International Journal of Analytical Chemistry The latest articles from Hindawi Publishing Corporation © 2016 , Hindawi Publishing Corporation . All rights reserved. Liquid Chromatography with Electrospray Ionization and Tandem Mass Spectrometry Applied in the Quantitative Analysis of Chitin-Derived Glucosamine for a Rapid Estimation of Fungal Biomass in Soil Tue, 09 Feb 2016 13:45:23 +0000 This method employs liquid chromatography-tandem mass spectrometry to rapidly quantify chitin-derived glucosamine for estimating fungal biomass. Analyte retention was achieved using hydrophilic interaction liquid chromatography, with a zwitter-ionic stationary phase (ZIC-HILIC), and isocratic elution using 60% 5 mM ammonium formate buffer (pH 3.0) and 40% ACN. Inclusion of muramic acid and its chromatographic separation from glucosamine enabled calculation of the bacterial contribution to the latter. Galactosamine, an isobaric isomer to glucosamine, found in significant amounts in soil samples, was also investigated. The two isomers form the same precursor and product ions and could not be chromatographically separated using this rapid method. Instead, glucosamine and galactosamine were distinguished mathematically, using the linear relationships describing the differences in product ion intensities for the two analytes. The m/z transitions of 180 72 and 180 84 were applied for the detection of glucosamine and galactosamine and that of 252 126 for muramic acid. Limits of detection were in the nanomolar range for all included analytes. The total analysis time was 6 min, providing a high sample throughput method. Madelen A. Olofsson and Dan Bylund Copyright © 2016 Madelen A. Olofsson and Dan Bylund. All rights reserved. Enantioseparation of Citalopram by RP-HPLC, Using Sulfobutyl Ether-β-Cyclodextrin as a Chiral Mobile Phase Additive Tue, 05 Jan 2016 08:32:23 +0000 Enantiomeric separation of citalopram (CIT) was developed using a reversed phase HPLC (RP-HPLC) with sulfobutylether-β-cyclodextrin (SBE-β-CD) as a chiral mobile phase additive. The effects of the pH value of aqueous buffer, concentration of chiral additive, composition of mobile phase, and column temperature on the enantioseparation of CIT were investigated on the Hedera ODS-2 C18 column (250 mm × 4.6 mm × 5.0 um). A satisfactory resolution was achieved at 25°C using a mobile phase consisting of a mixture of aqueous buffer (pH of 2.5, 5 mM sodium dihydrogen phosphate, and 12 mM SBE-β-CD), methanol, and acetonitrile with a volumetric ratio of 21 : 3 : 1 and flow rate of 1.0 mL/min. This analytical method was evaluated by examining the precision (lower than 3.0%), linearity (regression coefficients close to 1), limit of detection (0.070 µg/mL for ()-CIT and 0.076 µg/mL for ()-CIT), and limit of quantitation (0.235 µg/mL for ()-CIT and 0.254 µg/mL for ()-CIT). Yangfeng Peng, Quan Sophia He, and Jiang Cai Copyright © 2016 Yangfeng Peng et al. All rights reserved. Micellar Enhanced Spectrofluorimetric Method for the Determination of Ponatinib in Human Plasma and Urine via Cremophor RH 40 as Sensing Agent Thu, 31 Dec 2015 16:33:28 +0000 An impressively simple and precise spectrofluorimetric procedure was established and validated for ponatinib (PTB) quantitation in biological fluids such as human plasma and human urine. This method depends on examining the fluorescence characteristics of PTB in a micellar system of Cremophor RH 40 (Cr RH 40). Cr RH 40 enhanced the intrinsic fluorescence of PTB distinctly in aqueous water. The fluorescence spectra of PTB was recorded at 457 nm following its excitation at 305 nm. Maximum fluorescence intensity was attained by addition of 0.7 mL of Cr RH 40 and one mL of phosphate buffer to PTB aliquots and then dilution with distilled water. There is a linear relationship between the fluorescence intensity of PTB and its concentration over the range 5–120 ngmL−1, with limit of detection and limit of quantification equal to 0.905 ngmL−1 and 2.742 ngmL−1, respectively. The accuracy and the precisions of the proposed method were checked and gave adequate results. The adopted method was applied with a great success for PTB quantitation in different biological matrices (spiked human plasma and urine) giving high recovery values. Hany W. Darwish, Ahmed H. Bakheit, Ali Saber Abdelhameed, and Amer S. AlKhairallah Copyright © 2015 Hany W. Darwish et al. All rights reserved. Near-Infrared Spectroscopy as an Analytical Process Technology for the On-Line Quantification of Water Precipitation Processes during Danhong Injection Tue, 29 Dec 2015 13:08:42 +0000 This paper used near-infrared (NIR) spectroscopy for the on-line quantitative monitoring of water precipitation during Danhong injection. For these NIR measurements, two fiber optic probes designed to transmit NIR radiation through a 2 mm flow cell were used to collect spectra in real-time. Partial least squares regression (PLSR) was developed as the preferred chemometrics quantitative analysis of the critical intermediate qualities: the danshensu (DSS, (R)-3, 4-dihydroxyphenyllactic acid), protocatechuic aldehyde (PA), rosmarinic acid (RA), and salvianolic acid B (SAB) concentrations. Optimized PLSR models were successfully built and used for on-line detecting of the concentrations of DSS, PA, RA, and SAB of water precipitation during Danhong injection. Besides, the information of DSS, PA, RA, and