Murat Celik, Ayse Alp, Recep Dokuyucu, Ebru Zemheri, Seyma Ozkanli, Filiz Ertekin, Mehmet Yaldiz, Abdurrahman Akdag, Ozlem Ipci, and Serhat Toprak Copyright © 2015 Muhammet Murat Celik et al. All rights reserved. 1H HR-MAS NMR Spectroscopy and the Metabolite Determination of Typical Foods in Mediterranean Diet Thu, 01 Oct 2015 11:20:44 +0000 NMR spectroscopy has become an experimental technique widely used in food science. The experimental procedures that allow precise and quantitative analysis on different foods are relatively simple. For a better sensitivity and resolution, NMR spectroscopy is usually applied to liquid sample by means of extraction procedures that can be addressed to the observation of particular compounds. For the study of semisolid systems such as intact tissues, High-Resolution Magic Angle Spinning (HR-MAS) has received great attention within the biomedical area and beyond. Metabolic profiling and metabolism changes can be investigated both in animal organs and in foods. In this work we present a proton HR-MAS NMR study on the typical vegetable foods of Mediterranean diet such as the Protected Geographical Indication (PGI) cherry tomato of Pachino, the PGI Interdonato lemon of Messina, several Protected Designation of Origin (PDO) extra virgin olive oils from Sicily, and the Traditional Italian Food Product (PAT) red garlic of Nubia. We were able to identify and quantify the main metabolites within the studied systems that can be used for their characterization and authentication. Carmelo Corsaro, Domenico Mallamace, Sebastiano Vasi, Vincenzo Ferrantelli, Giacomo Dugo, and Nicola Cicero Copyright © 2015 Carmelo Corsaro et al. All rights reserved. Chemical Analysis of Suspected Unrecorded Alcoholic Beverages from the States of São Paulo and Minas Gerais, Brazil Thu, 01 Oct 2015 11:04:07 +0000 Our study analyzed 152 samples of alcoholic beverages collected from the states of São Paulo and Minas Gerais, Brazil, using gas chromatography with flame ionization detection (GC-FID) and mass spectrometry (GC-MS), Fourier transform infrared spectroscopy (FT-IR), and inductively coupled plasma atomic emission spectrometry (ICP-AES). The methanol content varied from 20 to 180 ppm in 28 samples, and the limit of the accepted level of 200 ppm was exceeded in only one sample. High content of cyanide derivatives and ethyl carbamate, above the accepted level of 150 ppb, was observed in 109 samples. Carbonyl compounds were also observed in 111 samples, showing hydroxy 2-propanone, 4-methyl-4-hepten-3-one, furfural, and 2-hydroxyethylcarbamate as main constituents. Copper was found at concentrations above 5 ppm in 26 samples; the maximum value observed was 28 ppm. This work evaluated the human health risk associated with the poor quality of suspected unrecorded alcohols beverages. Giuseppina Negri, Julino Assunção Rodrigues Soares Neto, and Elisaldo Luiz de Araujo Carlini Copyright © 2015 Giuseppina Negri et al. All rights reserved. Determination of Polyphenols, Capsaicinoids, and Vitamin C in New Hybrids of Chili Peppers Thu, 01 Oct 2015 08:31:01 +0000 Six hybrids were subjected to chromatographic analyses by HPLC for the determination of phytochemicals such as capsaicinoid, polyphenol, and vitamin C. The dynamics of ripening of 4 of the hybrids were also characterised. Seven capsaicinoids could be separated and determined; the major compounds were nordihydrocapsaicin, capsaicin, and dihydrocapsaicin, while homocapsaicin and homodihydrocapsaicin derivatives were detected as minor constituents. Capsaicin content ranged between 95.5 ± 4.15 and 1610.2 ± 91.46 μg/g FW, and the highest value was found in Bandai (C. frutescens) at the green ripening stage. The major capsaicinoids had a decreasing tendency in Bandai and Chili 3735 hybrids, while no change was observed in Beibeihong and Lolo during ripening. Nine polyphenol compounds were detected including 8 flavonoids and a nonflavonoid compound in the pods of all hybrids. The major components were naringenin-diglucoside, catechin, and vanillic acid-derivative and luteolin-glucoside. Naringenin-diglucoside ranged from 93.5 ± 4.26 to 368.8 ± 30.77 μg/g FW. Except vanillic acid-derivative, dominant polyphenols increased or remained unchanged during ripening. As for vitamin C, its content tended to increase with the advance in ripening in all hybrids included in this study. The highest value of 3689.4 ± 39.50 μg/g FW was recorded in Fire Flame hybrid. Zsuzsa Nagy, Hussein Daood, Zsuzsanna Ambrózy, and Lajos Helyes Copyright © 2015 Zsuzsa Nagy et al. All rights reserved. Sesquiterpene Lactones from Artemisia Genus: Biological Activities and Methods of Analysis Thu, 01 Oct 2015 06:39:46 +0000 