Journal of Analytical Methods in Chemistry The latest articles from Hindawi Publishing Corporation © 2014 , Hindawi Publishing Corporation . All rights reserved. Quality Control of Natural Product Medicine and Nutrient Supplements 2014 Thu, 21 Aug 2014 09:38:39 +0000 Ying-Yong Zhao, Shuang-Qing Zhang, Feng Wei, Yu-Ming Fan, Feng Sun, and Shuhua Bai Copyright © 2014 Ying-Yong Zhao et al. All rights reserved. Stacking and Analysis of Melamine in Milk Products with Acetonitrile-Salt Stacking Technique in Capillary Electrophoresis Mon, 18 Aug 2014 00:00:00 +0000 Melamine was measured in real milk products with capillary electrophoresis (CE) based on acetonitrile-salt stacking (ASS) method. Real milk samples were deproteinized with acetonitrile at a final concentration of 60% (v/v) and then injected hydrodynamically at 50 mBar for 40.0 s. The optimized buffer contains 80.0 mmol/L pH 2.8 phosphates. Melamine could be detected within 20.0 min at +10 kV with a low limit of detection (LOD) of 0.03 μmol/L. Satisfactory reproducibility (inter- and intraday RSD% both for migration time and peak area was lower than 5.0%) and a wide linearity range of 0.05 μmol/L ~ 10.0 μmol/L were achieved. The proposed method was suitable for routine assay of MEL in real milk samples that was subjected to a simple treatment step. Yu Kong, Chong Wei, Zhanwu Hou, Zilong Wang, Jiaqiang Yuan, Jiang Yu, Yongxi Zhao, Yuhai Tang, and Meili Gao Copyright © 2014 Yu Kong et al. All rights reserved. Determination of Flavanones in Orange Juices Obtained from Different Sources by HPLC/DAD Thu, 07 Aug 2014 10:56:09 +0000 Flavanones (hesperidin, naringenin, naringin, and poncirin) in industrial, hand-squeezed orange juices and from fresh-in-squeeze machines orange juices were determined by HPLC/DAD analysis using a previously described liquid-liquid extraction method. Method validation including the accuracy was performed by using recovery tests. Samples (36) collected from different Brazilian locations and brands were analyzed. Concentrations were determined using an external standard curve. The limits of detection (LOD) and the limits of quantification (LOQ) calculated were 0.0037, 1.87, 0.0147, and 0.0066 mg 100 g−1 and 0.0089, 7.84, 0.0302, and 0.0200 mg 100 g−1 for naringin, hesperidin, poncirin, and naringenin, respectively. The results demonstrated that hesperidin was present at the highest concentration levels, especially in the industrial orange juices. Its average content and concentration range were 69.85 and 18.80–139.00 mg 100 g−1. The other flavanones showed the lowest concentration levels. The average contents and concentration ranges found were 0.019, 0.01–0.30, and 0.12 and 0.1–0.17, 0.13, and 0.01–0.36 mg 100 g−1, respectively. The results were also evaluated using the principal component analysis (PCA) multivariate analysis technique which showed that poncirin, naringenin, and naringin were the principal elements that contributed to the variability in the sample concentrations. Lidércia C. R. Cerqueira e Silva, Jorge M. David, Rafael dos S. Q. Borges, Sérgio L. C. Ferreira, Juceni P. David, Pedro S. dos Reis, and Roy E. Bruns Copyright © 2014 Lidércia C. R. Cerqueira e Silva et al. All rights reserved. The Therapeutic Effect of Zuogui Wan in Gestational Diabetes Mellitus Rats Tue, 22 Jul 2014 08:59:48 +0000 In this experiment, we established an animal model of gestational diabetes mellitus rats using streptozotocin. Using the rat model of GDM, the pregnant rats in 1-19d were divided into three groups: (1) Zuogui Wan gestational diabetes mellitus group (group I, ). Compared with gestational diabetes mellitus rats as the control group, Zuogui Wan can change the indexes of fasting blood glucose, body weight, total cholesterol, insulin, and metabolism cage index significantly in Zuogui Wan gestational diabetes mellitus group. We can conclude that Zuogui Wan has the therapeutic effect on gestational diabetes mellitus. Yuwei Wang, Qianjin Feng, Xin Niu, Xinshe Liu, Kaixia Xu, Xiangzhu Yang, Huifeng Wang, and Qiuju Li Copyright © 2014 Yuwei Wang et al. All rights reserved. Quantitative Analysis of Adulterations in Oat Flour by FT-NIR Spectroscopy, Incomplete Unbalanced Randomized Block Design, and Partial Least Squares Sun, 20 Jul 2014 11:51:04 +0000 This paper developed a rapid and nondestructive method for quantitative analysis of a cheaper adulterant (wheat flour) in oat flour by NIR spectroscopy and chemometrics. Reflectance FT-NIR spectra in the range of 4000 to 12000 cm−1 of 300 oat flour objects adulterated with wheat flour were measured. The doping levels of wheat flour ranged from 5% to 50% (w/w). To ensure the generalization performance of the method, both the oat and the wheat flour samples were collected from different producing areas and an incomplete unbalanced randomized block (IURB) design was performed to include the significant variations that may be encountered