SAB concentrations would be instantly fed back to site technical personnel for control and adjustment timely. The verification experiments determined that the predicted values agreed with the actual homologic value. Xuesong Liu, Chunyan Wu, Shu Geng, Ye Jin, Lianjun Luan, Yong Chen, and Yongjiang Wu Copyright © 2015 Xuesong Liu et al. All rights reserved. Separation and Analysis of Boron Isotope in High Plant by Thermal Ionization Mass Spectrometry Thu, 24 Dec 2015 13:55:17 +0000 Knowledge of boron and its isotope in plants is useful to better understand the transposition and translocation of boron within plant, the geochemical behavior in the interface between soil and plant, and the biogeochemical cycle of boron. It is critical to develop a useful method to separate boron from the plant for the geochemical application of boron and its isotope. A method was developed for the extraction of boron in plant sample, whose isotope was determined by thermal ionization mass spectrometry. The results indicated that this method of dry ashing coupled with two-step ion-exchange chromatography is powerful for the separation of boron in plant sample with large amounts of organic matters completely. The ratios of boron isotope composition in those plant tissue samples ranged from to (total range: ) with a mean value of SD. The stem and root isotopic compositions were lower than those in flower and leaf. The molecular mechanism of boron isotope may be responsible for the observed variation of boron isotopic composition and are considered as a useful tool for the better understanding of boron cycling process in the environment and for the signature of living systems. Qingcai Xu, Yuliang Dong, Huayu Zhu, and Aide Sun Copyright © 2015 Qingcai Xu et al. All rights reserved. High Performance Liquid Chromatographic Assay for the Simultaneous Determination of Posaconazole and Vincristine in Rat Plasma Tue, 22 Dec 2015 08:34:09 +0000 Purpose. Developing a validated HPLC-DAD method for simultaneous determination of posaconazole (PSZ) and vincristine (VCR) in rat plasma. Methods. PSZ, VCR, and itraconazole (ITZ) were extracted from 200 μL plasma using diethyl ether in the presence of 0.1 M sodium hydroxide solution. The organic layer was evaporated in vacuo and dried residue was reconstituted and injected through HC-C18 (4.6 × 250 mm, 5 μm) column. In the mobile phase, acetonitrile and 0.015 M potassium dihydrogen orthophosphate (30 : 70 to 80 : 20, linear gradient over 7 minutes) pumped at 1.5 mL/min. VCR and PSZ were measured at 220 and 262 nm, respectively. Two Sprague Dawley rats were orally dosed PSZ followed by iv dosing of VCR and serial blood sampling was performed. Results. VCR, PSZ, and ITZ were successfully separated within 11 min. Calibration curves were linear over the range of 50–5000 ng/mL for both drugs. The CV% and % error of the mean were ≤18% and limit of quantitation was 50 ng/mL for both drugs. Rat plasma concentrations of PSZ and VCR were simultaneously measured up to 72 h and their calculated pharmacokinetics parameters were comparable to the literature. Conclusion. The assay was validated as per ICH guidelines and is appropriate for pharmacokinetics drug-drug interaction studies. Hadeel A. Khalil, Ahmed F. El-Yazbi, Tarek S. Belal, and Dalia A. Hamdy Copyright © 2015 Hadeel A. Khalil et al. All rights reserved. A New HPLC-ELSD Method for Simultaneous Determination of N-Acetylglucosamine and N-Acetylgalactosamine in Dairy Foods Tue, 15 Dec 2015 13:39:09 +0000 A rapid high performance liquid chromatographic method with evaporative light scattering detection (HPLC-ELSD), using a carbohydrate column, was developed for simultaneous determination of N-acetylglucosamine (GlcNAc) and N-acetylgalactosamine (GalNAc) in dairy foods. Sample preparation was performed by precipitation using acetonitrile. The limits of detection were 2.097 mg/L for GlcNAc and 3.247 mg/L for GalNAc. The limits of quantification were 6.043 mg/L for GlcNAc and 9.125 mg/L for GalNAc. Accuracy ranged from 96.4 to 105.7% for GlcNAc and from 97.1 to 104.1% for GalNAc. The precision of the method was <1.7% for GlcNAc and <2.2% for GalNAc. The mean recovery of the method was measured by spiking samples with 30.0–120.0 mg/L GlcNAc or 12.5–50.0 mg/L GalNAc and was found to be 95.1–105.5% for GlcNAc and 99.5–105.9% for GalNAc. The stability test results of standard solutions stored at 4, 20, and 40°C were 96.2–104.7% for GlcNAc and 98.0–106.5% for GalNAc. This study determined GlcNAc and GalNAc in dairy foods using HPLC-ELSD method. This rapid, simultaneous quantitation method might be useful as a mean of convenient quality control of dairy foods. Ho Jin Kim, In Kyung Bae, Min Hee Jeong, Hye Jin Park, Jin Sil Jung, and Jang Eok Kim Copyright © 2015 Ho Jin Kim et al. All rights reserved. Development and Validation of Simple RP-HPLC Method for Intracellular Determination of Fluconazole Concentration and Its Application to the Study of Candida albicans Azole Resistance Wed, 09 Dec 2015 07:57:45 +0000 Candida albicans (strains NCTC-885-653 and ATCC-10231) long-term cultivated in the presence of antifungal agent fluconazole (FLC) and classical microbiological methods for determination of minimal inhibitory concentration (MIC) were used in this study. A simple and sensitive method based on reverse-phase high-performance liquid chromatography (RP-HPLC) has