Sesquiterpene lactones are a large group of natural compounds, found primarily in plants of Asteraceae family, with over 5000 structures reported to date. Within this family, genus Artemisia is very well represented, having approximately 500 species characterized by the presence of eudesmanolides and guaianolides, especially highly oxygenated ones, and rarely of germacranolides. Sesquiterpene lactones exhibit a wide range of biological activities, such as antitumor, anti-inflammatory, analgesic, antiulcer, antibacterial, antifungal, antiviral, antiparasitic, and insect deterrent. Many of the biological activities are attributed to the α-methylene-γ-lactone group in their molecule which reacts through a Michael-addition with free sulfhydryl or amino groups in proteins and alkylates them. Due to the fact that most sesquiterpene lactones are thermolabile, less volatile compounds, they present no specific chromophores in the molecule and are sensitive to acidic and basic mediums, and their identification and quantification represent a difficult task for the analyst. Another problematic aspect is represented by the complexity of vegetal samples, which may contain compounds that can interfere with the analysis. Therefore, this paper proposes an overview of the methods used for the identification and quantification of sesquiterpene lactones found in Artemisia genus, as well as the optimal conditions for their extraction and separation. Bianca Ivanescu, Anca Miron, and Andreia Corciova Copyright © 2015 Bianca Ivanescu et al. All rights reserved. A Novel Computational Method to Reduce Leaky Reaction in DNA Strand Displacement Wed, 30 Sep 2015 16:35:54 +0000 DNA strand displacement technique is widely used in DNA programming, DNA biosensors, and gene analysis. In DNA strand displacement, leaky reactions can cause DNA signals decay and detecting DNA signals fails. The mostly used method to avoid leakage is cleaning up after upstream leaky reactions, and it remains a challenge to develop reliable DNA strand displacement technique with low leakage. In this work, we address the challenge by experimentally evaluating the basic factors, including reaction time, ratio of reactants, and ion concentration to the leakage in DNA strand displacement. Specifically, fluorescent probes and a hairpin structure reporting DNA strand are designed to detect the output of DNA strand displacement, and thus can evaluate the leakage of DNA strand displacement reactions with different reaction time, ratios of reactants, and ion concentrations. From the obtained data, mathematical models for evaluating leakage are achieved by curve derivation. As a result, it is obtained that long time incubation, high concentration of fuel strand, and inappropriate amount of ion concentration can weaken leaky reactions. This contributes to a method to set proper reaction conditions to reduce leakage in DNA strand displacement. Xin Li, Xun Wang, Tao Song, Wei Lu, Zhihua Chen, and Xiaolong Shi Copyright © 2015 Xin Li et al. All rights reserved. Hyperspectral Imaging Coupled with Random Frog and Calibration Models for Assessment of Total Soluble Solids in Mulberries Mon, 14 Sep 2015 09:56:47 +0000 Chemometrics methods coupled with hyperspectral imaging technology in visible and near infrared (Vis/NIR) region (380–1030 nm) were introduced to assess total soluble solids (TSS) in mulberries. Hyperspectral images of 310 mulberries were acquired by hyperspectral reflectance imaging system (512 bands) and their corresponding TSS contents were measured by a Brix meter. Random frog (RF) method was used to select important wavelengths from the full wavelengths. TSS values in mulberry fruits were predicted by partial least squares regression (PLSR) and least-square support vector machine (LS-SVM) models based on full wavelengths and the selected important wavelengths. The optimal PLSR model with 23 important wavelengths was employed to visualise the spatial distribution of TSS in tested samples, and TSS concentrations in mulberries were revealed through the TSS spatial distribution. The results declared that hyperspectral imaging is promising for determining the spatial distribution of TSS content in mulberry fruits, which provides a reference for detecting the internal quality of fruits. Yan-Ru Zhao, Ke-Qiang Yu, and Yong He Copyright © 2015 Yan-Ru Zhao et al. All rights reserved. Paclobutrazol Residue Determination in Potato and Soil Using Low Temperature Partition Extraction and Ultrahigh Performance Liquid Chromatography Tandem Mass Spectrometry Thu, 10 Sep 2015 07:31:13 +0000 A simple, accurate, and highly sensitive analytical method was developed for determining the paclobutrazol residue in potato