in future samples. Partial least squares regression (PLSR) was used to develop calibration models for predicting the levels of wheat flour. Different preprocessing methods including smoothing, taking second-order derivative (D2), and standard normal variate (SNV) transformation were investigated to improve the model accuracy of PLS. The root mean squared error of Monte Carlo cross-validation (RMSEMCCV) and root mean squared error of prediction (RMSEP) were 1.921 and 1.975 (%, w/w) by D2-PLS, respectively. The results indicate that NIR and chemometrics can provide a rapid method for quantitative analysis of wheat flour in oat flour. Ning Wang, Xingxiang Zhang, Zhuo Yu, Guodong Li, and Bin Zhou Copyright © 2014 Ning Wang et al. All rights reserved. Automated System for Kinetic Analysis of Particle Size Distributions for Pharmaceutically Relevant Systems Wed, 16 Jul 2014 14:15:37 +0000 Detailing the kinetics of particle formation for pharmaceutically relevant solutions is challenging, especially when considering the combination of formulations, containers, and timescales of clinical importance. This paper describes a method for using commercial software Automate with a stream-selector valve capable of sampling container solutions from within an environmental chamber. The tool was built to monitor changes in particle size distributions via instrumental particle counters but can be adapted to other solution-based sensors. The tool and methodology were demonstrated to be highly effective for measuring dynamic changes in emulsion globule distributions as a function of storage and mixing conditions important for parenteral nutrition. Higher levels of agitation induced the fastest growth of large globules (≥5 μm) while the gentler conditions actually showed a decrease in the number of these large globules. The same methodology recorded calcium phosphate precipitation kinetics as a function of [Ca2+] and pH. This automated system is readily adaptable to a wide range of pharmaceutically relevant systems where the particle size is expected to vary with time. This instrumentation can dramatically reduce the time and resources needed to probe complex formulation issues while providing new insights for monitoring the kinetics as a function of key variables. John-Bruce D. Green, Phillip W. Carter, Yingqing Zhang, Dipa Patel, Priyanka Kotha, and Thomas Gonyon Copyright © 2014 John-Bruce D. Green et al. All rights reserved. Rapid Discrimination of the Geographical Origins of an Oolong Tea (Anxi-Tieguanyin) by Near-Infrared Spectroscopy and Partial Least Squares Discriminant Analysis Thu, 26 Jun 2014 00:00:00 +0000 This paper focuses on a rapid and nondestructive way to discriminate the geographical origin of Anxi-Tieguanyin tea by near-infrared (NIR) spectroscopy and chemometrics. 450 representative samples were collected from Anxi County, the original producing area of Tieguanyin tea, and another 120 Tieguanyin samples with similar appearance were collected from unprotected producing areas in China. All these samples were measured by NIR. The Stahel-Donoho estimates (SDE) outlyingness diagnosis was used to remove the outliers. Partial least squares discriminant analysis (PLSDA) was performed to develop a classification model and predict the authenticity of unknown objects. To improve the sensitivity and specificity of classification, the raw data was preprocessed to reduce unwanted spectral variations by standard normal variate (SNV) transformation, taking second-order derivatives (D2) spectra, and smoothing. As the best model, the sensitivity and specificity reached 0.931 and 1.000 with SNV spectra. Combination of NIR spectrometry and statistical model selection can provide an effective and rapid method to discriminate the geographical producing area of Anxi-Tieguanyin. Si-Min Yan, Jun-Ping Liu, Lu Xu, Xian-Shu Fu, Hai-Feng Cui, Zhen-Yu Yun, Xiao-Ping Yu, and Zi-Hong Ye Copyright © 2014 Si-Min Yan et al. All rights reserved. Quantification of Photocyanine in Human Serum by High-Performance Liquid Chromatography-Tandem Mass Spectrometry and Its Application in a Pharmacokinetic Study Tue, 24 Jun 2014 00:00:00 +0000 Photocyanine is a novel anticancer drug. Its pharmacokinetic study in cancer patients is therefore very important for choosing doses, and dosing intervals in clinical application. A rapid, selective and sensitive high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed and validated for the determination of photocyanine in patient serum. Sample preparation involved one-step protein precipitation by adding methanol and N,N-dimethyl formamide to 0.1 mL serum. The detection was performed on a triple quadrupole tandem mass spectrometer operating in multiple reaction-monitoring (MRM) mode. Each sample was chromatographed within 7 min. Linear calibration curves were obtained for photocyanine at a concentration range of 20–2000 ng/mL (), with the