been developed for the determination of FLC intracellular concentration in C. albicans using tinidazole as an internal standard. Following extraction with dichloromethane, the chromatographic separation was achieved on a Machery-Nagel EC250/2 Nucleodur-100-3 C18 column by gradient elution using the mobile phase consisting of (A) 0.01 M ammonium acetate buffer, pH = 5.00, and (B) acetonitrile. Different analytical performance parameters such as linearity, precision, accuracy, limit of quantification (LOQ), and robustness were determined according to US DHHS FDA and EMEA guidelines. The method was linear for FLC ranging from 100 to 10000 ng/mL. The intraday and interday precisions (relative standard deviation) were within 2.79 and 2.64%, respectively, and the accuracy (relative error) was less than 2.82%. The extraction recovery ranged from 79.3 to 85.5%. The reliable method was successfully applied to C. albicans azole-resistance study and it was shown that intracellular concentration of FLC correlated with a yeast drug susceptibility profile and MIC values. Tigran K. Davtyan, Levon A. Melikyan, Nune A. Nikoyan, Hripsime P. Aleksanyan, and Nairi G. Grigoryan Copyright © 2015 Tigran K. Davtyan et al. All rights reserved. Simultaneous Detection and Estimation of Catechol, Hydroquinone, and Resorcinol in Binary and Ternary Mixtures Using Electrochemical Techniques Tue, 01 Dec 2015 10:08:24 +0000 Cyclic voltammetry (CV) and differential pulse voltammetry (DPV) were performed with a glassy carbon electrode (GCE) modified with polyglutamic acid (PGA) on the three dihydroxybenzene isomers, catechol (CT), hydroquinone (HQ), and resorcinol (RS). At bare GCE, these isomers exhibited voltammograms with highly overlapped redox peaks that impeded their simultaneous detection in binary and ternary mixtures. On the contrary, at PGA modified GCE binary and ternary mixtures of the dihydroxybenzene isomers showed well-resolved redox peaks in both CV and DPV experiments. This resolving ability of PGA modified GCE proves its potential to be exploited as an electrochemical sensor for the simultaneous detection of these isomers. Md. Uzzal Hossain, Md. Toufiqur Rahman, and Md. Qamrul Ehsan Copyright © 2015 Md. Uzzal Hossain et al. All rights reserved. Highly Sensitive Immunochromatographic Identification of Tetracycline Antibiotics in Milk Wed, 25 Nov 2015 12:04:28 +0000 A rapid immunochromatographic assay was developed for the control of tetracycline (TC). The assay is based on the competition between immobilized TC-protein conjugate and TC in a tested sample for binding with polyclonal anti-TC antibodies conjugated to colloidal gold during the flow of the sample along a membrane strip with immobilized reactants. Conjugation of colloidal gold and the total immunoglobulin (IgG) fraction of polyclonal antibodies was used to increase the assay sensitivity to ensure low content of specific antibodies in the conjugate. This allowed effective inhibition of free TC and conjugate binding in the strip test zone. Photometric marker registration allows control of the reduction of binding, thereby enhancing detection sensitivity. The proposed assay allows TC to be detected at concentrations up to 20 ng/mL, exceeding the limit of detection of the known analogues, in a wide working range (more than two orders) of 60 pg/mL to 10 ng/mL, ensured through the use of polyclonal antibodies. The assay time is 10 min. The efficiency of the designed assay is shown to identify TC in milk; the degree of recovery of TC ranges from 90 to 112%. The precision of the concentrations measurements was no more than 10%. N. A. Taranova, A. S. Kruhlik, E. A. Zvereva, V. V. Shmanai, I. I. Vashkevich, D. A. Semyonov, S. A. Eremin, A. V. Zherdev, and B. B. Dzantiev Copyright © 2015 N. A. Taranova et al. All rights reserved. Effects of Bahir Dar Textile Factory Effluents on the Water Quality of the Head Waters of Blue Nile River, Ethiopia Tue, 24 Nov 2015 07:40:14 +0000 The study was conducted in 2013/14 with the objective of determining the effects of Bahir Dar textile factory effluents on the head of Blue Nile River water quality. Dissolve oxygen was higher at the upstream site of the river, whereas BOD5, TDS, and total alkalinity values were higher at wastewater outlet of the factory site. The mean values of dissolved oxygen, BOD5, and total alkalinity were above maximum permissible limits set by WHO for drinking water at head of Blue Nile River. The mean value of BOD5 was above permissible limit of IFC for textile effluents to be discharged to surface water. A total of 836 aquatic macroinvertebrate individuals belonging to 21 families were collected. The Shannon-Wiener Diversity Index, the Hilsenhoff family-level biotic index, family richness, and percent dipterans were calculated. Hilsenhoff family-level biotic index and percent dipterans metrics differed significantly among sampling sites . Hilsenhoff family-level biotic index was higher at the most downstream site but percent dipterans were higher at site of discharge of effluent to the head of Blue Nile River. Therefore, there is indication that effluent demands frequent control and proper treatment before being discharged to the environment. Abrehet Kahsay Mehari, Shewit Gebremedhin, and Belayneh Ayele Copyright © 2015 Abrehet Kahsay Mehari et al. All rights reserved. Extraction and Analysis of Strontium in