and soil, the dynamics dissipation in soil. Extraction was carried out by low temperature partitioning and analyzed by ultrahigh performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). For a favor extraction yield, the parameters such as temperature and solvent were optimized. The result showed that sample would be easily frozen and separated using acetonitrile under −20°C for 10 min. The limit of detection (LOD) was 0.5 μg/kg, and the limit of quantification (LOQ) was 2 and 5 μg/kg for potato and soil, respectively. The influence of paclobutrazol residue in potato was evaluated. The possible contamination of paclobutrazol from surface can be rinsed by distilled water or peeled off, but the paclobutrazol in potato harvest comes mainly from absorption and transport, which could not be removed by peeling. The half-life of paclobutrazol in soil was 20.64 days, and the residue was below 0.22 mg/kg on 50th day after spraying. According to the risk assessment with Need Maximum Daily Intake (NEDI) and Acceptable Daily Intake (ADI), a Maximum Residue Limit (MRL) of paclobutrazol in potato was recommended as 1.0 mg/kg. Hongcheng Liu, Tao Lin, Jia Mao, Huan Lu, Dongshun Yang, Jiliang Wang, and Qiwan Li Copyright © 2015 Hongcheng Liu et al. All rights reserved. Bioaccumulation of Antimony and Arsenic in Vegetables and Health Risk Assessment in the Superlarge Antimony-Mining Area, China Wed, 09 Sep 2015 09:55:16 +0000 Heavy metal pollution in soils caused by mining and smelting has attracted worldwide attention for its potential health risks to residents. This paper studies the concentrations and accumulations of Sb and As in both soils and vegetables and the human health risks of Sb and As in vegetables from Xikuangshan (XKS) Sb mine, Hunan, China. Results showed that the soils were severely polluted by Sb and As; Sb and As have significant positive correlation. Sb and As concentrations in vegetables were quite different: Coriandrum sativum L. was the highest in Sb, Allium fistulosum L. was the highest in As, and Brassica pekinensis L. was the lowest in both Sb and As; Daucus carota L. and Coriandrum sativum L. showed advantage in accumulating Sb and As; Coriandrum sativum L. had higher capacity of redistributing Sb and As within the plant. Health risk assessment results showed that the hazard quotient (HQ) values of Sb and As in vegetables were in the ranges of 1.61–3.33 and 0.09–0.39, respectively; the chronic daily intake (CDI) and hazard quotient (HQ) values of Sb were over the safe limit recommended by FAO and WHO, indicating that long-term consumption of vegetables from the surrounding soils of XKS mine may bring health risks to residents. Defang Zeng, Saijun Zhou, Bozhi Ren, and Tengshu Chen Copyright © 2015 Defang Zeng et al. All rights reserved. A Novel Analytical Method for Trace Ammonium in Freshwater and Seawater Using 4-Methoxyphthalaldehyde as Fluorescent Reagent Tue, 01 Sep 2015 11:35:25 +0000 A novel fluorescent reagent for determination of ammonium, 4-methoxyphthalaldehyde (MOPA), was successfully synthesized in this study. Under alkaline conditions, MOPA could reacted with ammonium rapidly at room temperature, producing fluorescent substance which had maximum excitation at 370 nm and emission wavelength at 454 nm. Based on this, a novel fluorescence analysis method was established for the determination of trace ammonium in natural water. Experimental parameters including reagent concentration, pH, reaction equilibrium time, and metal ions masking agent were optimized. The results showed that the optimized MOPA concentration was 0.12 g/L, pH was in the range of 11.2–12.0, and sulfite concentration was 0.051 g/L, respectively. Metal ions masking agent had no obvious effect on the fluorescence signal. With the reaction time of 15 minutes, linear range of this method was between 0.025 and 0.300 μmol/L, and the method detecting limit was 0.0058 μmol/L. The matrix recovery of the proposed method was in the range of 93.6–108.1%. Compared with the OPA method, this method was much more sensitive and rapid without the interference of background peak and would be more suitable for developing a portable fluorescence detection system. Ying Liang, Yingming Pan, Qing Guo, Hongzhi Hu, Chancui Wu, and Qian Zhang Copyright © 2015 Ying Liang et al. All rights reserved. Rapid Discrimination for Traditional Complex Herbal Medicines from Different Parts, Collection Time, and Origins Using High-Performance Liquid Chromatography and Near-Infrared Spectral Fingerprints with Aid of Pattern Recognition Methods Sun, 09 Aug 2015 06:04:25 +0000 As an effective method, the fingerprint technique, which emphasized the whole compositions of samples, has already