lower limit of quantification (LLOQ) being 20 ng/mL. The intrabatch accuracy ranged from 101.98% to 107.54%, and the interbatch accuracy varied from 100.52% to 105.62%. Stability tests showed that photocyanine was stable throughout the analytical procedure. This study is the first to utilize the HPLC-MS/MS method for the pharmacokinetic study of photocyanine in six cancer patients who had received a single dose of photocyanine (0.1 mg/kg) administered intravenously. Bing-Tian Bi, Ben-Yan Zou, Li-Ting Deng, Jing Zhan, Hai Liao, Kun-Yao Feng, and Su Li Copyright © 2014 Bing-Tian Bi et al. All rights reserved. Quasireversible Process of Dopamine on Copper-Nickel Hydroxide Composite/Nitrogen Doped Graphene/Nafion Modified GCE and Its Electrochemical Application Mon, 16 Jun 2014 12:21:11 +0000 Cu-Ni(OH)2/N-GR/Nafion/GCE has been prepared by electrodeposition and activation with NaOH. The proposed modified GCE was studied by electrochemical methods. It is found that dopamine shows favorable redox cyclic voltammetric response on the proposed modified GCE with peak separation of 25 mV and large current compared with on single-component modified GCE. The kinetic of electrode process has also been investigated with rate constant of 6.618 × 10−3 cm/s, which can be deduced to be a quasireversible or near-reversible process. The proposed method has been used for DA detection with linear range of 1.0 × 10−7 mol/L to 4.6 × 10−5 mol/L, and the detection limit is 3.3 × 10−8 mol/L. The proposed method has favorable stability and reproducibility and has also been used to determine DA in simulated samples and DA injections with favorable recoveries of 98.4% to 102.6%. Chuan-yin Liu, Zhong-yong Liu, Rong Peng, and Zhi-cheng Zhong Copyright © 2014 Chuan-yin Liu et al. All rights reserved. Chemistry of Medicinal Plants, Foods, and Natural Products Wed, 04 Jun 2014 09:29:37 +0000 Shixin Deng, Shao-Nong Chen, and Jian Yang Copyright © 2014 Shixin Deng et al. All rights reserved. Study on the Effect of Electrochemical Dechlorination Reduction of Hexachlorobenzene Using Different Cathodes Wed, 04 Jun 2014 06:51:24 +0000 Hexachlorobenzene (HCB) is a persistent organic pollutant and poses great threat on ecosystem and human health. In order to investigate the degradation law of HCB, a RuO2/Ti material was used as the anode, meanwhile, zinc, stainless steel, graphite, and RuO2/Ti were used as the cathode, respectively. The gas chromatography (GC) was used to analyze the electrochemical products of HCB on different cathodes. The results showed that the cathode materials significantly affected the dechlorination efficiency of HCB, and the degradation of HCB was reductive dechlorination which occurred only on the cathode. During the reductive process, chlorine atoms were replaced one by one on various intermediates such as pentachlorobenzene, tetrachlorobenzene, and trichlorobenzene occurred; the trichlorobenzene was obtained when zinc was used as cathode. The rapid dechlorination of HCB suggested that the electrochemical method using zinc or stainless steel as cathode could be used for remediation of polychlorinated aromatic compounds in the environment. The dechlorination approach of HCB by stainless steel cathode could be proposed. Yingru Wang and Xiaohua Lu Copyright © 2014 Yingru Wang and Xiaohua Lu. All rights reserved. Comparability of a Three-Dimensional Structure in Biopharmaceuticals Using Spectroscopic Methods Thu, 22 May 2014 15:47:29 +0000 Protein structure depends on weak interactions and covalent bonds, like disulfide bridges, established according to the environmental conditions. Here, we present the validation of two spectroscopic methodologies for the measurement of free and unoxidized thiols, as an attribute of structural integrity, using 5,5′-dithionitrobenzoic acid (DTNB) and DyLight Maleimide (DLM) as derivatizing agents. These methods were used to compare Rituximab and Etanercept products from different manufacturers. Physicochemical comparability was demonstrated for Rituximab products as DTNB showed no statistical differences under native, denaturing, and denaturing-reducing conditions, with Student’s -test values of 0.6233, 0.4022, and 0.1475, respectively. While for Etanercept products no statistical differences were observed under native () and denaturing conditions (), denaturing-reducing conditions revealed cysteine contents of 98% and 101%, towards the theoretical value of 58, for the evaluated products from different Etanercept manufacturers. DLM supported equality between Rituximab products under native () and denaturing conditions (), but showed statistical differences among Etanercept products under native conditions (). DLM suggested that Infinitam has fewer exposed thiols than Enbrel, although DTNB method, circular dichroism (CD), fluorescence (TCSPC), and activity (TNFα neutralization) showed no differences. Overall, this data revealed the