Optimization of Four Different Rosemary Extraction Techniques Using Plackett-Burman Design and Comparison of Their Antioxidant Compounds.

Rosemary has many medicinal and therapeutic properties and therefore it is important to study how to maximize the recovery of its bioactive compounds. In the present study, four different extraction techniques were used, namely stirring extraction (STE), pulsed electric field-assisted extraction (PEF), ultrasound probe-assisted extraction (UPAE), and ultrasound bath-assisted extraction (UBAE). First, some primary experiments were carried out in order to optimize each technique individually through the Plackett-Burman design. Then, each technique was applied under optimal conditions and the results were compared with each other. The optimal total polyphenol content (TPC) of STE is ~19 mg gallic acid equivalents per gram of dry weight (dw), while the antioxidant activity of the extract is 162 µmol ascorbic acid equivalents (AAEs) per gram of dw via FRAP and ~110 µmol AAE per gram of dw via DPPH. As for PEF, the optimal TPC is ~12 mg GAE/g dw, and the FRAP and DPPH values are ~102 and ~70 µmol AAE per gram of dw, respectively. When it comes to UPAE, the optimal TPC is ~16 mg GAE/g dw and the antioxidant capacity of the extract is ~128 µmol AAE/g dw through FRAP and ~98 µmol AAE/g dw through DPPH. UBAE optimal extract yielded ~17 mg GAE/g dw TPC, ~146 µmol AAE/g dw for FRAP, and ~143 µmol AAE/g dw for DPPH. The highest flavonoid content (~6.5 mg rutin equivalent/g dw) and DPPH (~143 µmol ascorbic acid equivalent/g dw) is obtained through UBAE. UPAE has been shown to be more efficient in recovering ascorbic acid (~20 mg/g dw). Additionally, the chlorophyll-to-carotenoid ratios of UPAE and UBAE were 2.98 and 2.96, respectively, indicating that the extracts had a generally positive impact on health. Considering the environmental impact of each extraction technique but also which antioxidant factor needs to be maximized, the most suitable extraction technique will be chosen.

Effect of ultrasonic treatment during fermentation on the quality of fortified sweet wine.

The present study aimed to investigate the potential of ultrasonic treatment during fermentation for enhancing the quality of fortified wines with varying time and power settings. Chemical analysis and sensory evaluation were conducted to assess the impact of ultrasonic treatment on wine quality. Results showed that ultrasonic treatment could increase total anthocyanin and total phenol content, reduce anthocyanin degradation rate, and improve color stability. Moreover, ethyl carbamate content was lower in the ultrasonic group after aging compared to non-ultrasonic group. A combination of 200 W for 20 min resulted in higher sensory scores and more coordinated taste, while a combination of 400 W for 40 min produced higher levels of volatile compounds (21860.12 µg/L) leading to a richer and more elegant aroma. Therefore, ultrasound can be used as a potential technology to improve the quality of wine.

Should we think about green or white analytical chemistry? Case study: Accelerated sample preparation using an ultrasonic bath for the simultaneous determination of Mn and Fe in beef.

Green Analytical Chemistry (GAC) metrics include a variety of criteria, such as the regent amounts and toxicity, energy consumption, generated waste, among others. The analytical greenness metric (AGREE) and its variant for sample preparation (AGREEprep) cover different aspects that contribute to the environmental sustainability of sample preparation. White Analytical Chemistry (WAC) considers not only environmental aspects but also analytical and practical aspects with a holistic vision based on a Red-Green-Blue color model. A case study is presented to assess the green and white profile of a method based on ultrasound-assisted extraction and determination of Mn and Fe in beef using microwave-induced plasma atomic emission spectroscopy (MP AES). The method was validated and resulted simple, fast without external heating using diluted acids. It was concluded that we should think in green sample preparation with the AGREEprep tool, as well as in white holistic assessments (WAC) as both constitute complementary tools.

A comparative study on the influence of single and combined ultrasounds assisted flake graphite flotation.

