SM Analytical and Bioanalytical Techniques

Archive Articles

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Sorption Properties of Methyl Orange onto Chemically Modified Chitosan: Thermodynamics and Kinetics Studies

A new kind of sorbent with high adsorption capacity and stability was prepared using chitosan and epichlorohydrin through a cross-linking reaction and assessed by using methyl orange. The sorption capability was evaluated by means of kinetics and equilibrium studies. Relevant factors for such sorption process were also assessed. After optimization of the relevant sorption factors, the percentages for methyl orange removal by chitosan and by modified chitosan were 82%, and 67%, respectively. Although the cross-linked chitosan offered the lowest removal percentage, this sorbent presented other relevant advantages when compared to non-modified chitosan, such as higher chemical and thermal stabilities.

Juliana CM Caje, Paula Marcelle de Oliveira, Felipe S Semaan, Raphael C Cruz, Ricardo J. Cassella and Wagner F. Pacheco


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Quantitative Headspace Solid-Phase Microextraction Gas Chromatography Mass Spectrometry (HS-SPME-GC-MS/ MS) Method for the Determination of Tributyltin in Sediment: Validation according to EU Directive Requirement

The Directive 2013/39/EU has reviewed the list of priority substances under the European Water Framework Directive (WFD; Directive 2000/60/EC) and has strengthened the principle of flexibility for Member States in applying the Environmental Quality Standard (EQS) for alternative matrices. Coherently, it has established new EQS for biota and it has invited Member States to set EQS for more opportune matrices, able to advantage the monitoring strategy and offer the same level of protection, such as sediment. The present work developed a (HS)SPME-GC-MS/MS method for the analysis of Tributyltin (TBT) in sediment samples and, through an in depth validation process, it assessed the compliance with the technical specification required by the EU Directive 2009/90/EC for chemical status analysis under the scope of the WFD. The EQS established for TBT in sediment by the Italian Environmental Ministry was used as reference. The method fulfils the minimum performance criteria required by the EU Directive 2009/90/EC (Method Detection Limit (MDL) and Minimum Level Of Quantitation (ML), expressed as ng Sn g-1 d.w., were 0.2 and 0.5, respectively). More generally, the analytical figures of merit achieved, were satisfying for the target TBT concentration range (recovery: 90-111%, intermediate precision range: 6-12%).

Seta Noventa¹, Malgorzata Formalewicz¹, Jvan Barbaro², Claudia Gion¹, Federico Rampazzo¹, Massimo Gabellini³, Rossella Boscolo¹, and Daniela Berto¹*

 


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Method Development and Validation for the Determination of Pravastatin in Human Plasma by Lc-Ms/Ms

A simple, rapid, sensitive and selective liquid chromatography/tandem mass spectrometry (LC/MS/MS) method was developed and validated for the quantification of pravastatin in human plasma. Pravastatin-D3 was used as an internal standard. The analyte was extracted from human plasma samples by liquid-liquid extraction technique. Due to the presence of isobaric metabolites, 3α-iso-pravastatin and 6-epi-pravastatin, chromatographic conditions were optimized, with a C18 column by using a mixture of 0.1% acetic acid in water and acetonitrile/ methanol (43:57,v/v) as the mobile phase at a flow rate of 0.6 mL/min. The calibration curve obtained was linear (r2 ≥ 0.9900) over the concentration range of 0.500-500 ng/mL. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. The method was suitable for supporting clinical studies.

Lian Chen, Paresh Joshi, Andrii Piatkivskyi, Kalem Aguilar, and Jenny Lin*


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Cramer Rao Lower Bound CRB Shape Detection Method

In this paper we investigate the problem of tracking a moving but non-vibrating cylindrical object and estimating its size and shape using an artificial lateral line system, an d determine the lower bound that the estimator can be reached. Based on a nonlinear analytical model for the moving object-induced flow field, a two-stage extended Kalman filter is proposed to estimate the location, velocity, size, and shapes of the object. Simulation results on tracking an ellipsoidal cross-section are presented to illustrate the approach.