capabilities and drawbacks of each thiol quantification technique and their correlation with protein structure. Víctor Pérez Medina Martínez, Mario E. Abad-Javier, Alexis J. Romero-Díaz, Francisco Villaseñor-Ortega, Néstor O. Pérez, Luis F. Flores-Ortiz, and Emilio Medina-Rivero Copyright © 2014 Víctor Pérez Medina Martínez et al. All rights reserved. Simultaneous Quantification of Ten Active Components in Traditional Chinese Formula Sijunzi Decoction Using a UPLC-PDA Method Tue, 20 May 2014 06:38:05 +0000 Sijunzi decoction (SJZT), a traditional Chinese formula (TCMF) consisting of four herbs, has been widely used for the treatment of various gastrointestinal symptoms. However, its modernization process is hindered by the lack of a powerful quality control method that covers the major active components in the formula. The aim of this study was to establish a UPLC method for the quantitative determination of ten active components in Sijunzi decoction including ginsenoside Rg1, Re, Rb1, liquiritin, liquiritigenin, glycyrrhizic acid, atractylenolide I, atractylenolide II, atractylenolide III, and pachymic acid. Separation was achieved using an ACQUITY UPLC BEHC18 column (2.1 mm × 100 mm, 1.7 μm) with a gradient elution program consisting of acetonitrile and 0.1% phosphoric acid solution. The detection wavelengths were set at 203, 254, 222, and 267 nm. The method was validated for linearity, accuracy, precision, limit of detection, and limit of quantification. The validated method was successfully applied to the simultaneous quantification of ten active compounds from several finished batches of SJZT. This validated that UPLC method is expected to provide a new basis for the quality control of SJZT. Kang An, Guo Jin-rui, Zhang Zhen, and Wang Xiao-long Copyright © 2014 Kang An et al. All rights reserved. Ultrasensitive Detection of Ferulic Acid Using Poly(diallyldimethylammonium chloride) Functionalized Graphene-Based Electrochemical Sensor Mon, 12 May 2014 14:13:14 +0000 The electrochemical redox of ferulic acid (FA) was investigated systematically by cyclic voltammetry (CV) with a poly(diallyldimethylammonium chloride) functionalized graphene-modified glassy carbon electrode (PDDA-G/GCE) as a working electrode. A simple and sensitive differential pulse voltammetry (DPV) technique was proposed for the direct quantitative determination of FA in Angelica sinensis and spiked human urine samples for the first time. The dependence of the intensities of currents and potentials on nature of the supporting electrolyte, pH, scan rate, and concentration was investigated. Under optimal conditions, the proposed sensor exhibited excellent electrochemical sensitivity to FA, and the oxidation peak current was proportional to FA concentration in the range of  M  M, with a relatively low detection limit of  M. This fabricated sensor also displayed acceptable reproducibility, long-term stability, and high selectivity with negligible interferences from common interfering species. Besides, it was applied to detect FA in Angelica sinensis and biological samples with satisfactory results, making it a potential alternative tool for the quantitative detection of FA in pharmaceutical analysis. Lin-jie Liu, Xia Gao, Pei Zhang, Shi-lan Feng, Fang-di Hu, Ying-dong Li, and Chun-ming Wang Copyright © 2014 Lin-jie Liu et al. All rights reserved. Quantitative Analysis of Panax ginseng by FT-NIR Spectroscopy Mon, 05 May 2014 07:16:07 +0000 Near-infrared spectroscopy (NIRS), a rapid and efficient tool, was used to determine the total amount of nine ginsenosides in Panax ginseng. In the study, the regression models were established using multivariate regression methods with the results from conventional chemical analytical methods as reference values. The multivariate regression methods, partial least squares regression (PLSR) and principal component regression (PCR), were discussed and the PLSR was more suitable. Multiplicative scatter correction (MSC), second derivative, and Savitzky-Golay smoothing were utilized together for the spectral preprocessing. When evaluating the final model, factors such as correlation coefficient (R2) and the root mean square error of prediction (RMSEP) were considered. The final optimal results of PLSR model showed that root mean square error of prediction (RMSEP) and correlation coefficients (R2) in the calibration set were 0.159 and 0.963, respectively. The results demonstrated that the NIRS as a new method can be applied to the quality control of Ginseng Radix et Rhizoma. Xin-fang Xu, Li-xing Nie, Li-li Pan, Bian Hao, Shao-xiong Yuan, Rui-chao Lin, Hai-bo Bu, Dan Wang, Ling Dong, and Xiang-ri Li Copyright © 2014 Xin-fang Xu et al. All rights reserved. Electrochemical Immunoassay of Escherichia coli O157:H7 Using Ag@SiO2 Nanoparticles as Labels Sun, 27 Apr 2014 13:21:09 +0000 Silica coated silver (Ag@SiO2) nanoparticles were prepared and characterized