Water Sample Using a Sr2+ Selective Polymer as the Absorbent Phase Thu, 12 Nov 2015 11:31:36 +0000 A kind of Sr2+ selective resin was applied as an absorption phase to extract Sr2+ ion from an aqueous solution, and the amount of Sr2+ was determined using inductively coupled plasma optical emission spectrometer. Factors, including absorption time, temperature, stirring rate, salt-out effect, desorption, and the pH of the aqueous solution, were investigated to optimize the absorption efficiency of Sr2+. Foreign ions were examined to observe their effects on the absorption behavior of Sr2+. The optimum condition was absorption time at 20 min, pH of aqueous solution 7, temperature of 35°C, and 600 rpm stirring rate. A 10 mL solution of 0.1 mol/L HCl is used as the desorption agent. The linear range of Sr2+ concentrations from 50 to 1200 μg/L was investigated with the slope of 183 μg/L. The limit of detection was 21 μg/L with 4.23% relative standard deviation. The correlation coefficient was found to be 0.9947. Under the optimized conditions, the concentrations of Sr2+ in four water samples were detected by the developed method. We propose that this method effectively extracts strontium ion from environmental water samples. Rongjian Ying Copyright © 2015 Rongjian Ying. All rights reserved. Photodegradation of Eosin Y Using Silver-Doped Magnetic Nanoparticles Wed, 04 Nov 2015 06:34:59 +0000 The purification of industrial wastewater from dyes is becoming increasingly important since they are toxic or carcinogenic to human beings. Nanomaterials have been receiving significant attention due to their unique physical and chemical properties compared with their larger-size counterparts. The aim of the present investigation was to fabricate magnetic nanoparticles (MNPs) using a coprecipitation method, followed by coating with silver (Ag) in order to enhance the photocatalytic activity of the MNPs by loading metal onto them. The fabricated magnetic nanoparticles coated with Ag were characterised using different instruments such as a scanning electron microscope (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray (EDAX) spectroscopy, and X-ray diffraction (XRD) analysis. The average size of the magnetic nanoparticles had a mean diameter of about 48 nm, and the average particle size changed to 55 nm after doping. The fabricated Ag-doped magnetic nanoparticles were used for the degradation of eosin Y under UV-lamp irradiation. The experimental results revealed that the use of fabricated magnetic nanoparticles coated with Ag can be considered as reliable methods for the removal of eosin Y since the slope of evaluation of pseudo-first-order rate constant from the slope of the plot between and the irradiation time was found to be linear. Ag-Fe3O4 nanoparticles would be considered an efficient photocatalyst to degrade textile dyes avoiding the tedious filtration step. Eman Alzahrani Copyright © 2015 Eman Alzahrani. All rights reserved. Development of a HPLC Method for the Quantitative Determination of Capsaicin in Collagen Sponge Tue, 03 Nov 2015 07:46:37 +0000 Controlling the concentration of drugs in pharmaceutical products is essential to patient’s safety. In this study, a simple and sensitive HPLC method is developed to quantitatively analyze capsaicin in collagen sponge. The capsaicin from sponge was extracted for 30 min with ultrasonic wave extraction technique and methanol was used as solvent. The chromatographic method was performed by using isocratic system composed of acetonitrile-water (70 : 30) with a flow rate of 1 mL/min and the detection wavelength was at 280 nm. Capsaicin can be successfully separated with good linearity (the regression equation is A = 9.7182C + 0.8547; R2 = 1.0) and perfect recovery (99.72%). The mean capsaicin concentration in collagen sponge was 49.32 mg/g (RSD = 1.30%; n = 3). In conclusion, the ultrasonic wave extraction method is simple and the extracting efficiency is high. The HPLC assay has excellent sensitivity and specificity and is a convenient method for capsaicin detection in collagen sponge. This paper firstly discusses the quantitative analysis of capsaicin in collagen sponge. Chun-Lian Guo, Hong-Ying Chen, Bi-Ling Cui, Yu-Huan Chen, Yan-Fang Zhou, Xin-Sheng Peng, and Qin Wang Copyright © 2015 Chun-Lian Guo et al. All rights reserved. Total Phenolic, Flavonoid, Tomatine, and Tomatidine Contents and Antioxidant and Antimicrobial Activities of Extracts of Tomato Plant Sun, 01 Nov 2015 12:25:40 +0000 The purpose of this study was to evaluate the antioxidant and antimicrobial properties of extracts of different fractions of two tomato plant cultivars. The stems, roots, leaves, and whole-plant fractions were evaluated. Tomatine and tomatidine were identified by HPLC-DAD. The leaf extracts from the two varieties showed the highest flavonoids, chlorophyll, carotenoids, and total phenolics contents and the highest antioxidant activity determined by DPPH, ABTS, and ORAC. A positive correlation was observed between the antioxidant capacities of the extracts and the total phenolic, flavonoid, and chlorophyll contents. The Pitenza variety extracts inhibited the growth of pathogens such as E. coli O157:H7, Salmonella Typhimurium, Staphylococcus aureus, and Listeria ivanovii, yielding inhibition halos of 8.0 to 12.9 mm in diameter and MIC values of 12.5 to 3.125 mg/mL. These results