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Journal of Analytical Methods in Chemistry

Lingzhi Zhao, Liu Zhao, Yanqing Miao, Chunye Liu, Chenxiao Zhang
The detection of pyrophosphatase (PPase) activity is of great significance in diagnosing diseases and understanding the function of PPase-related biological events. This study constructed a turn off-on-off fluorescent system for PPase activity assay based on PPase-regulated competitive coordination of Cu(2+) between a water-soluble fluorescent probe 6,7-dihydroxycoumarin (DHC) and pyrophosphate (PPi). The probe DHC can coordinate with Cu(2+) and consequently display on-off type fluorescence response. Furthermore, the in situ formed nonfluorescent Cu(2+)-DHC complex can act as an effective off-on type fluorescent probe for sensing PPi due to the higher coordination reactivity between Cu(2+) and PPi than that between Cu(2+) and DHC...
2016: Journal of Analytical Methods in Chemistry
Lidiane Raquel Verola Mataveli, Márcia Liane Buzzo, Luciana Juncioni de Arauz, Maria de Fátima Henriques Carvalho, Edna Emy Kumagai Arakaki, Richard Matsuzaki, Paulo Tiglea
This study is aimed at investigating a suitable method for rice sample preparation as well as validating and applying the method for monitoring the concentration of total arsenic, cadmium, and lead in rice by using Inductively Coupled Plasma Mass Spectrometry (ICP-MS). Various rice sample preparation procedures were evaluated. The analytical method was validated by measuring several parameters including limit of detection (LOD), limit of quantification (LOQ), linearity, relative bias, and repeatability. Regarding the sample preparation, recoveries of spiked samples were within the acceptable range from 89...
2016: Journal of Analytical Methods in Chemistry
Carlos Cardoso-Palacios, Ingela Lanekoff
Counterfeit pharmaceutical drugs imply an increasing threat to the global public health. It is necessary to have systems to control the products that reach the market and to detect falsified medicines. In this work, molecules in several pharmaceutical tablets were directly analyzed using nanospray desorption electrospray ionization mass spectrometry (nano-DESI MS). Nano-DESI is an ambient surface sampling technique which enables sampling of molecules directly from the surface of the tablets without any sample pretreatment...
2016: Journal of Analytical Methods in Chemistry
Chalder Nogueira Nunes, Lucas Ely Pauluk, Maria Lurdes Felsner, Vanessa Egéa Dos Anjos, Sueli Pércio Quináia
17α-Ethinyl estradiol (EE2), which is used worldwide in the treatment of some cancers and as a contraceptive, is often found in aquatic systems and is considered a pharmaceutically active compound (PhACs) in the environment. Current methods for the determination of this compound, such as chromatography, are expensive and lengthy and require large amounts of toxic organic solvents. In this work, a voltammetric procedure is developed and validated as a screening tool for detecting EE2 in water samples without prior extraction, clean-up, or derivatization steps...
2016: Journal of Analytical Methods in Chemistry
Thamani T Gondo, Veronica C Obuseng, Lesego C Mmualefe, Harriet Okatch
HS-SPME was optimised using blank plant sample for analysis of organochlorine pesticides (OCPs) of varying polarities in selected medicinal plants obtained from northern part of Botswana, where OCPs such as DDT and endosulfan have been historically applied to control disease carrying vectors (mosquitos and tsetse fly). The optimised SPME parameters were used to isolate analytes from root samples of five medicinal plants obtained from Maun and Kasane, Botswana. The final analytes determination was done with a gas chromatograph equipped with GC-ECD and analyte was confirmed using electron ionisation mass spectrometer (GC-MS)...
2016: Journal of Analytical Methods in Chemistry
Xiaodong Wei, Hongling Shen, Lijun Wang, Qingyan Meng, Wenjie Liu
A comprehensive two-dimensional (2D) reverse phase (RP) liquid chromatography (LC) method is developed for alkaloid analysis. This offline comprehensive 2D method is developed using different pH values. With a pH value of 10.5, most alkaloids appear in the form of neutral molecules possessing high retention factors based on their polarity, while the alkaloid polarity order is changed when the pH value decreased to 3.0. The performance of pH modulated 2D LC is demonstrated with 8 alkaloid standards which resulted in orthogonal separation...