been used in various fields, especially in identifying and assessing the quality of herbal medicines. High-performance liquid chromatography (HPLC) and near-infrared (NIR), with their unique characteristics of reliability, versatility, precision, and simple measurement, played an important role among all the fingerprint techniques. In this paper, a supervised pattern recognition method based on PLSDA algorithm by HPLC and NIR has been established to identify the information of Hibiscus mutabilis L. and Berberidis radix, two common kinds of herbal medicines. By comparing component analysis (PCA), linear discriminant analysis (LDA), and particularly partial least squares discriminant analysis (PLSDA) with different fingerprint preprocessing of NIR spectra variables, PLSDA model showed perfect functions on the analysis of samples as well as chromatograms. Most important, this pattern recognition method by HPLC and NIR can be used to identify different collection parts, collection time, and different origins or various species belonging to the same genera of herbal medicines which proved to be a promising approach for the identification of complex information of herbal medicines. Haiyan Fu, Yao Fan, Xu Zhang, Hanyue Lan, Tianming Yang, Mei Shao, and Sihan Li Copyright © 2015 Haiyan Fu et al. All rights reserved. Effects of Oxygen Element and Oxygen-Containing Functional Groups on Surface Wettability of Coal Dust with Various Metamorphic Degrees Based on XPS Experiment Wed, 15 Jul 2015 13:54:59 +0000 To investigate the difference of surface oxygen element and oxygen-containing functional groups among coal dusts with different metamorphic degrees and their influence on surface wettability, a series of X-ray photoelectron spectroscopy experiments on 6 coal samples are carried out. The result demonstrates that the O/C ratio of coal surface shows an overall increasing trend compared with the result of its elements analysis. As the metamorphic degree increases, the O/C ratio on the surface gradually declines and the hydrophilic groups tend to fall off from coal surface. It could be found that different coals show different surface distributions of carboxyl and hydroxyl which are considered as the greatest promoter to the wettability of coal surface. With the change of metamorphic degree, the distribution of ether group is irregular while the carbonyl distribution keeps stable. In general, as the metamorphic degree goes higher, the content of oxygen-containing polar group tends to reduce. According to the measurement results, the contact angle is negatively related to the content of oxygen element, surface oxygen, and polar groups. In addition, compared with surface oxygen content, the content of oxygen-containing polar group serves as a more reasonable indicator of coal dust wettability. Gang Zhou, Cuicui Xu, Weimin Cheng, Qi Zhang, and Wen Nie Copyright © 2015 Gang Zhou et al. All rights reserved. Comparison of Mineral Element Content in a Functional Food Maca (Lepidium meyenii Walp.) from Asia and South America Wed, 08 Jul 2015 09:59:09 +0000 Contents of eight mineral elements in maca (Lepidium meyenii Walp.) from China and Peru were determined by inductively coupled plasma optical emission spectroscopy. Cu contents in maca samples from China (2.5–31 mg kg−1 dry weight, dw) were higher than the samples from Peru (<2.1 mg kg−1 dw). Na in two samples from China was found to be significantly of high content (2400 and 2600 mg kg−1 dw). The contents (mg kg−1 dw) of B, Co, Cr, Li, Ni, and Zn were, respectively, 8.1–21, <0.023, <1.1~3.5, 0.020–0.17, 0.085–4.5, and 10–39 for the samples from China, while being 6.6–12, <0.023, <1.1~2.3, 0.035–0.063, 0.68–1.7, and 27–39 for the samples from Peru. Ji Zhang, Han-Mo Wang, Yan-Li Zhao, Zhi-Tian Zuo, Yuan-Zhong Wang, and Hang Jin Copyright © 2015 Ji Zhang et al. All rights reserved. Recent Developments in the Speciation and Determination of Mercury Using Various Analytical Techniques Sun, 05 Jul 2015 12:40:29 +0000 This paper reviews the speciation and determination of mercury by various analytical techniques such as atomic absorption spectrometry, voltammetry, inductively coupled plasma techniques, spectrophotometry, spectrofluorometry, high performance liquid chromatography, and gas chromatography. Approximately 126 research papers on the speciation and determination of mercury by various analytical techniques published in international journals since 2013 are reviewed. Lakshmi Narayana Suvarapu and Sung-Ok Baek Copyright © 2015 Lakshmi Narayana Suvarapu and Sung-Ok Baek. All rights reserved. Optimization of a CUPRAC-Based HPLC Postcolumn Assay and Its Applications for Ginkgo biloba L. Extracts Sun, 05 Jul 