suggest that tomato plant shows well potential as sources of various bioactive compounds, antioxidants, and antimicrobials. Norma Patricia Silva-Beltrán, Saul Ruiz-Cruz, Luis Alberto Cira-Chávez, María Isabel Estrada-Alvarado, José de Jesús Ornelas-Paz, Marco Antonio López-Mata, Carmen Lizette Del-Toro-Sánchez, J. Fernando Ayala-Zavala, and Enrique Márquez-Ríos Copyright © 2015 Norma Patricia Silva-Beltrán et al. All rights reserved. Spectrophotometric Analysis of Caffeine Thu, 29 Oct 2015 11:52:07 +0000 The nature of caffeine reveals that it is a bitter white crystalline alkaloid. It is a common ingredient in a variety of drinks (soft and energy drinks) and is also used in combination with various medicines. In order to maintain the optimum level of caffeine, various spectrophotometric methods have been developed. The monitoring of caffeine is very important aspect because of its consumption in higher doses that can lead to various physiological disorders. This paper incorporates various spectrophotometric methods used in the analysis of caffeine in various environmental samples such as pharmaceuticals, soft and energy drinks, tea, and coffee. A range of spectrophotometric methodologies including chemometric techniques and derivatization of spectra have been used to analyse the caffeine. Showkat Ahmad Bhawani, Sim Siong Fong, and Mohamad Nasir Mohamad Ibrahim Copyright © 2015 Showkat Ahmad Bhawani et al. All rights reserved. Validation of a HPLC/FLD Method for Quantification of Tocotrienols in Human Plasma Wed, 28 Oct 2015 12:43:06 +0000 Quantification of tocotrienols in human plasma is critical when the attention towards tocotrienols on its distinctive properties is arising. We aim to develop a simple and practical normal-phase high performance liquid chromatography method to quantify the amount of four tocotrienol homologues in human plasma. Using both the external and internal standards, tocotrienol homologues were quantified via a normal-phase high performance liquid chromatography with fluorescence detector maintained at the excitation wavelength of 295 nm and the emission wavelength of 325 nm. The four tocotrienol homologues were well separated within 30 minutes. A large interindividual variation between subjects was observed as the absorption of tocotrienols is dependent on food matrix and gut lipolysis. The accuracies of lower and upper limit of quantification ranged between 92% and 109% for intraday assays and 90% and 112% for interday assays. This method was successfully applied to quantify the total amount of four tocotrienol homologues in human plasma. Hui-Ling Che, Doryn Meam-Yee Tan, Puvaneswari Meganathan, Yee-Lin Gan, Ghazali Abdul Razak, and Ju-Yen Fu Copyright © 2015 Hui-Ling Che et al. All rights reserved. Development of a Portable Single Photon Ionization-Photoelectron Ionization Time-of-Flight Mass Spectrometer Mon, 26 Oct 2015 06:38:26 +0000 A vacuum ultraviolet lamp based single photon ionization- (SPI-) photoelectron ionization (PEI) portable reflecting time-of-flight mass spectrometer (TOFMS) was designed for online monitoring gas samples. It has a dual mode ionization source: SPI for analyte with ionization energy (IE) below 10.6 eV and PEI for IE higher than 10.6 eV. Two kinds of sampling inlets, a capillary inlet and a membrane inlet, are utilized for high concentration and trace volatile organic compounds, respectively. A mass resolution of 1100 at m/z 64 has been obtained with a total size of 40 × 31 × 29 cm, the weight is 27 kg, and the power consumption is only 70 W. A mixture of benzene, toluene, and xylene (BTX), SO2, and discharging products of SF6 were used to test its performance, and the result showed that the limit of quantitation for BTX is as low as 5 ppbv (S/N = 10 : 1) with linear dynamic ranges greater than four orders of magnitude. The portable TOFMS was also evaluated by analyzing volatile organic compounds from wine and decomposition products of SF6 inside of a gas-insulated switchgear. Yunguang Huang, Jinxu Li, Bin Tang, Liping Zhu, Keyong Hou, and Haiyang Li Copyright © 2015 Yunguang Huang et al. All rights reserved. Stability-Indicating Assay for the Determination of Pentobarbital Sodium in Liquid Formulations Mon, 12 Oct 2015 08:46:40 +0000 A stability-indicating assay by reversed-phase high performance liquid chromatography (RP-HPLC) method was developed for the determination of pentobarbital sodium in oral formulations: a drug used for infant sedation in computed tomography (CT) or magnetic resonance imaging (MRI) scan. The chromatographic separation was achieved on a reversed-phase C18 column, using isocratic elution and a detector set at 214 nm. The optimized mobile phase consisted of a 0.01 M potassium buffer pH 3 and methanol (40 : 60, v/v). The flow rate was 1.0 mL/min and the run time of analysis was 5 min. The linearity of the method was demonstrated in the range of 5 to 250 μg/mL pentobarbital sodium solution ( = 0.999). The limit of detection and limit of quantification were 2.10 and 3.97 μg/mL, respectively. The intraday and interday precisions were less than 2.1%. Accuracy of the method ranged from 99.2 to 101.3%. Stability studies indicate that the drug is stable to sunlight and in aqueous solution. Accelerated pentobarbital sodium breakdown by strong alkaline, acidic, or oxidative stress produced noninterfering peaks. This method allows accurate