by transmission electron microscope (TEM) and UV-vis absorption, and the nanoparticles were used as labels in sandwich-type immunosensor of Escherichia coli O157:H7 (E. coli O157:H7). The labels involved in immunoreaction were dissolved by mixed acid of hydrofluoric acid and nitric acid, and the released Ag+ ions were electrochemical stripping analyzed (via differential pulse voltammetry, DPV) at poly(acrylic acid)/poly(diallyldimethylammonium chloride)/carbon nanotubes (PAA/PDCNT) modified glass carbon electrode (GCE), which obviously enhanced the signal of Ag+ stripping. Then, the number of E. coli O157:H7 could be indirectly reflected by the signal intensity of labeled Ag+. And the results showed that the DPV signals were proportional to the logarithm of the E. coli O157:H7 concentration in the range from 20 cfu/mL to  cfu/mL with the detection limit of 13 cfu/mL. Guang-Zhu Chen, Zheng-Zhi Yin, and Jv-Feng Lou Copyright © 2014 Guang-Zhu Chen et al. All rights reserved. Quantitative Analysis of Matrine in Liquid Crystalline Nanoparticles by HPLC Mon, 14 Apr 2014 16:19:44 +0000 A reversed-phase high-performance liquid chromatographic method has been developed to quantitatively determine matrine in liquid crystal nanoparticles. The chromatographic method is carried out using an isocratic system. The mobile phase was composed of methanol-PBS(pH6.8)-triethylamine (50 : 50 : 0.1%) with a flow rate of 1 mL/min with SPD-20A UV/vis detector and the detection wavelength was at 220 nm. The linearity of matrine is in the range of 1.6 to 200.0 μg/mL. The regression equation is (). The average recovery is 101.7%; %  (). This method provides a simple and accurate strategy to determine matrine in liquid crystalline nanoparticle. Xinsheng Peng, Baohong Li, Min Hu, Yahao Ling, Yuan Tian, Yanxing Zhou, and Yanfang Zhou Copyright © 2014 Xinsheng Peng et al. All rights reserved. Studies on the Anti-Inflammatory Effect and Its Mechanisms of Sophoridine Wed, 09 Apr 2014 08:51:35 +0000 This work is to study the anti-inflammatory effect and its mechanisms of sophoridine in vitro and in vivo. For this aim, the influences of sophoridine on several inflammatory mediators were investigated. Excessive inflammatory response in vitro model was developed by using lipopolysaccharide (LPS) to stimulate the mouse peritoneal macrophages and HL-60 cells to produce IL-6 and IL-8. Carrageenin-induced mouse paw edema model was used as inflammatory response in vivo model. MTT method, ultraviolet spectrophotometric method, and radioimmunoassay were used to measure the changes of TNFα, IL-6, PGE2, and IL-8 in in vitro cell culture supernatant or in the local inflammatory exudates. The results showed that sophoridine inhibited the production of IL-8 in in vitro cell culture supernatant and inhibited the production of TNFα, PGE2, and IL-8 in the local inflammatory exudates but had no significant effects on the production of IL-6 in vitro and in vivo. It is demonstrated that sophoridine’s anti-inflammatory effect was due to its ability to inhibit the production of cytokine and inflammatory mediators. Xiumei Huang, Bo Li, and Lianzhong Shen Copyright © 2014 Xiumei Huang et al. All rights reserved. Optimization of Fluorometric Assay for Ozone in Solution Mon, 24 Mar 2014 07:20:50 +0000 Ozone is widely used for sterilization, deodorization, and cleaning. However, the effects of ozone on human are not well understood, because there is currently no reliable assay method for ozone. Therefore the accurate measurement of ozone is important for its safe use. Here, we report optimized conditions for use with fluorescein derivative 1 (probe 1). Under optimum conditions, probe 1 reacted with ozone quantitatively and specifically to generate a fluorescent substance with an excitation maximum at 493 nm and an emission maximum at 523 nm. We conclude that this assay will be useful for quantifying ozone in solution. Hiromi Nagano, Gotaro Shiota, and Hidetoshi Arakawa Copyright © 2014 Hiromi Nagano et al. All rights reserved. Extraction and Chromatographic Determination of Shikimic Acid in Chinese Conifer Needles with 1-Benzyl-3-methylimidazolium Bromide Ionic Liquid Aqueous Solutions Sun, 23 Mar 2014 09:45:38 +0000 An ionic liquids-based ultrasound-assisted extraction (ILUAE) method was successfully developed for extracting shikimic acid from conifer needles. Eleven 1-alkyl-3-methylimidazolium ionic liquids with different cations and anions were investigated and 1-benzyl-3-methylimidazolium bromide solution was selected as the solvent. The conditions for ILUAE, including the ionic liquid concentration, ultrasound power, ultrasound time, and liquid-solid ratio, were optimized. The proposed method had good recovery (99.37%–100.11%) and reproducibility (RSD, n = 6; 3.6%). ILUAE was an efficient, rapid, and simple sample preparation technique that showed high reproducibility. Based on the results, a number