Ultrasound has emerged as a promising technique for improving the mineral flotation performance. However, limited research exists regarding the influence of different ultrasound types on the flotation process. Specifically, the impact of combined ultrasound and the comparison of horn- and bath-type ultrasounds on flotation have not been fully investigated. To address this knowledge gap, a comprehensive study to explore the effects of different ultrasonic pretreatments on the flotation of flake graphite was conducted. A Box-Behnken design is employed to analyze the effects of combined ultrasound on graphite flotation. By characterizing the properties of graphite samples before and after the ultrasonic treatment, the aim is to elucidate the mechanism underlying the impact of ultrasound on graphite flotation. The experimental results indicated that the ultrasonic cavitation intensity exerted a significant influence on the graphite flotation recovery. Both horn- and bath- type ultrasounds contributed to flotation, but horn-type ultrasound demonstrated a more pronounced effect, leading to a 7% increase in flotation recovery, whereas bath-type ultrasound resulted in only a 2% increase. Furthermore, the cavitation intensity of combined ultrasound was found to be higher than that of single-frequency ultrasound in the same duration. However, the performance of graphite flotation was better with short duration combined ultrasound pretreatment, while the opposite trend was observed for a long duration ultrasound pretreatment. These findings may inform the development of more efficient and effective ultrasonic pretreatments for flotation separation processes.

Silica extraction from rice hull ash through the sol-gel process under ultrasound.

Rice is among the main foods produced in the world and is part of the daily diet of most families. The main waste from rice processing is rice husk (RH), which has been used as biomass for energy generation through combustion. In this process, rice husk ash (RHA) is generated as a residue, and its silica (SiO2) content varies from 85 to 98%. The present work describes the study of the extraction of silica from RHA by the ultrasound-assisted sol-gel method. An experimental design based on the response surface methodology (RSM) with the symmetrical, second-order rotational central composite design (RCCD) was applied to determine the best extraction conditions considering extraction time and molar ratio (n) as variables = nNaOH/nSilica). These optimal conditions were then applied to three ash samples, two obtained by the combustion process in a boiler furnace, with a mobile grate system (RHAC1 and RHAC2), and one obtained by the pyrolysis process (RHAP) carried out in a fixed bed reactor. Results showed that a molar ratio of 4.4, and an extraction time of 107 min were the best extraction conditions, leading to a yield of 73.3% for RHAP, 43.9% for RHAC1, and 31.1% for RHAC2. It was found that the extraction yield and textural properties of the silica obtained depend on the characteristics of the ash used. The silica extracted from RHAC1 presented a surface area of 465 m2.g-1, mesopores of 4.69 nm, purity greater than 95%, and an ultra-fine granulometric distribution, reaching nanoparticle dimensions, characteristics comparable to commercially available silicas.

The Effect of Ultrasonic Treatment on the Binding of the Inclusion Complex ß-Cyclodextrin-peppermint Oil with Cellulose Material.

The purpose of the research was to measure the increase in the binding of inclusion complexes ß-cyclodextrin-peppermint oil (ß-CD_PM) to cellulose in cotton and cotton/polyester material with BTCA as the crosslinking agent by applying an ultrasonic bath at room temperature and a frequency of 80 kHz for 10 min. After sonication, the samples were left in a bath for 24 h after which they were dried, thermocondensed and subjected to a number of wash cycles. The treated samples were analysed with Attenuated total reflection (ATR) units heated up to 300 °C (Golden Gate (FTIR-ATR)) to monitor chemical changes indicative of crosslinking, while physico-chemical changes in the samples were monitored by using Fourier transform infrared spectroscopy (FTIR-ATR). Mechanical properties were measured according to EN ISO 13934-1:1999, and coloristic changes were evaluated by the whiteness degree according to CIE (WCIE) and the yellowing index (YI), while antimicrobial activity was determined according to AATCC TM 147-2016. The results show a physico-chemical modification of the UZV-treated cellulosic material. Moreover, partial antimicrobial efficacy on Gram-negative bacteria was confirmed for treated fabrics.

Hazelnut Shells as Source of Active Ingredients: Extracts Preparation and Characterization.