2015 11:11:27 +0000 The aim of the present work was to improve and validate the HPLC-CUPRAC postcolumn method for the evaluation of active antioxidant markers from the acetonic extracts of Ginkgo biloba leaves. Improvement of the HPLC online assay was performed by evaluating the suitable loop temperature, the reaction loop length, and the impact of flow rate. Separation of the analytes was performed by the HPLC method on an ACE C18 analytical column using a gradient elution program. The separated antioxidant markers in the extracts reacted with copper(II)-neocuproine (Cu(II)-Nc) reagent in the postcolumn reaction coil. The reagent was reduced by antioxidants to the copper(I)-neocuproine (Cu(I)-Nc) chelate with a maximum absorption at 450 nm. Validation experiments confirmed sufficient precision, sensitivity, and effectiveness of the corresponding method, which could be used for further evaluations of active antioxidant compounds in similar plant materials. Laura Rimkiene, Liudas Ivanauskas, Asta Kubiliene, Konradas Vitkevicius, Guoda Kiliuviene, and Valdas Jakstas Copyright © 2015 Laura Rimkiene et al. All rights reserved. Quality Degradation of Chinese White Lotus Seeds Caused by Dampening during Processing and Storage: Rapid and Nondestructive Discrimination Using Near-Infrared Spectroscopy Sun, 28 Jun 2015 09:49:40 +0000 Dampening during processing or storage can largely influence the quality of white lotus seeds (WLS). This paper investigated the feasibility of using near-infrared (NIR) spectroscopy and chemometrics for rapid and nondestructive discrimination of the dampened WLS. Regular () and dampened () WLS objects were collected from five main producing areas and NIR reflectance spectra (4000–12000 cm−1) were measured for bare kernels. The influence of spectral preprocessing methods, including smoothing, taking second-order derivatives (D2), and standard normal variate (SNV), on partial least squares discrimination analysis (PLSDA) was compared to select the optimal data preprocessing method. A moving-window strategy was combined with PLSDA (MWPLSDA) to select the most informative wavelength intervals for classification. Based on the selected spectral ranges, the sensitivity, specificity, and accuracy were 0.927, 0.950, and 0.937 for SNV-MWPLSDA, respectively. Lu Xu, Hai-Yan Fu, Chen-Bo Cai, and Yuan-Bin She Copyright © 2015 Lu Xu et al. All rights reserved. Analysis of the Metals in Soil-Water Interface in a Manganese Mine Wed, 17 Jun 2015 08:06:36 +0000 In order to reveal the influence of the metals of soil-water interface in a manganese mine (Xiangtan, China), on local water environment, there are six kinds of metals (Mn, Ni, Cu, Zn, Cd, and Pb) characterized by measuring their concentration, correlation, source, and special distribution using principal component analysis, single factor, and Nemero comprehensive pollution index. The results showed that the corresponding average concentration was 0.3358, 0.045, 0.0105, 0.0148, 0.0067, and 0.0389 mg/L. The logarithmic concentration of Mn, Zn, and Pb was normal distribution. The correlation coefficients (between Mn and Pb, Mn and Zn, Mn and Ni, Cu and Zn, Cu and Pb, and Zn and Cd) were found to range from 0.5 to 0.6, and those between Cu and Ni and Cu and Cd were below 0.3. It was found that Zn and Mn pollution were caused primarily by ore mining, mineral waste transportation, tailing slag, and smelting plants, while Cu and Ni mainly originate from the mining industry activities and the traffic transportation in the mining area. In addition, the Cd was considered to be produced primarily from the agricultural or anthropogenic activities. The pollution indexes indicated that metal pollution degree was different in soil-water interface streams as listed in increasing order of pollution level as Zn > Ni > Cu > Pb > Mn > Cd. For all of the pollution of the soil-water interface streams, there was moderate metal pollution but along the eastern mine area the pollution seemed to get more serious. There was only a small amount of soil-water interface streams not contaminated by the metals. Bozhi Ren, Qian Wang, Yangbo Chen, Wenjie Ding, and Xie Zheng Copyright © 2015 Bozhi Ren et al. All rights reserved. Relevance of Toxicity Assessment in Wastewater Treatments: Case Study—Four Fenton Processes Applied to the Mineralization of C.I. Acid Red 14 Mon, 08 Jun 2015 11:20:26 +0000 Fenton and Fenton-like processes, both in homogeneous and heterogeneous phases, have been applied to an aqueous solution containing the dye AR 14 in order to study the mineralization and toxicity of the solutions generated after color elimination. The mineralization of AR 14 occurred slower than the decolorization. The