Ahmad T Abdulsadda*


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A Study on Semi-Late Maize Hybrids for Resistance to Smut of Maize /Ustilago maydis/

The most efficient method of controlling diseases of economic importance in agricultural crops is breeding of resistant varieties. The objective of the study was to determine the extent of the attack of smut of maize /Ustilago maydis/ on 22 hybrids and 4 maize standards under conditions, conducive to the spread of the pathogen.

The study was conducted in the experimental fields of the Institute of Agriculture and Seed Science “Obraztsov Chiflik”, Ruse during the period 2012 - 2014. 26 germplasms of Preliminary Variety Trial N 2 (PVT) were included.

Ustilago maydis is a common disease in most parts of the world, where maize is grown. In all above-ground organs of the plant, tumors of smutty mass are formed. The pathogen attack leads to stunted growth of the host plant, reducing yield, and economic losses.

The analysis of data about the new hybrids of IASS “Obraztsov Chiflik” - Ruse showed that fifteen of them were resistant.

The resistance was the highest in the hybrids: St.20, Eks.12, Eks.10, Eks.23, Eks.16, Eks.2, Eks.3, Eks.4, Eks.6, Eks.9, Eks.13, Eks.17, Eks.19, Eks.20, 2 Eks.6. They may be used as sources of resistance. Susceptible were: Eks.15, Eks.11, Eks.8, Eks.24, Eks.1, Eks.5, St.7, Eks.14, Eks.18, Eks.22, Eks.25.

Iliana Ivanova, Lyubomir Ivanov, and Gergana Ivanova*


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Composition and Antioxidant Activity of Vitex agnus-castus L and Rosmarinus Officinalis L. Leaves Essential Oils Cultivated in Syria

Medicinal plants contain a wide variety of chemicals which have very important roles in numerous applications including medicinal and those related with industry. Essential oils represent valuable sources for natural antioxidants. The aim of our study was to evaluate the chemical composition and antioxidant activity of the essential oils extracted from leaves of Syrian Vitex agnus-castus L. and Rosmarinus officinalis L., where is both essential oils were extracted and analyzed by gas chromatography-mass spectrometry. The antioxidant activities of these essential oils were determined by three different test systems, scavenging effect on 2,2-diphenyl-1-picrylhydrazyl radical, total phenolic and flavonoids contents. The main constituents found in Vitex agnus-castus L. essential oil were 1,8-Cineole (19.34%) and Sabinene (12.50%), while the major constituents in Rosmarinus officinalis L. essential oil were 1,8-Cineole (28.03%) and α-Pinene (14.70%). The results showed that 2,2-diphenyl-1-picrylhydrazyl radical scavenging and total phenolic contents of Vitex agnus-castus L. essential oil were higher than Rosmarinus officinalis L. essential oil. Total flavonoids contents were not detected in both essential oils. The Vitex agnus-castus L. and Rosmarinus officinalis L. essential oils are sources of natural antioxidants. Therefore, further work is needed to identify the compound(s) responsible for the antioxidant activity of Vitex agnus-castus L. and Rosmarinus officinalis L. essential oils.

Faten Al Saka, Manal Daghestani, and Francois Karabet*


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A Validated Reversed Phase HPLC Method for Simultaneous Determination of the antihistaminic Cetirizine and Beta2-adrenergic agonist Salbutamol in their Co-formulated Tablets

New HPLC method is adopted in this research for simultaneous determination of Cetirizine (CTZ) and salbutamol (SAL) in their tablets. The developed method used C18 column and a mobile phase composed of methanol: 0.1M phosphate buffer in the ratio (80:20 v/v) operating at pH 3.5.Nimsulide was used as internal standard (IS).The peak area ratio - concentration plot indicated the linearity over ranges of 5-50 and 4-80µg/mL for CTZ and SAL with limit of detection of 0.57 and 2.00µg/mL respectively. Comparing the proposed method with a comparison method revealed that there was no significant difference between the two methods in regards to accuracy and precision.