Hazelnut shells represent a waste material (about 42% of the total biomass) deriving from hazelnut harvest. These are mainly used as a heating source; however, they represent an interesting source of polyphenols useful in health field. The impact on phenolic profile and concentrations of hazelnut shell extracts obtained by three extraction methods (maceration, ultrasonic bath, and high-power ultrasonic), as well as temperature, extraction time, and preventive maceration, was studied. The prepared extracts were characterized in terms of chemical composition, antioxidant and antimicrobial activities. Eighteen different phenolic compounds were identified and quantified by chemical analysis and gallic acid was the most abundant in all the extracts analyzed. Other relevant compounds were chlorogenic acid, protocatechuic acid and catechin. Preventive maceration had a positive effect on the extraction of different types of compounds regardless of the method performed. Application of the high-power ultrasonic method had different effects, either positive or negative, depending on the type of compound and extraction time. All the prepared extracts showed antioxidant activity especially those prepared by maceration, and many of them were able to inhibit the growth of both B. subtilis and B. cereus.

Sono-synthesis approach improves anticancer activity of ZnO nanoparticles: reactive oxygen species depletion for killing human osteosarcoma cells.

Aim: To investigate the effect of ultrasound during the synthesis of ZnO nanoparticles (NPs) on their anticancer activity. Materials & methods: ZnO NPs were synthesized in the presence and absence of ultrasonic irradiation. Biological tests were performed on human osteosarcoma cancer cells (Saos-2). Results: The sono-synthesized sample indicated higher cytotoxicity than the conventional one. (IC50 = 16.48 ± 0.41 µg/ml for sonochemical ZnO; 26.96 ± 0.33 µg/ml for conventional ZnO). Both sonochemical and conventional samples acted like antioxidants and reduced intracellular reactive oxygen species level. This reduction was more significant in cells treated with the sono-synthesized sample. The sono-synthesized ZnO NPs showed more tumor selectivity than the conventional sample. Conclusion: Sono-synthesis of ZnO NPs by a bath sonicator could improve their anticancer activity.

Polycyclic musk fragrances (PMFs) in wastewater and activated sludge: analytical protocol and application to a real case study.

Two different analytical methods for the determination of polycyclic musk fragrances (PMFs) in wastewater and in activated sludge were developed. PMFs in filtered water samples were determined by gas chromatography coupled with a triple-quadrupole mass spectrometer in selected reaction monitoring (SRM) mode. Activated sludge samples were extracted using an ultrasonic bath and analysed using a GC-Ion trap. The developed methods respected a linear model (R2 > 0.995). Detection limits of selected compounds (Celestolide, Galaxolide, Galaxolidone, Phantolide and Tonalide) varied from 1.7 to 80 ng L-1 for water and from 0.1 ng g-1 to 210 ng g-1 for activated sludge considering laboratory contamination for each PMF. Recovery studies were performed on spiked water samples and, for sludges, on procedural blanks, showing recoveries above 70% for all the considered compounds, while recovery of the internal standard was always above limit of acceptance (30%). Proposed methods were used to determine PMFs concentrations in wastewaters and activated sludges of a wastewater treatment plant (WWTP) located in Northern Italy. Concentrations in the range of µg L-1 of Galaxolide and of its metabolite Galaxolidone were detected even in the WWTP effluent. Biotransformation of Galaxolide into Galaxolidone occurred during biological treatment with the consequent release of this compound through WWTP effluents. In activated sludges, concentrations of all PMFs except Galaxolidone were one order of magnitude higher than wastewaters, as expected according to their physicochemical properties. Present wastewater treatment technologies were confirmed to not be efficient in removing PMFs from influent wastewaters since with only ≃ 30% of Celestolide and Tonalide were removed.

A Comparison between Ultrasonic Bath and Direct Sonicator on Osteochondral Tissue Decellularization.

BACKGROUND: Decellularization techniques have been widely used in tissue engineering recently. However, applying these methods which are based on removing cells and maintaining the extracellular matrix (ECM) encountered some difficulties for dense tissues such as articular cartilage. Together with chemical agents, using physical methods is suggested to help decellularization of tissues. METHODS: In this study, to improve decellularization of articular cartilage, the effects of direct and indirect ultrasonic waves as a physical method in addition to sodium dodecyl sulfate (SDS) as chemical agents with 0.1% and 1% (w/v) concentrations were examined. Decellularization process was evaluated by nucleus staining with hematoxylin and eosin (H and E) and by staining glycosaminoglycans (GAG) and collagen. RESULTS: The H and E staining indicated that 1% (w/v) SDS in addition to ultrasonic bath for 5 h significantly decreased the cell nucleus residue to lacuna ratio by 66%. Scanning electron microscopy showed that using direct sonication caused formation of micropores on the surface of the sample which results in better penetration of decellularization material and better cell attachment after decellularization. Alcian Blue and Picrosirius Red staining represented GAG and collagen, respectively, which maintained in ECM structure after decellularization by ultrasonic bath and direct sonicator. CONCLUSION: Ultrasonic bath can help better penetration of the decellularization material into the cartilage. This improves the speed of the decellularization process while it has no significant defect on the structure of the tissue.