Microtox analysis of the treated solutions showed low toxicity intrinsic to the chemicals used in the process rather than the degradation products obtained after the treatment of the dye solution. The dye degradation for the Fenton oxidation process was initially faster than for the Fenton-like process but after a short time, the four processes showed similar degradation yields. All processes have shown good results being the heterogeneous process the most convenient since the pH adjustment is not necessary, the catalyst is recovered and reused and the generation of contaminated sludge is avoided. Rajaa Idel-aouad, Manuel Valiente, Carmen Gutiérrez-Bouzán, Mercè Vilaseca, Abdlrani Yaacoubi, Boumediene Tanouti, and Montserrat López-Mesas Copyright © 2015 Rajaa Idel-aouad et al. All rights reserved. Content and Bioaccumulation of Nine Mineral Elements in Ten Mushroom Species of the Genus Boletus Thu, 04 Jun 2015 13:41:53 +0000 Concentrations and bioconcentration potential of nine elements (Ca, Cu, Fe, K, Mg, Mn, Na, P, and Zn) in ten species of wild edible Boletus and the corresponding underlying soils were analyzed. The analyses were performed using inductively coupled plasma atomic emission spectrophotometer. Boletus showed relative abundant contents of P, K, Fe, Mg, Ca, and Na and less of Zn, Cu, and Mn. Caps compared to stalks were enriched in P, K, Cu, Mg, and Zn, while stalks were enriched in Mn. The elements such as P and K were accumulated (), while Ca, Fe, Mg, Mn, and Na were excluded () in the fruiting bodies. The correlation analysis indicated high correlations between Cu, Mn, Ca, and Fe in the mushrooms as compared to the corresponding soils. Significant correlations were also obtained between Cu-P (), Fe-P (), and Zn-P () for caps and Cu-Mg (), Fe-Mg (), Zn-Mg (), and Zn-P () for stalks. The results of this study imply that ability of fungi to accumulate elements from substrate could be influenced by mushroom species and underlying soil substrates. Xue-Mei Wang, Ji Zhang, Tao Li, Yuan-Zhong Wang, and Hong-Gao Liu Copyright © 2015 Xue-Mei Wang et al. All rights reserved. Capillary Electrophoresis Single-Strand Conformational Polymorphisms as a Method to Differentiate Algal Species Tue, 26 May 2015 11:56:06 +0000 Capillary electrophoresis single-strand conformational polymorphism (CE-SSCP) was explored as a fast and inexpensive method to differentiate both prokaryotic (blue-green) and eukaryotic (green and brown) algae. A selection of two blue-green algae (Nostoc muscorum and Anabaena inaequalis), five green algae (Chlorella vulgaris, Oedogonium foveolatum, Mougeotia sp., Scenedesmus quadricauda, and Ulothrix fimbriata), and one brown algae (Ectocarpus sp.) were examined and CE-SSCP electropherogram “fingerprints” were compared to each other for two variable regions of either the 16S or 18S rDNA gene. The electropherogram patterns were remarkably stable and consistent for each particular species. The patterns were unique to each species, although some common features were observed between the different types of algae. CE-SSCP could be a useful method for monitoring changes in an algae species over time as potential shifts in species occurred. Alice Jernigan and Christa Hestekin Copyright © 2015 Alice Jernigan and Christa Hestekin. All rights reserved. Determination of Nicotine in Tobacco by Chemometric Optimization and Cation-Selective Exhaustive Injection in Combination with Sweeping-Micellar Electrokinetic Chromatography Tue, 26 May 2015 08:41:36 +0000 Nicotine is a potent chemical that excites the central nervous system and refreshes people. It is also physically addictive and causes dependence. To reduce the harm of tobacco products for smokers, a law was introduced that requires tobacco product containers to be marked with the amount of nicotine as well as tar. In this paper, an online stacking capillary electrophoresis (CE) method with cation-selective exhaustive injection sweeping-micellar electrokinetic chromatography (CSEI-sweeping-MEKC) is proposed for the optimized analysis of nicotine in tobacco. A higher conductivity buffer (160 mM phosphate buffer (pH 3)) zone was injected into the capillary, allowing for the analytes to be electrokinetically injected at a voltage of 15 kV for 15 min. Using 50 mM sodium dodecyl sulfate and 25% methanol in the sweeping buffer, nicotine was detected with high sensitivity. Thus, optimized conditions adapted from a chemometric approach provided a 6000-fold increase in the nicotine detection sensitivity using the CSEI-sweeping-MEKC method in comparison to normal CZE. The limits of detection were 0.5 nM for nicotine. The stacking method in combination with direct injection which matrix