2016: Journal of Analytical Methods in Chemistry
Yang Liu, Zhaoxia Liu, Huaxin Yang, Lan He
Quantitative nuclear magnetic resonance (qNMR) is a powerful tool in measuring drug content because of its high speed, sensitivity, and precision. Most of the reports were based on proton qNMR ((1)H qNMR) and only a few fluorine qNMR ((19)F qNMR) were reported. No research has been conducted to directly compare the advantage and disadvantage between these two methods. In the present study, both (19)F and (1)H qNMR were performed to characterize the content of atorvastatin calcium with the same internal standard...
2016: Journal of Analytical Methods in Chemistry
Alireza Feizbakhsh, Amir Hossein Mohsen Sarrafi, Shokooh Ehteshami
Polythiophene/chitosan magnetic nanocomposite as an adsorbent of magnetic solid phase extraction was proposed for the isolation of fluoxetine in aqueous and biological samples prior to fluorescence detection at 246 nm. The synthesized nanoparticles, chitosan and polythiophene magnetic nanocomposite, were characterized by scanning electron microscopy, FT-IR, TGA, and EDAX. The separation of the target analyte from the aqueous solution containing the fluoxetine and polythiophene/chitosan magnetic nanocomposite was simply achieved by applying external magnetic field...
2016: Journal of Analytical Methods in Chemistry
Haiqing Yu, Joann J Lu, Wei Rao, Shaorong Liu
Density gradient centrifugation is widely utilized for various high purity sample preparations, and density gradient ultracentrifugation (DGU) is often used for more resolution-demanding purification of organelles and protein complexes. Accurately locating different isopycnic layers and precisely extracting solutions from these layers play a critical role in achieving high-resolution DGU separations. In this technique note, we develop a DGU procedure by freezing the solution rapidly (but gently) after centrifugation to fix the resolved layers and by slicing the frozen solution to fractionate the sample...
2016: Journal of Analytical Methods in Chemistry
Shiva Ram Bhandari, Jun Gu Lee
To evaluate the ripening-dependent changes in phytonutrients, seven commercial cultivars (two general and five cherry) of tomatoes were cultivated under greenhouse conditions. Fruits were harvested at breaker, turning, pink, light red, and red stages of each cultivar, and antioxidant contents, color attributes, and antioxidant activities were measured. During ripening process, lycopene content increased from the breaker to red stage, while lutein displayed the reverse accumulation pattern, with higher values during the breaker stage...
2016: Journal of Analytical Methods in Chemistry
Ali Gholami, Atefeh Mohsenikia, Saeed Masoum
Formaldehyde is commonly used in detergents and cosmetic products as antibacterial agent and preservative. This substance is unfavorable for human health because it is known to be toxic for humans and causes irritation of eyes and skins. The toxicology studies of this compound indicate risk of detergents and cosmetic formulations with a minimum content of 0.05% free formaldehyde. Therefore, determination of formaldehyde as quality control parameter is very important. In this study, a photoluminescence method was achieved by using 2-methyl acetoacetanilide...
2016: Journal of Analytical Methods in Chemistry
Lígia Pimentel, Ana Gomes, Manuela Pintado, Luis Miguel Rodríguez-Alcalá
The lipid fraction of milk is one of the most complex matrixes in foodstuffs due to the presence of a high number of moieties with different physical and chemical properties. Glycerolipids include glycerol and two fatty acids esterified in positions sn-1 and sn-2 with higher concentration of unsaturated fatty acids than in the triglyceride fraction of milk. Sphingolipids consist of a sphingoid base linked to a fatty acid across an amide bond. Their amphiphilic nature makes them suitable to be added into a variety of foods and recent investigations show that phospholipids, mainly phosphatidylserine and sphingomyelin, can exert antimicrobial, antiviral, and anticancer activities as well as positive effects in Alzheimer's disease, stress, and memory decline...
2016: Journal of Analytical Methods in Chemistry
Stefano Gentili, Renata Solimini, Roberta Tittarelli, Giulio Mannocchi, Francesco Paolo Busardò
The reliability of DrugWipe 5A on site test for principal drugs of abuse (cannabis, amphetamines, cocaine, and opiates) detection in oral fluid was assessed by comparing the on-site results with headspace solid-phase microextraction (HS-SPME) gas chromatography-mass spectrometry (GC-MS) analysis on samples extracted by the device collection pad. Oral fluid samples were collected at recreational settings (e.g., discos, pubs, and music bars) of Rome metropolitan area. Eighty-three club goers underwent the on-site drug screening test with one device...