and reliable determination of pentobarbital sodium for drug stability assay in pharmaceutical studies. Myriam Ajemni, Issa-Bella Balde, Sofiane Kabiche, Sandra Carret, Jean-Eudes Fontan, Salvatore Cisternino, and Joël Schlatter Copyright © 2015 Myriam Ajemni et al. All rights reserved. Similarity Evaluation of Different Origins and Species of Dendrobiums by GC-MS and FTIR Analysis of Polysaccharides Sun, 11 Oct 2015 10:01:57 +0000 GC-MS method combined with FTIR techniques by the analysis of polysaccharide was applied to evaluate the similarity between wild (W) and tissue-cultured (TC) Dendrobium huoshanense (DHS), Dendrobium officinale (DO), and Dendrobium moniliforme (DM) as well as 3 wild Dendrobium spp.: Dendrobium henanense (DHN), Dendrobium loddigesii (DL), and Dendrobium crepidatum (DC). Eight monosaccharides involving xylose, arabinose, rhamnose, glucose, mannose, fructose, galactose, and galacturonic acid were identified in the polysaccharide from each Dendrobium sample while the contents of the monosugars varied remarkably across origins and species. Further similarity evaluation based on GC-MS data showed that the values of different origins of DHS, DO, and DM were 0.831, 0.865, and 0.884, respectively, while the values ranged from 0.475 to 0.837 across species. FTIR files of the polysaccharides revealed that the similarity coefficients between W and TC-DHS, DO, and DM were 88.7%, 86.8%, and 88.5%, respectively, in contrast to the similarity coefficients varying from 57.4% to 82.6% across species. These results suggested that the structures of polysaccharides between different origins of the investigated Dendrobiums might be higher than what we had supposed. Nai-Dong Chen, Nai-Fu Chen, Jun Li, Cai-Yun Cao, Jin-Mei Wang, and He-Ping Huang Copyright © 2015 Nai-Dong Chen et al. All rights reserved. Simultaneous Determination of Salicylic Acid, Jasmonic Acid, Methyl Salicylate, and Methyl Jasmonate from Ulmus pumila Leaves by GC-MS Thu, 17 Sep 2015 12:55:52 +0000 Salicylic acid, jasmonic acid, methyl salicylate, and methyl jasmonate are important phytohormones and defensive signaling compounds, so it is of great importance to determine their levels rapidly and accurately. The study uses Ulmus pumila leaves infected by Tetraneura akinire Sasaki at different stages as materials; after extraction with 80% methanol and ethyl acetate and purification with primary secondary amine (PSA) and graphitized carbon blacks (GCB), the contents of signal compounds salicylic acid, jasmonic acid, methyl salicylate, and methyl jasmonate were determined by GC-MS. The results showed that the level of salicylic acid, jasmonic acid, methyl salicylate, and methyl jasmonate increased remarkably in U. pumila once infected by T. akinire Sasaki, but the maximums of these four compounds occurred at different times. Salicylic acid level reached the highest at the early stage, and jasmonic acid level went to the maximum in the middle stage; by contrast, change of content of methyl salicylate and methyl jasmonate was the quite opposite. Zhi-hong Huang, Zhi-li Wang, Bao-lin Shi, Dong Wei, Jian-xin Chen, Su-li Wang, and Bao-jia Gao Copyright © 2015 Zhi-hong Huang et al. All rights reserved. Ammonium Ion Exchanged Zeolite for Laser Desorption/Ionization Mass Spectrometry of Phosphorylated Peptides Sun, 13 Sep 2015 14:02:53 +0000 α-Cyano-4-hydroxycinnamic acid (CHCA), an organic matrix molecule for matrix-assisted laser desorption/ionization mass spectrometry, was adsorbed to -type zeolite surface, and this new matrix was used for the detection of low-molecular-weight compounds. It was found that this matrix could simplify the mass spectrum in the low-molecular-weight region and prevent interference from fragments and alkali metal ion adducted species. CHCA adsorbed to -type ZSM5 zeolite (CHCA/NH4ZSM5) was used to measure atropine and aconitine, two toxic alkaloids in plants. In addition, CHCA/NH4ZSM5 enabled us to detect phosphorylated peptides; peaks of the protonated peptides had higher intensities than the peaks observed using CHCA only. Mengrui Yang and Tatsuya Fujino Copyright © 2015 Mengrui Yang and Tatsuya Fujino. All rights reserved. Some Rare Earth Elements Analysis by Microwave Plasma Torch Coupled with the Linear Ion Trap Mass Spectrometry Wed, 02 Sep 2015 09:54:52 +0000 A sensitive mass spectrometric analysis method based on the microwave plasma technique is developed for the fast detection of trace rare earth elements (REEs) in aqueous solution. The plasma was produced from a microwave plasma torch (MPT) under atmospheric pressure and was used as ambient ion source of a linear ion trap mass spectrometer (LTQ). Water samples were directly pneumatically nebulized to flow into the plasma through the central tube of MPT. For some REEs, the generated composite ions were detected in both positive and negative ion modes and further characterized in tandem mass spectrometry. Under the optimized conditions, the limit of detection (LOD) was at the level 0.1 ng/mL using MS2 procedure in negative mode. A single REE analysis can be completed within 2~3 minutes with the relative standard deviation ranging between 2.4% and 21.2% (six repeated measurements) for the 5 experimental runs. Moreover, the recovery rates of these REEs are between the range of 97.6%–122.1%. Two real samples have also been analyzed, including well and orange