Effects of high power ultrasound treatments on the phenolic, chromatic and aroma composition of young and aged red wine.

In this study, the effects of both ultrasonic bath and probe treatments on the phenolic, chromatic and aroma composition of young red wine Cabernet Sauvignon were studied and modeled by artificial neural networks (ANNs). Moreover, the effect of high power ultrasound (HPU) along with antioxidants addition (sulfur dioxide and glutathione) was investigated during 6 months of aging in bottles. Lower amplitude and temperature, shorter treatment duration and particularly lower frequency showed a more favorable and milder effect on the chemical composition of wine. In the case of the ultrasonic probe treatment, similar effect was achieved primarily by a larger probe diameter as well as lower amplitude and treatment duration. Selected ANN models showed the best predictions for the chromatic characteristics followed by total phenolics and anthocyanins. The changes induced by HPU treatment after 6 months of aging were mainly detected in the composition of phenolic compounds (both total and individual), where higher concentration of antioxidants (sulfur dioxide and glutathione) slowed down the decrease rate of these compounds during aging. However, HPU treatment did not influence most of the chromatic characteristics and aroma compounds, except lightness and fatty acids. The obtained results indicated that suitable ultrasound treatment might accelerate some aging reactions and shorten the period of wine aging.

Influence of surface treatments in flexural strength and superficial topography of a lithium disilicate ceramic / Influência dos tratamentos de superfície na resistência à flexão e na topografia superficial de uma cerâmica de dissilicato de lítio

Objective: The aim of the study was to evaluate the influence of different surface post-etching treatments in flexural strength, contact angle and surface roughness of a lithium disilicate ceramic. Material and Methods: 60 bars (16 x 2 x 4 mm) were divided in six groups (n=10): C, no treatment; HF, hydrofluoric acid for 20 s (HF) + washing (60 s), drying (30s); HFL, HF + washing (60 s), drying (30 s) and luting; HFNL, HF + washing (60 s) + neutralization with sodium bicarbonate (SB) for 40 s + washing (5s), drying (30 s) and luting; HFUL, HF + washing (60 s) + ultrasonic bath (UB) for 4 min, drying (30 s) and luting; HFNUL, HF + washing (60 s) + SB (40 s) + UB (4 min) and luting. The bars were submitted to three-points flexural strength test. 25 ceramic blocks (12 x 7 x 7 mm) were divided into five groups (n=5) to evaluate roughness and contact angle C - no treatment; HF - HF ; HFU - HF and UB for 5 min ; HFN - HF and SB; HFNU - HF, UB and SB. A scanning electron microscope (SEM) showed the surface of the samples. ANOVA one-way statistical analysis was done for comparison of results. Results: There was no statistical difference for flexural strength (p-value = 0.15) and for surface roughness (p-valor = 0.15). However, it was obtained statistically significant difference for contact angle (p-valor = 0.00). SEM images showed precipitates after the acid etching, which were removed by post-etching treatments. Conclusion: It can be concluded that the different post-etching surface treatments did not increase the flexural strength, surface roughness, but it influenced the ceramic wetting and SEM images (AU)

