SM Analytical and Bioanalytical Techniques

Archive Articles

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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*