of plant species, namely, Picea koraiensis, Picea meyeri, Pinus elliottii, and Pinus banksiana, were identified as among the best resources of shikimic acid. Fengli Chen, Kexin Hou, Shuangyang Li, Yuangang Zu, and Lei Yang Copyright © 2014 Fengli Chen et al. All rights reserved. Determination of Lactones in Wines by Headspace Solid-Phase Microextraction and Gas Chromatography Coupled with Mass Spectrometry Thu, 20 Mar 2014 07:52:54 +0000 Application of headspace solid-phase microextraction (HS-SPME) coupled with high-resolution gas chromatographic (HRGC) analysis was studied for determining lactones in wines. Six different SPME fibers were tested, and the influence of different factors such as temperature and time of desorption, ionic strength, time of extraction, content of sugar, ethanol, tannins and anthocyanins, and pH and influence of SO2 were studied. The proposed HS-SPME-GC method is an appropriate technique for the quantitative analysis of -butyrolactone, -hexalactone, trans-whiskey lactone, -octalactone, cis-whiskey lactone, -nonalactone, -decalactone, -decalactone, and -undecalactone in wines. Method reproducibility and repeatability ranged between 0.6 and 5.2% for all compounds. Detection limit for -butyrolactone was 0.17 mg/L and a few g/L for the rest of the compounds. The optimized method has been applied to several wine samples. S. J. Pérez-Olivero, M. L. Pérez-Pont, J. E. Conde, and J. P. Pérez-Trujillo Copyright © 2014 S. J. Pérez-Olivero et al. All rights reserved. Urinary Metabolomics on the Biochemical Profiles in Diet-Induced Hyperlipidemia Rat Using Ultraperformance Liquid Chromatography Coupled with Quadrupole Time-of-Flight SYNAPT High-Definition Mass Spectrometry Tue, 18 Mar 2014 07:17:09 +0000 Ultraperformance liquid chromatography coupled with quadrupole time-of-flight synapt high-definition mass spectrometry metabolomics was used to characterize the urinary metabolic profiling of diet-induced hyperlipidaemia in a rat model. Analysis was done by orthogonal partial least squares discriminant analysis, correlation analysis, heat map analysis, and KEGG pathways analysis. Potential biomarkers were chosen by S-plot and were identified by accurate mass, isotopic pattern, and MS/MS fragments information. Significant differences in fatty acid, amino acid, nucleoside, and bile acid were observed, indicating the perturbations of fatty acid, amino acid, nucleoside, and bile acid metabolisms in diet-induced hyperlipidaemia rats. This study provides further insight into the metabolic profiling across a wide range of biochemical pathways in response to diet-induced hyperlipidaemia. Hua Miao, Hua Chen, Xu Zhang, Lu Yin, Dan-Qian Chen, Xian-Long Cheng, Xu Bai, and Feng Wei Copyright © 2014 Hua Miao et al. All rights reserved. Simultaneous Quantitative and Qualitative Analysis of Flavonoids from Ultraviolet-B Radiation in Leaves and Roots of Scutellaria baicalensis Georgi Using LC-UV-ESI-Q/TOF/MS Thu, 13 Mar 2014 16:46:12 +0000 Scutellaria baicalensis Georgi is one of the most widely used traditional Chinese herbal medicines. It has been used for anti-inflammatory, anticancer, antibacterial activities, and so forth. Long-term enhanced ultraviolet-B (UV-B) radiation caused more effect on leaves than on roots of the plant. Liquid chromatography-ultraviolet detection coupled with electrospray ionization quadrupole time-of-flight mass spectrometry (LC-UV-ESI-Q/TOF/MS) method was applied for simultaneous quantitative and qualitative analysis of flavonoids in leaves and roots of S. baicalensis by enhanced UV-B radiation. Both low-intensity radiation and high-intensity radiation were not significantly increaseing the contents of baicalin, wogonoside, and wogonin in roots. However different intensity of radiation has different effects on several flavonoids in leaves. Both low-intensity radiation and high-intensity radiation had no significant effect on contents of baicalin and tectoridin in leaves; the content of scutellarin was significantly decreased by low-intensity radiation; chrysin was detected in low-intensity radiation and high-intensity radiation, and chrysin content is the highest in low-intensity radiation, but chrysin was not detected in control group. Different changes of different flavonoids under enhanced UV-B radiation indicate that induction on flavonoids is selective by enhanced UV-B radiation. Wen-Ting Tang, Min-Feng Fang, Xiao Liu, and Ming Yue Copyright © 2014 Wen-Ting Tang et al. All rights reserved. Using the Doubly Charged Selected Ion Coupled with MS/MS Fragments Monitoring (DCSI-MS/MS) Mode for the Identification of Gelatin Species Thu, 13 Mar 2014 13:47:53 +0000 In electrospray ionization (ESI) mode, peptides and proteins can be multiply charged ions; in this situation a doubly charged selected ion (DCSI) coupled with mass spectrometry (MS/MS) fragments monitoring (DCSI-MS/MS) method is the most suitable scanning