components would not interfere with assay performance was successfully applied to the detection of nicotine in tobacco samples. Yi-Hui Lin, Chia-Hsien Feng, Shih-Wei Wang, Po-Yun Ko, Ming-Hsun Lee, and Yen-Ling Chen Copyright © 2015 Yi-Hui Lin et al. All rights reserved. Applying 1H NMR Spectroscopy to Detect Changes in the Urinary Metabolite Levels of Chinese Half-Pipe Snowboarders after Different Exercises Mon, 25 May 2015 14:25:39 +0000 Monitoring physical training is important for the health and performance of athletes, and real-time assessment of fatigue is crucial to improve training efficiency. The relationship between key biomarkers and exercise has been reported. The aim of this study was to determine the effects of different levels of training exercises on the urine metabolome. 1H NMR-based metabolomics analysis was performed on urine samples from half-pipe snowboarders, and spectral profiles were subjected to PCA and PLS-DA. Our results show that metabolic profiles varied during different stages of exercises. Lactate, alanine, trimethylamine, malonate, taurine, and glycine levels decreased while TMAO and phenylalanine levels increased in the stage with higher amount and intensity of exercise. Although the amount of exercise was reduced in subsequent stage, no significant variations of metabolic profile were found. Metabolic changes induced by training level were analyzed with related metabolic pathway. Studying metabolome changes can provide a better understanding of the physiology of athletes and could aid in adjusting training. Fuqiu Wang, Jiao Han, Qing He, Zhufeng Geng, Zhiwei Deng, and Decai Qiao Copyright © 2015 Fuqiu Wang et al. All rights reserved. Ultra High Performance Liquid Chromatography Method for the Determination of Two Recently FDA Approved TKIs in Human Plasma Using Diode Array Detection Mon, 25 May 2015 13:21:21 +0000 Generally, tyrosine kinase inhibitors have narrow therapeutic window and large interpatient variability compared to intrapatient variability. In order to support its therapeutic drug monitoring, two fast and accurate methods were developed for the determination of recently FDA approved anticancer tyrosine kinase inhibitors, afatinib and ibrutinib, in human plasma using ultra high performance liquid chromatography coupled to PDA detection. Diclofenac sodium was used as internal standard. The chromatographic separation was achieved on an Acquity UPLC BEH C18 analytical column using a mobile phase combining ammonium formate buffer and acetonitrile at a constant flow rate of 0.4 mL/min using gradient elution mode. A µSPE (solid phase extraction) procedure, using Oasis MCX µElution plates, was processed and it gave satisfying and reproducible results in terms of extraction yields. Additionally, the methods were successfully validated using the accuracy profiles approach (β = 95% and acceptance limits = ±15%) over the ranges 5–250 ng/mL for afatinib and from 5 to 400 ng/mL for ibrutinib in human plasma. Marwa Fouad, Maxime Helvenstein, and Bertrand Blankert Copyright © 2015 Marwa Fouad et al. All rights reserved. Amine Analysis Using AlexaFluor 488 Succinimidyl Ester and Capillary Electrophoresis with Laser-Induced Fluorescence Tue, 19 May 2015 09:47:38 +0000 Fluorescent probes enable detection of otherwise nonfluorescent species via highly sensitive laser-induced fluorescence. Organic amines are predominantly nonfluorescent and are of analytical interest in agricultural and food science, biomedical applications, and biowarfare detection. Alexa Fluor 488 N-hydroxysuccinimidyl ester (AF488 NHS-ester) is an amine-specific fluorescent probe. Here, we demonstrate low limit of detection of long-chain (C9 to C18) primary amines and optimize AF488 derivatization of long-chain primary amines. The reaction was found to be equally efficient in all solvents studied (dimethylsulfoxide, ethanol, and N,N-dimethylformamide). While an organic base (N,N-diisopropylethylamine) is required to achieve efficient reaction between AF488 NHS-ester and organic amines with longer hydrophobic chains, high concentrations (>5 mM) result in increased levels of ethylamine and propylamine in the blank. Optimal incubation times were found to be >12 hrs at room temperature. We present an initial capillary electrophoresis separation for analysis using a simple micellar electrokinetic chromatography (MEKC) buffer consisting of 12 mM sodium dodecylsulfate (SDS) and 5 mM carbonate, pH 10. Limits of detection using the optimized labeling conditions and these separation conditions were 5–17 nM. The method presented here represents a novel addition to the arsenal of fluorescent probes available for highly sensitive analysis of small organic