juice. These experimental data demonstrated that this method is a useful tool for the field analysis of REEs in water and can be used as an alternative supplement of ICP-MS. Xiaohong Xiong, Tao Jiang, Wenhao Qi, Jun Zuo, Meiling Yang, Qiang Fei, Saijin Xiao, Aimin Yu, Zhiqiang Zhu, and Huanwen Chen Copyright © 2015 Xiaohong Xiong et al. All rights reserved. Risk Assessment and Prediction of Heavy Metal Pollution in Groundwater and River Sediment: A Case Study of a Typical Agricultural Irrigation Area in Northeast China Sun, 23 Aug 2015 12:39:59 +0000 The areas with typical municipal sewage discharge river and irrigation water function were selected as study sites in northeast China. The samples from groundwater and river sediment in this area were collected for the concentrations and forms of heavy metals (Cr(VI), Cd, As, and Pb) analysis. The risk assessment of heavy metal pollution was conducted based on single-factor pollution index (I) and Nemerow pollution index (NI). The results showed that only one groundwater sampling site reached a polluted level of heavy metals. There was a high potential ecological risk of Cd on the N21-2 sampling site in river sediment. The morphological analysis results of heavy metals in sediment showed that the release of heavy metals can be inferred as one of the main pollution sources of groundwater. In addition, the changes in the concentration and migration scope of As were predicted by using the Groundwater Modeling System (GMS). The predicted results showed that As will migrate downstream in the next decade, and the changing trend of As polluted areas was changed with As content districts because of some pump wells downstream to form groundwater depression cone, which made the solute transfer upstream. Shuang Zhong, Hui Geng, Fengjun Zhang, Zhaoying Liu, Tianye Wang, and Boyu Song Copyright © 2015 Shuang Zhong et al. All rights reserved. Online NIR Analysis and Prediction Model for Synthesis Process of Ethyl 2-Chloropropionate Thu, 20 Aug 2015 14:06:31 +0000 Online near-infrared spectroscopy was used as a process analysis technique in the synthesis of 2-chloropropionate for the first time. Then, the partial least squares regression (PLSR) quantitative model of the product solution concentration was established and optimized. Correlation coefficient () of partial least squares regression (PLSR) calibration model was 0.9944, and the root mean square error of correction (RMSEC) was 0.018105 mol/L. These values of PLSR and RMSEC could prove that the quantitative calibration model had good performance. Moreover, the root mean square error of prediction (RMSEP) of validation set was 0.036429 mol/L. The results were very similar to those of offline gas chromatographic analysis, which could prove the method was valid. Wei Zhang, Hang Song, Jing Lu, Wen Liu, Lirong Nie, and Shun Yao Copyright © 2015 Wei Zhang et al. All rights reserved. Quantification of Niacin and Its Metabolite Nicotinuric Acid in Human Plasma by LC-MS/MS: Application to a Clinical Trial of a Fixed Dose Combination Tablet of Niacin Extended-Release/Simvastatin (500 mg/10 mg) in Healthy Chinese Volunteers Wed, 05 Aug 2015 11:49:05 +0000 Our paper aimed to develop rapid, sensitive, and specific LC-MS/MS method for the quantification of niacin (NA) and its metabolite nicotinuric acid (NUA) in human plasma. Following protein precipitation with acetonitrile, the NA, NUA, and internal standard (5-fluorouracil) were separated on a Zorbax 300SB-C8 column (250 mm × 4.6 mm, 5 μm) with a mobile phase consisting of methanol-2 mM ammonium acetate (3 : 97, v/v) at a flow rate of 1 mL/min (split 1 : 1). A tandem mass spectrometer equipped with electrospray ionization source was used as the detector and operated in negative ion mode. The linear concentration ranges of the calibration curves were 5–800 ng/mL for NA and NUA. The intra-assay RSD for quality control (QC) samples were from 5.0% to 8.7% for NA, and 5.5% to 7.6% for NUA. The interassay RSD for QC samples were from 2.8% to 9.4% for NA, and 3.7% to 5.8% for NUA. The relative errors for QC samples were from −2.2% to 2.3% for NA, and −0.6% to 3.2% for NUA. The method was successfully applied to the investigation of the pharmacokinetic profiles of NA, NUA in human after single dose administration of Niacin extended-release/Simvastatin tablet (500 mg/10 mg). Pingping Zhang, Yantong Sun, Guobing Shi, Yin Sui, Qiuying Li, Yunbiao Tang, and Jingkai Gu Copyright © 2015 Pingping Zhang et al. All rights reserved. Fast Differential Analysis of Propolis Using Surface Desorption Atmospheric Pressure Chemical Ionization Mass Spectrometry Mon, 03 Aug 2015 12:35:02 +0000 Mass spectral fingerprints of 24 raw propolis samples, including 23 from China and one from the United States, were directly obtained using surface desorption atmospheric pressure chemical ionization mass spectrometry (SDAPCI-MS) without sample pretreatment. Under the optimized experimental conditions, the most abundant signals were detected in the mass ranges of 70 to 500 m/z and 200 to 350 m/z, respectively. Principal component analyses (PCA) for the two mass ranges showed similarities in that the colors had a significant correlation with the first two PCs; in contrast there was no correlation with the climatic zones from which the samples originated. Analytes such as chrysin, pinocembrin, and quercetin were detected