mode to detect known peptides in complex samples when an ion-trap mass spectrometer is the instrument used for the analysis. In this mode, the MS detector is programmed to only select a doubly charged ion as a precursor and to perform continuous MS/MS on one or more of the selected precursors, either during a specific time interval or along the whole chromatographic run. Gelatin is a mixture of high molecular weight polypeptides from the hydrolysis of collagen. In this study, the DCSI-MS/MS monitoring mode was applied to the detection of previously characterized species-specific peptides from different gelatins. The proposed methodology makes use of tryptic digestion for sample preparation and peptide separation and identification by rapid resolution liquid chromatography coupled to an ion trap working in the DCSI-MS/MS mode for the analysis. This methodology was applied to the differential classification of five commercial, homological species of gelatins and proved to be an excellent tool for gelatin product authentication. Xian-Long Cheng, Feng Wei, Jia Chen, Ming-hua Li, Lei Zhang, Ying-Yong Zhao, Xin-Yue Xiao, Shuang-cheng Ma, and Rui-Chao Lin Copyright © 2014 Xian-Long Cheng et al. All rights reserved. One Single Amino Acid for Estimation the Content of Total Free Amino Acids in Qingkailing Injection Using High-Performance Liquid Chromatography-Diode Array Detection Thu, 13 Mar 2014 09:38:05 +0000 Qingkailing injection (QKLI), a modern traditional Chinese medicine preparation, has been widely used in clinics due to its fast and significant efficacy in treatment of high fever. The free amino acids (AAs) were considered to be the most abundant active ingredients indisputably. So developing an accurate and simple determination method to measure the contents of total free AAs in QKLI is very crucial. In current study, the accurate and simple method of using one single standard AA for simultaneous quantification of multiple AAs (One for M) in QKLI was developed. Particularly, the calculation methods and the robustness of relative correction factors (RCFs) were investigated systematically. No statistically significant difference between these two quantification methods of One for M and classic regression equation was found by the -test (  =  95%, ). The results showed that the precision (RSD < 4.88%), the robustness (RSD < 4.04%), and the average recoveries (94.11%–107.94%) of this newly proposed method all met the requirements for content determination. This One for M method will provide a scientific reference for the quantitative determination of AAs in other traditional Chinese medicines and their preparations owing to its accuracy and simplicity. Li Zhang, Xue Wang, Jiankun Su, Haiyu Liu, Zhixin Zhang, Lingling Qin, Cheng He, Long Peng, Mingxing Guo, and Xiaoyan Gao Copyright © 2014 Li Zhang et al. All rights reserved. A New Method for the Analysis of Bacterial Endotoxins in Ultrapure Paraffin Oil Sun, 09 Mar 2014 13:40:38 +0000 The paper demonstrates the feasibility of the gel-clot method for the analysis of bacterial endotoxins in water extracts of ultrapure paraffin oil which is a water insoluble oily medical device. Because ultrapure paraffin oil is water insoluble oily liquid, the ultrapure paraffin oil (10 mL) was shaken with 10 mL water for 15 minutes at 2000 rpm, the endotoxin present was extracted to the aqueous phase without interference inhibition/enhancement of the product, the recovery of the endotoxin added to the ultrapure paraffin oil was determined. A validation study confirmed that endotoxins present in ultrapure paraffin oil which is water insoluble liquid medical device pass over into the aqueous phase at concentrations of 20, 10, and 5 EU/mL with recoveries of 94.2% to 111%. So the conclusion is that the gel-clot test is suitable for detecting bacterial endotoxins in ultrapure paraffin oil which is a water insoluble oily medical device. Dandan Chen Copyright © 2014 Dandan Chen. All rights reserved. Study on Dicarboxylic Acids in Aerosol Samples with Capillary Electrophoresis Sun, 09 Mar 2014 06:24:36 +0000 The research was performed to study the simultaneous detection of a homologous series of α, ω-dicarboxylic acids (C2–C10), oxalic, malonic, succinic, glutaric, adipic, pimelic, suberic, azelaic, and sebacic acids, with capillary electrophoresis using indirect UV detection. Good separation efficiency in 2,6-pyridinedicarboxylic acid as background electrolyte modified with myristyl trimethyl ammonium bromide was obtained. The dicarboxylic acids were ionised and separated within five minutes. For the study, authentic samples were collected onto dry cellulose membrane filters of a cascade impactor (12 stages) from outdoor spring aerosols in an urban area. Hot water and ultrasonication extraction methods were used to isolate the acids from membrane filters. Due to the low concentrations of acids in the aerosols, the