Fatma Ahmed Aly, Nahed EL-Enany, Heba Elmansi* and Amany Nabil 


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Relationship between Wheat Head Blight Levels and Deoxynivalenol, Deoxynivalenol-3-Glucoside Contents

Field wheat panicles infected with and without wheat head blight were collected in 2012 from Jiangsu province where Fusarium Head Blight (FHB) is prevalent. The collected panicles infected with FHB were assessed in the laboratory for Disease Severity Levels (DSL). A series of wheat samples with varying Rate of Diseased Panicles (RDP) and varying DSL were prepared by adding diseased panicles to healthy ones and analyzed using Ultra-Performance Liquid Chromatography Tandem Mass Spectrometry (UPLC-MS/MS) for their Deoxynivalenol (DON) and Deoxynivalenol-3-Glucoside (D3G) contents. Consistent increases of DON and D3G levels were observed as the RDP and DSL of the wheat samples were enhanced, showing a distinct linear correlation between disease index (DI) of wheat head blight and DON and D3G content. The linear regression models were calculated as YDON =257.78XDI +2315.61 (r=0.96) and YD3G =41.81XDI-43.79 (r=0.96). The models were validated with field samples collected in 2013 and showed a good fit for variation trends, but overestimated DON content and underestimated D3G content.

Huijie Zhang¹,², Li Wu¹,², Juan Sun¹,², Yan Zhang¹,², Xiaoli Dong¹,², Weixi Li¹,², Xuexu Hu¹,², Lijuan Sun¹,², and Bujun Wang¹,²*


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Environmental Dioxin Pollution and its Influence on the African Americans

Dioxins are a group of chemically-related compounds that are persistent environmental pollutants and are formed as an unintentional by-product of many industrial processes involving chlorine such as waste incineration, chemical and pesticide manufacturing and pulp and paper bleaching. Some toxicity of other dioxins and chemicals like PCBs that act like dioxin are measured in relation to TCDD. However, dioxin is a general name for a large group of chemical compounds with similar structure. These compounds are made up of the number of the chlorine atoms and their positions in the dioxin molecule are what determine the toxicity of different dioxins. Dioxin is formed by burning chlorine-based chemical compounds with paper mills which use chlorine bleaching in their process and with the production of Polyvinyl Chloride (PVC) plastics and with the production of certain chlorinated chemicals. In September 1994, by the U.S, Environmental Protection Agency clearly describes dioxin as a serious public health threat. According to the EPA report, not only does there appear to be no “safe” level of exposure to dioxin, but levels of dioxin and dioxin-like chemicals have been found in the general U.S population that are at or near levels associated with adverse health effects. Dioxin was the primary toxic component of Agent Orange, which was found at Love Canal in Niagara Falls, NY and was the basis for evacuations at Times Beach, MO and Seveso, Italy. The most toxic compound is 2, 3, 7, 8 - Tetrachlorodibenzo - Para - Dioxin or TCDD.

Prabir K Mandal*, Aaliyah Tomkins, Anita Mandal and Jakori Duffy 


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Formulations Prepared with Bioadhesive Polymers for Application in Vaginal Mucosa

T he vaginal lumen is affected by several pathologies - most of them are vaginitis caused by bacteria, fungi, protozoa or viruses. A considerable number of antimicrobial, antiviral, antifungal and antiprotozoal drugs have been therefore traditionally administered into this site, as well as spermicidal agents, prostaglandins and steroids.