Objetivo: O objetivo do estudo foi avaliar a influência de diferentes tratamentos pós-condicionamento na resistência à flexão, ângulo de contato e rugosidade superficial de uma cerâmica de dissilicato de lítio. Material e Métodos: 60 barras (16 x 2 x 4 mm) foram divididas em seis grupos (n = 10): C, sem tratamento; HF, ácido fluorídrico durante 20 s (HF) + lavagem (60 s), secagem (30 s); HFL, lavagem com HF + (60 s), secagem (30 s) e cimentação; HFNL, HF + lavagem (60 s) + neutralização com bicarbonato de sódio (SB) por 40 s + lavagem (5s), secagem (30 s) e cimentação; HFUL, HF + lavagem (60 s) + banho ultrassônico (UB) por 4 min, secagem (30 s) e cimentação; HFNUL, HF + lavagem (60 s) + SB (40 s) + UB (4 min) e cimentação. As barras foram submetidas ao teste de resistência à flexão de três pontos. 25 blocos cerâmicos (12 x 7 x 7 mm) foram divididos em cinco grupos (n = 5) para avaliação da rugosidade superficial e ângulo de contato C - sem tratamento; HF - HF; HFU - HF e UB por 5 min; HFN - HF e SB; HFNU - HF, UB e SB. Um microscópio eletrônico de varredura (MEV) foi utilizado para análise da superfície das amostras. A análise estatística unidirecional ANOVA-um fator foi realizada para comparação dos resultados. Resultados: Não houve diferença estatística para a resistência à flexão (p-valor = 0,15) e para a rugosidade superficial (p-valor = 0,15). No entanto, obteve-se diferença estatisticamente significante para o ângulo de contato (p-valor = 0,00). Imagens de microscopia eletrônica de varredura mostraram a formação de precipitados após o ataque ácido, que foram removidos pelos tratamentos pós-condicionamento. Conclusão: Pode-se concluir que os diferentes tratamentos de superfície pós-condicionamento não aumentaram a resistência à flexão, rugosidade da superfície, mas influenciaram na molhabilidade da cerâmica e nas imagens em MEV.(AU)

The effect of high-energy environments on the structure of laccase-polymerized poly(catechol).

The laccase polymerization of catechol was performed using different reactors namely a water bath (WB), an ultrasonic bath (US) and a high-pressure homogenizer (HPH). The total content of free OH and the MALDI-TOF spectra of polymers obtained demonstrated that reactions are favored in the presence of high-energy environments. Higher conversion yields and polymerization degrees (DP) were obtained after polymerization using US or HPH. Molecular dynamic simulation studies supported these findings by revealing a more open enzyme active site upon environments with high molecular agitation. The higher mass transport generated by US and HPH is the main feature responsible for a higher substrate accessibility to the enzyme which contributed to produce longer polymers.

Solvent Orange 60 is a potent contact sensitizer in occupational and everyday life.

BACKGROUND: Solvent Orange (SO) 60 is a perinone-type dye that is often used in plastic materials such as spectacle frames and has been shown to cause contact allergy. The first case of SO 60 allergic contact dermatitis caused by spectacle frames was reported in 1999, and the second in 2011. We have recently seen 10 patients, of whom 6 developed dermatitis in the retroauricular/temporal area after wearing plastic spectacles. OBJECTIVES: To report the cause of the dermatitis in the 10 patients and to describe our first case with occupational SO 60 contact allergy. METHODS: In this retrospective study, patch test results of 10 patients, tested with the Swedish baseline series and our specific spectacle and/or plastic series, including SO 60 1.0% pet., in 2011-2017 were analysed. RESULTS: Ten patients, 2 males and 8 females, aged 43 to 71 years, reacted positively to SO 60 1.0% pet., namely, 4 pensioners, 2 nurses, 1 office worker, 1 teacher, 1 shop assistant, and 1 unemployed person. Four of the patients had an atopic history. Patch test reactions varied from + to +++; some had spread >20 cm outside the test area in terms of erythematous, infiltrated skin with papules. Retesting of patient no. 1 with serial dilutions of SO 60 in acetone showed positive reactions down to 1 ppm. Three patients reacted to the extracts of their earpieces. Gas chromatography-mass spectrometry was used to confirm the presence of SO 60 in 2 earpieces. CONCLUSIONS: SO 60 should be included in any spectacle patch test series that may be used. If there is a strong suspicion of contact allergy to SO 60 before patch testing, lowering the test concentration from 1.0% to 0.01% should be considered.

Intensified synthesis of medium chain triglycerides using ultrasonic reactors at a capacity of 4L.