extracts were concentrated with solid-phase extraction (SPE) before determination. The enrichment of the carboxylic acids was between 86 and 134% with sample pretreatment followed by 100-time increase by preparation of the sample to 50 μL. Inaccuracy was optimised for all the sample processing steps. The aerosols contained dicarboxylic acids C2–C10. Then, mostly they contained C2, C5, and C10. Only one sample contained succinic acid. In the study, the concentrations of the acids in aerosols were lower than 10 ng/m3. Heidi Adler and Heli Sirén Copyright © 2014 Heidi Adler and Heli Sirén. All rights reserved. Simultaneous Determination of Cortisol and Cortisone from Human Serum by Liquid Chromatography-Tandem Mass Spectrometry Thu, 06 Mar 2014 09:00:12 +0000 A fast, sensitive, and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was validated and then the levels of cortisol and cortisone from sera of healthy adults were determined by the LC-MS/MS method. One hundred μL of serum sample was directly extracted by adding 2 mL ethyl acetate, followed by chromatographic separation on a C18 column with a mobile phase consisting of 5 mM ammonium acetate and methanol (25 : 75, v/v). The precision, accuracy, and average recovery of the method were 1.5–5.3%, 95.4–102.5%, and 96.4% for cortisol, and 1.9–6.0%, 89.2–98.8%, and 79.9% for cortisone, respectively. The method was linear from 1.0 to 500.0 ng/mL for cortisol and 2.5 to 100.0 ng/mL for cortisone. The limits of detection (LOD) and quantification (LOQ) were 0.2 and 1.0 ng/mL for cortisol, and 1.0 and 2.5 ng/mL for cortisone, respectively. The average cortisol concentration ( ng/mL) of samples collected between 9:00 and 11:00 a.m. was higher approximately 4.4 times than that of cortisone ( ng/mL) . The average cortisone/cortisol ratio was 0.225. Therefore, the LC-MS/MS method may be useful for the diagnosis of some adrenal diseases and the assessment of 11β-hydroxysteroid dehydrogenase (11β-HSD) activity in clinical laboratories. Sanghoo Lee, Hwan-Sub Lim, Hye-Jin Shin, Seol-A Kim, Jimyeong Park, Hyun-Chul Kim, Hyogyeong Kim, Hyung Joo Kim, Yun-Tae Kim, Kyoung-Ryul Lee, and Young-Jin Kim Copyright © 2014 Sanghoo Lee et al. All rights reserved. Preparation and Characterization of an Amphipathic Magnetic Nanosphere Wed, 05 Mar 2014 13:38:03 +0000 The amphipathic magnetic nanospheres were synthesized using C8 and polyethylene glycol as ligands. Their morphology, structure, and composition were characterized by transmission electron microscope, Fourier transform infrared, and elementary analysis. The prepared materials presented uniform sphere with size distribution about 200 nm. The magnetic characteristics of magnetic nanomaterials were measured by vibrating sample magnetometer. The target products had a saturation magnetization value of 50 emu g−1 and superparamagnetism. The adsorption capability was also studied by static tests, and the material was applied to enrich benzenesulfonamide from calf serum. The results exhibited that the C8-PEG phase owned better adsorption capability, biocompatible property, and dispersivity in aqueous samples. Yongsheng Ji, Ruihong Lv, Zhigang Xu, Chuande Zhao, and Haixia Zhang Copyright © 2014 Yongsheng Ji et al. All rights reserved. Determination of Polyphenol Components of Korean Prostrate Spurge (Euphorbia supina) by Using Liquid Chromatography—Tandem Mass Spectrometry: Overall Contribution to Antioxidant Activity Mon, 03 Mar 2014 08:07:27 +0000 The Korean prostrate spurge Euphorbia supina is a weed that has been used in folk medicine in Korea against a variety of diseases. Nine polyphenols were characterized for this plant by using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) and the results were compared with the literature data. The individual components were validated using the calibration curves of structurally related external standards and quantified for the first time by using the validated method. Correlation coefficients () were >0.9907. The limit of detection and limit of quantification of the method were >0.028 mg/L and 0.094 mg/L, respectively. Recoveries measured at 50 mg/L and 100 mg/L were 76.1–102.8% and 85.2–98.6%, respectively. The total amount of the identified polyphenols was 3352.9 ± 2.8 mg/kg fresh plant. Quercetin and kaempferol derivatives formed 84.8% of the total polyphenols. The antioxidant activities of the flavonoids were evaluated in terms of 1,1-diphenyl-2-picrylhydrazyl and 2,2′-azinobis(3-ethylbenzothiazoline-6-sulfonic acid) radical cation-scavenging activity, and the reducing power showed a dose-dependent increase. Cell viability was effectively suppressed at polyphenol mixture concentrations >250 mg/L. Yi Song, Sung Woo Jeong, Won Sup Lee, Semin Park, Yun-Hi Kim, Gon-Sup Kim, Soo Jung Lee, Jong Sung Jin, Chi-Yeon Kim, Ji Eun Lee, Se Yun Ok, Ki-Min Bark, and Sung Chul Shin Copyright © 2014 Yi Song et al. All rights reserved.