molecules. Christian G. Kendall, Amanda M. Stockton, Stephen Leicht, Heather McCaig, Shirley Chung, Valerie Scott, Fang Zhong, and Ying Lin Copyright © 2015 Christian G. Kendall et al. All rights reserved. Single-Round Patterned DNA Library Microarray Aptamer Lead Identification Thu, 14 May 2015 12:53:53 +0000 A method for identifying an aptamer in a single round was developed using custom DNA microarrays containing computationally derived patterned libraries incorporating no information on the sequences of previously reported thrombin binding aptamers. The DNA library was specifically designed to increase the probability of binding by enhancing structural complexity in a sequence-space confined environment, much like generating lead compounds in a combinatorial drug screening library. The sequence demonstrating the highest fluorescence intensity upon target addition was confirmed to bind the target molecule thrombin with specificity by surface plasmon resonance, and a novel imino proton NMR/2D NOESY combination was used to screen the structure for G-quartet formation. We propose that the lack of G-quartet structure in microarray-derived aptamers may highlight differences in binding mechanisms between surface-immobilized and solution based strategies. This proof-of-principle study highlights the use of a computational driven methodology to create a DNA library rather than a SELEX based approach. This work is beneficial to the biosensor field where aptamers selected by solution based evolution have proven challenging to retain binding function when immobilized on a surface. Jennifer A. Martin, Peter A. Mirau, Yaroslav Chushak, Jorge L. Chávez, Rajesh R. Naik, Joshua A. Hagen, and Nancy Kelley-Loughnane Copyright © 2015 Jennifer A. Martin et al. All rights reserved. A Stability-Indicating HPLC-DAD Method for Determination of Ferulic Acid into Microparticles: Development, Validation, Forced Degradation, and Encapsulation Efficiency Wed, 13 May 2015 09:39:49 +0000 A simple stability-indicating HPLC-DAD method was validated for the determination of ferulic acid (FA) in polymeric microparticles. Chromatographic conditions consisted of a RP C18 column (250 mm × 4.60 mm, 5 μm, 110 Å) using a mixture of methanol and water pH 3.0 (48 : 52 v/v) as mobile phase at a flow rate of 1.0 mL/min with UV detection at 320 nm. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of quantification, limit of detection, accuracy, precision, and robustness provided suitable results regarding all parameters investigated. The calibration curve was linear in the concentration range of 10.0–70.0 μg/mL with a correlation coefficient >0.999. Precision (intraday and interday) was demonstrated by a relative standard deviation lower than 2.0%. Accuracy was assessed by the recovery test of FA from polymeric microparticles (99.02% to 100.73%). Specificity showed no interference from the components of polymeric microparticles or from the degradation products derived from acidic, basic, and photolytic conditions. In conclusion, the method is suitable to be applied to assay FA as bulk drug and into polymeric microparticles and can be used for studying its stability and degradation kinetics. Jessica Mendes Nadal, Maria da Graça Toledo, Yasmine Mendes Pupo, Josiane Padilha de Paula, Paulo Vitor Farago, and Sandra Maria Warumby Zanin Copyright © 2015 Jessica Mendes Nadal et al. All rights reserved. Identification and Quality Assessment of Chrysanthemum Buds by CE Fingerprinting Thu, 30 Apr 2015 11:49:01 +0000 A simple and efficient fingerprinting method for chrysanthemum buds was developed with the aim of establishing a quality control protocol based on biochemical makeup. Chrysanthemum bud samples were successively extracted by water and alcohol. The fingerprints of the chrysanthemum buds samples were obtained using capillary electrophoresis and electrochemical detection (CE-ED) employing copper and carbon working electrodes to capture all of the chemical information. 10 batches of chrysanthemum buds were collected from different regions and various factories to establish the baseline fingerprint. The experimental data of 10 batches electropherogram buds by CE were analyzed by correlation coefficient and the included angle cosine methods. A standard chrysanthemum bud fingerprint including 24 common peaks was established, 12 from each electrode, which was successfully applied to identify and distinguish between chrysanthemum buds from 2 other chrysanthemum species. These results demonstrate that fingerprint analysis can be used as an important criterion for chrysanthemum buds quality control. Xiaoping Xing and Dan Li Copyright © 2015 Xiaoping Xing and Dan Li. All rights reserved.