Lipids are considered as one of the most crucial nutrients for humans and among the various classes, medium chain triglycerides (MCTs) are considered as the most important functional foods and nutraceuticals. The present work deals with the intensification of synthesis of MCTs at a large capacity of 4L based on the use of ultrasonic bath and ultrasonic longitudinal horn. The effect of operating parameters like molar ratio of the reactants, type of catalyst and catalyst loading as well as the temperature on the extent of conversion has been investigated. The effect of molar ratio of lauric acid and glycerol was investigated over the range of 1:2 to 1:8 whereas the effect of loading of sulfuric acid was studied over the range of 4 ml/L-10 ml/L and zinc chloride loading over the range of 1 g/L-4 g/L. The effect of temperature was also studied using the conventional approach where it has been observed that 90 °C is an optimum temperature giving the extent of conversion as 72%. Also, the use of homogeneous catalyst as sulphuric acid was found to be more effective as compared to the solid catalyst as zinc chloride. It was observed that the maximum extent of conversion as 77.5% was obtained at 8 ml/L of sulfuric acid and molar ratio of 1:6 using ultrasonic longitudinal horn with US bath giving lower conversion as compared to US longitudinal horn but higher than the conventional approach under same operating conditions. The present work clearly established the intensification benefits in terms of reduction in time and higher conversion using cavitational reactors.

Ultrasound-assisted chemoenzymatic epoxidation of soybean oil by using lipase as biocatalyst.

The present work reports the use of ultrasonic irradiation for enhancing lipase catalyzed epoxidation of soybean oil. Higher degree of unsaturated fatty acids, present in the soybean oil was converted to epoxidized soybean oil by using an immobilized lipase, Candida antarctica (Novozym 435). The effects of various parameters on the relative percentage conversion of the double bond to oxirane oxygen were investigated and the optimum conditions were established. The parameters studied were temperature, hydrogen peroxide to ethylenic unsaturation mole ratio, stirring speed, solvent ratio, catalyst loading, ultrasound frequency, ultrasound input power and duty cycle. The main objective of this work was to intensify chemoenzymatic epoxidation of the soybean oil by using ultrasound, to reduce the time required for epoxidation. Epoxidation of the soybean oil was achieved under mild reaction conditions by indirect ultrasonic irradiations (using ultrasonic bath). The relative percentage conversion to oxirane oxygen of 91.22% was achieved within 5h. The lipase was remarkably stable under optimized reaction conditions, later was recovered and reused six times to produce epoxidized soybean oil (ESO).

Cleaning of used rotary nickel-titanium files in an ultrasonic bath by locally intensified acoustic cavitation.

AIM: To compare the pre-sterilization cleaning of rotary Ni-Ti files of different sizes previously used a. ex vivo and b. clinically by a washer-disinfector, a regular ultrasonic bath, and the same ultrasonic bath in combination with a recently developed cavitation intensifying method. METHODOLOGY: Two sets of two hundred rotary Ni-Ti files, one previously used ex vivo and another one used clinically, were collected from the undergraduate and postgraduate clinics of the Academic Centre for Dentistry Amsterdam (ACTA). The instruments were immersed in an enzymatic solution and subsequently cleaned either by a washer-disinfector, a regular ultrasonic bath combined with a glass beaker, the same bath combined with a beaker lined with two cavitation intensifying sheets or with two standard plastic sheets. The positive control consisted of used files that did not undergo any cleaning and the negative control included new unused files. The instruments were then stained to reveal remaining protein material and scored under a stereoscopic microscope. The results were analysed by nonparametric statistical tests (α = 0.05). RESULTS: No significant difference was found between the combination of the ultrasonic bath and the regular glass beaker and the same ultrasonic bath with the beaker lined with the cavitation intensifying sheets. The washer-disinfector left significantly more debris compared to the latter group when clinically used files were evaluated (P ≤ 0.001). The effect of instrument size on cleaning was not consistent. CONCLUSION: None of the tested methods was able to remove all residual protein material from the files; however, it could be noted that this study did not follow the reprocessing protocol provided by the manufacturer.

Allergic contact dermatitis caused by dimethylthiocarbamylbenzothiazole sulfide (DMTBS) in canvas shoes: in search of the culprit allergen.