and identified using multiple stage mass spectrometry within 3 min. Therefore, SDAPCI-MS can be used for rapid and reliable high-throughput analysis of propolis. Xue-yong Huang, Xia-li Guo, Huo-lin Luo, Xiao-wei Fang, Teng-gao Zhu, Xing-lei Zhang, Huan-wen Chen, and Li-ping Luo Copyright © 2015 Xue-yong Huang et al. All rights reserved. Comparative Analysis of Amino Acids, Nucleosides, and Nucleobases in Thais clavigera from Different Distribution Regions by Using Hydrophilic Interaction Ultra-Performance Liquid Chromatography Coupled with Triple Quadrupole Tandem Mass Spectrometry Tue, 28 Jul 2015 12:12:10 +0000 Thais clavigera, as function food, is distributed widely along the coasts of China. To compare and tap its potentially nutritional and functional values, hydrophilic interaction ultra-performance liquid chromatography coupled with triplequadrupole tandem mass spectrometry (HILIC-UPLC-TQ-MS/MS) was used for simultaneous identification and quantification of amino acids, nucleosides, and nucleobases in the extracts of T. clavigera from 19 sea areas in China, and a PCA was further performed for comparing their content variation in different distribution regions. The total contents of amino acids varied from 116.74 mg/g to 298.58 mg/g being higher than contents of nucleosides and nucleobases that varied from 2.65 mg/g and 20.49 mg/g. Among the habitats, Hainan province had content advantages on others. By PCA, samples collected from different regions were classified into three groups. For specific constituents, lysine accounted for large part of essential amino acids; glycine and taurine also play important roles in the delicate taste and health care function of it. Inosine takes up most of total contents of nucleosides and nucleobases. These results provided good data for establishing quality standard of T. clavigera related products and their further development and utilization. Yahui Ge, Yuping Tang, Sheng Guo, Xin Liu, Zhenhua Zhu, Pei Liu, and Jin-ao Duan Copyright © 2015 Yahui Ge et al. All rights reserved. Development and Validation of a GC-MS Method for the Detection and Quantification of Clotiapine in Blood and Urine Specimens and Application to a Postmortem Case Tue, 07 Jul 2015 09:35:30 +0000 Introduction. Clotiapine is an atypical antipsychotic of the dibenzothiazepine class introduced in a few European countries since 1970, efficient in treatment-resistant schizophrenic patients. There is little published data on the therapeutic and toxic concentrations of this drug. Aims. The aim of the present study is the development and validation of a method that allows the detection and quantification of clotiapine in blood and urine specimens by gas chromatography-mass spectrometry (GC-MS). Methods. Validation was performed working on spiked postmortem blood and urine samples. Samples were extracted with liquid-liquid extraction (LLE) technique at pH 8.5 with n-hexane/dichloromethane (85/15 v/v) and analysis was followed by GC-MS. Methadone-d9 was used as internal standard. Results. The limit of detection (LOD) was 1.2 and 1.3 ng/mL for urine and blood, respectively, while the lower limit of quantification (LLOQ) was 3.9 and 4.3 ng/mL, respectively. Linearity, precision, selectivity, accuracy, and recovery were also determined. The method was applied to a postmortem case. The blood and urine clotiapine concentrations were 1.32 and 0.49 μg/mL, respectively. Conclusions. A reliable GC-MS method for the detection and quantification of clotiapine in blood and urine samples has been developed and fully validated and then applied to a postmortem case. Giulio Mannocchi, Flaminia Pantano, Roberta Tittarelli, Miriam Catanese, Federica Umani Ronchi, and Francesco Paolo Busardò Copyright © 2015 Giulio Mannocchi et al. All rights reserved. Production of Sterilizing Agents from Calendula officinalis Extracts Optimized by Response Surface Methodology Thu, 07 May 2015 11:30:04 +0000 The aim of this study was to produce hand sterilizing liquid and wet wipes with the extracts of Calendula officinalis. Since this plant has well known antimicrobial activity due to its phytochemical constituents, the increase in the extraction yield was chosen as the principle part of the production process. To achieve the maximum yield, parameters of solid-to-liquid ratio, extraction temperature, and time were studied. The optimum conditions were determined by response surface methodology as 41°C, 7 h, and 3.3 g/200 mL for temperature, time, and solid-to-liquid ratio, respectively. The yield achieved at those conditions was found to be 90 percent. The highest amounts of flavonoids were detected at optimum, whereas the highest triterpene and saponin constituents were determined at different design points. The microbial efficiencies of extracts were determined by the inhibition of the growth of selected microorganisms. Different dilution rates and interaction times were used as parameters of inhibition. Not any of the constituent but symbiotic relation in-between reached the highest inhibition of 90 percent. The pH values of the extracts were 5.1 to 5.4. As a result, the extraction of Calendula officinalis at the optimum conditions can be used effectively in the production of wet wipes and hand sterilizing liquid. Fatih Mehmet Goktas, Bilgesu Sahin, and Sibel Yigitarslan Copyright © 2015 Fatih Mehmet Goktas et al. All rights reserved.