Maíra N Pereira and Guilherme M Gelfuso* 


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Volatile Compounds of Freshly Prepared Lemon Juice from the Region of Kalamata

Background: Lemon is a favorable fruit due to its vitamin C content and numerous other applications in the daily diet

Aim: The aim of this study was to investigate the volatile profile of lemon juice prepared from home cultivated lemon trees in the region of Kalamata

Methods: Lemons (Maglini cv.) cultivated in home gardens were collected, washed and hand squeezed lemon juice was prepared. The volatile pattern was determined using solid phase micro extraction coupled to gas chromatography mass spectrometry (HS-SPME-GC/MS).

Results: Results showed that the volatile fraction of lemon juice was largely dominated by terpenoids. Limonene was the most abundant volatile compound followed by γ-terpinene, sabinene and neryl acetate.

Conclusion: Lemon juice from Kalamata is a rich source of terpenoids, especially limonene, and may be considered in adding valuable sensory characteristics or health benefits in other commercially available juices, food products, or specific pharmaceutical supplements.

Ioannis K Karabagias


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Statin-updates

Cholesterol common part of cell membrane is transported in blood in form of particles containing lipids and proteins called lipoproteins. Level of Low Density Lipoprotein (LDL-c) associate with Cardio Vascular Disease (CVD) and level of High Density Lipoprotein (HDL-c) are related with a lower risk of such disease. Many medications are available for lipid lowering therapy and statin is first line drug. From the introduction of Lovastatin in 1978 to pitavastatin till now, the research has not been finished in findings of beneficial to adverse events of statin. Many face to face clinical studies was reported to explain statin role in lipid profile modification, pleiotropic effects, pharmacodynamic and kinetics, lipophilicity, adverse event reporting, dose/dosage recommended etc. This review gives the update of such trials.

Selvasudha Nandakumar¹, Kailasam Koumaravelou², and Sridurga Devi N³*


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Microscopic Identification of Vine Black Pigment In A Tempera Painting By Francisco De Goya

This paper aims to advance our understanding of the morphological differentiation of vine black pigment encountered in a monochrome painting on alabaster produced by Francisco de Goya: Maja y Celestina.

1) Micro-Raman Spectroscopy (mRS) applied “in situ”, focusing the laser directly on to the surface of the work and also on the stratigraphy prepared via a micro sample of the painting.

2) Scanning Electron Microscopy connected to an Energy-Dispersive X-Ray spectroscopy system (SEM-EDX), applied to the stratigraphy and also to a small portion of black-paint powder, scrapped from the edge of the work.

3) Visible and near-infrared spectrophotometry, applied “in situ” on to the surface of the picture. The results obtained via the mRS are inconclusive, as is the case with the results obtained via visible and near-infrared spectrophotometry.

However, observation of the high magnifications enabled by the scanning electron microscopy and EDX microanalysis have allowed us to identify morphologically vine black pigment, which are combined with one another black pigment (lamp black) to form the single color present in the painting.

Thus, in the case of vine black pigment, polygonal forms were observed that may indicate the rigid walls characteristic of vegetable cells, given its botanical origin.

Gold leaf particles were also found, added to the mix of blacks, and we believe that they may be indicative of Goya’s aesthetic decisions, adding brightness and warmth to the dark color. Furthermore, a range of other pigments were also identified: lead white, bone black and black iron oxides, which, in principle, we attribute to contamination in the workshop.

The black pigments that were identified are bound together by a mixture of linseed oil and egg yolk, denoting a tempera grass painting technique.

Highlights

This study focuses on the first work executed on an alabaster board that is classified as an original by Francisco de Goya [1].

• The painting involves a pictorial composition rendered exclusively in black.

• Via SEM-EDX it has been possible to morphologically differentiate vine black pigment based on the cellular

• Polygonal shapes were observed with SEM and may indicate the rigid walls characteristic of vegetable cells.

• This innovative study proposes the morphological characterization of vine black pigment.

Luis Rodrigo Rodríguez-Simón¹, Vicente Del Sol López², and Miguel Ángel León Coloma³*