BACKGROUND: During rubber vulcanization, new compounds can be formed. OBJECTIVES: To report a case of allergic shoe dermatitis in which the search for the allergen ultimately led to the identification of dimethylthiocarbamylbenzothiazole sulfide (DMTBS). METHODS: A female presented with eczema on her feet after wearing Sperry Top Sider® canvas sneakers. Patch testing was performed with the European baseline series, additional series, shoe materials, and extracts of shoe materials. Thin-layer chromatography (TLC) was performed for additional patch testing, and high-performance liquid chromatography and gas chromatography-mass spectometry were used for chemical analysis. RESULTS: Positive reactions were found to thiuram mix (+), tetramethylthiuram monosulfide (TMTM) (+), shoe material (+), and shoe extracts in eth. (++) and acetone (+). The extracts did not contain TMTM or other components of thiuram mix. TLC strips yielded a positive reaction (+) to one spot, whereas chemical analysis gave a negative result. Thereafter, a similar sneaker from another patient with shoe dermatitis was analysed, and DMBTS was identified. New extracts of the shoe of our first patient were then also shown to contain DMTBS. DMTBS as culprit allergen was confirmed by positive patch testing with a dilution series with DMTBS. CONCLUSION: DMBTS was identified as the culprit allergen in shoe dermatitis, giving rise to compound allergy. The positive reaction to TMTM was considered to represent cross-reactivity.

Improved crystallization of ammonium sulphate using ultrasound assisted approach with comparison with the conventional approach.

In chemical processing industries, crystallization is one of the most important operations to obtain solid products with desired purity and characteristics. With distinct processing problems for the conventional approaches for crystallization, research into alternate approaches such as ultrasound assisted crystallization has been on the forefront. The present work deals with comparison of the conventional approach and ultrasound assisted approach for crystallization of ammonium sulphate followed by detailed understanding into the effect of important operating parameters (initial concentration, pH, agitation speed, depth of horn, and cooling approach) on the metastable zone width and average crystal size. Ultrasound assisted crystallization has been investigated using both ultrasonic bath and ultrasonic horn to understand the effect of type of irradiation. It has been observed that the maximum reduction in the MSZW was obtained using ultrasonic horn under conditions of optimized initial concentration. The order of average crystal size obtained for ammonium sulphate was conventional cooling crystallization>ultrasonic bath>ultrasonic horn. The average crystal size obtained was in the range of 411-450µm for conventional approach of cooling crystallization, 350-400µm using ultrasonic bath and 200-250µm using ultrasonic horn. The analysis of crystal size distribution and surface characteristics using the SEM analysis was also performed under set of optimized parameters established using the particle size analysis. Overall the work has clearly established that the ultrasound assisted crystallization gave better results as compared to the conventional cooling crystallization in terms of reduced metastable zone width, better crystal characteristics and less agglomeration.

Determination of orientin in Trollius chinensis using ultrasound-assisted extraction and high performance liquid chromatography: Several often-overlooked sample preparation parameters in an ultrasonic bath.

The erratic pressure intensities and cavitation exhibited in an ultrasonic bath pose various during practical application. To achieve the most efficient experimental design, this manuscript aims to discover violently sites that are subject to the effect of slight changes in position on cavitation and ultrasound intensity distributed in the ultrasonic bath. In addition, optimization several often over-looked ultrasound parameters and experimental conditions, are intended to place the reaction vessel properly and operate under suitable experimental conditions to obtain the maximum yield of target analyte. In this study, an investigation of the various ultrasound intensities and cavitation in ultrasonic bath space were conducted with the help of the orientin yield using ultrasound-assisted extraction. Conventional parameters such as the volume fraction of ethanol, liquid-solid ratio, ultrasound irradiation power, time and frequency, and reaction temperature were investigated, all of which affect the extractive yield factors. Also several often over-looked parameters such as the extraction vessel position in the ultrasonic bath base, the distance between the bottom of the extraction vessel and the ultrasonic bath base, the diameter, the shape and the texture of the extraction vessel, height of the liquid medium and the ultrasound propagating medium salt concentration in the ultrasonic bath were tested exhaustively in this study. These results can therefore serve as a guide to optimize the usage of the ultrasonic bath for future applications.