2016: Journal of Analytical Methods in Chemistry
Jae Sung Pyo
A gas chromatography-mass spectrometry (GC-MS) method for the determination of propofol in human plasma has been developed and validated. Propofol was extracted from human plasma by using mixed-mode cation exchange/reversed-phase (MCX) cartridges. As propofol easily volatilizes during concentration, 100% methanol was injected directly into GC-MS to elute propofol. Despite avoiding concentration process of the eluted solution, lower limit of quantization (LLOQ) of propofol was 25 ng/mL. The validated method exhibited good linearity (R (2) = 0...
2016: Journal of Analytical Methods in Chemistry
Shunjun Xu, Jiejing Yu, Liu Yang, Yaling Zhu, Shuai Sun, Zhengdi Xu
Chuan-Ke-Zhi (CKZ), a purified Herba Epimedii extract, is a potent Chinese medicine preparation whose main bioactive components are a class of flavonoid glycosides such as epimedins A, B, and C and icariin. And epimedin C is far more abundant than other flavones in this extract. This study aims to investigate the pharmacokinetic and bioavailability of epimedin C and what effects, if any, other ingredients in CKZ have on its pharmacokinetics. Epimedin C, CKZ, and a combination of epimedins A, B, and C and icariin were, respectively, administrated to rats, and then the pharmacokinetic parameters of epimedin C in the three groups were calculated and compared...
2016: Journal of Analytical Methods in Chemistry
Rosa E Gavilán, Carolina Nebot, Maria Veiga-Gómez, Paula Roca-Saavedra, Beatriz Vazquez Belda, Carlos M Franco, Alberto Cepeda
The Commission Regulation 574/2011/EC set up maximum levels of coccidiostats and histomonostats in nonmedicated feed as a consequence of carry-over during manufacturing. Carry-over takes place from medicated to nonmedicated feed during feed production. Similar contamination could also occur for other pharmaceuticals such as tetracyclines, a group of antibiotics commonly employed in food production animal. The objective of this work is to present a simple and fast method for the simultaneous detection of four tetracyclines (chlortetracycline, doxycycline, oxytetracycline, and tetracycline) in nontarget feed at a μg/kg level...
2016: Journal of Analytical Methods in Chemistry
Deysiane Oliveira Brandão, Geovani Pereira Guimarães, Ravely Lucena Santos, Fernando José de Lima Ramos Júnior, Karla Monik Alves da Silva, Fabio Santos de Souza, Rui Oliveira Macêdo
Momordica charantia is a species cultivated throughout the world and widely used in folk medicine, and its medicinal benefits are well documented, especially its pharmacological properties, including antimicrobial activities. Analytical methods have been used to aid in the characterization of compounds derived from plant drug extracts and their products. This paper developed a methodological model to evaluate the integrity of the vegetable drug M. charantia in different particle sizes, using different analytical methods...
2016: Journal of Analytical Methods in Chemistry
Catarina Varanda, Inês Portugal, Jorge Ribeiro, Artur M S Silva, Carlos M Silva
Over the recent years, bitumen modification with polymers, acids, or mineral fillers has gained relevance to adjust its performance properties. This work reports the use of polyphosphoric acid (PPA) for the modification of formulated bitumen. With this objective, an in-depth literature review on PPA modification was firstly performed. Subsequently, five individual refinery components were selected for the preparation of bitumen blends, namely, asphaltic residue, vacuum residue, and three lube oils extracts...
2016: Journal of Analytical Methods in Chemistry
U Gianfranco Spizzirri, Nevio Picci, Donatella Restuccia
Biogenic amines (BAs), that is, spermine, spermidine, putrescine, histamine, tyramine, β-phenylethylamine, cadaverine, and serotonin, have been determined in several samples of tea leaves, tea infusions, and tea drinks by LC-UV method after derivatization with dansyl chloride. Different extraction solvents have been tested and TCA 5% showed better analytical performances in terms of linearity, recovery percentages, LOD, LOQ, and repeatability than HCl 0.1 M and HClO4 0.1 M and was finally exploited for the quantitative determination of BAs in all samples...
2016: Journal of Analytical Methods in Chemistry
L Cossignani, D Montesano, M S Simonetti, F Blasi
Stereospecific analysis is an important tool for the characterization of lipid fraction of food products. In the present research, an approach to characterize arabica and robusta varieties by structural analysis of the triacylglycerol (TAG) fraction is reported. The lipids were Soxhlet extracted from ground roasted coffee beans with petroleum ether, and the fatty acids (FA) were determined as their corresponding methyl esters. The results of a chemical-enzymatic-chromatographic method were elaborated by a chemometric procedure, Linear Discriminant Analysis (LDA)...
2016: Journal of Analytical Methods in Chemistry
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