Mixed fermentation and electrospray drying for the development of a novel stabilized wheat germ powder containing highly viable probiotic cultures.

Nondairy fermented probiotic powder was developed based on stabilized wheat germ through mixed fermentation (Lactobacillus acidophilus and Lactobacillus plantarum) and electrospraying process. In the first step, the effect of mixed fermentation on lipase and lipoxygenase activity of wheat germ was investigated. The results showed a significant reduction in the activity of both enzymes (82.72% for lipase and 72% for lipoxygenase), therefore, mixed fermentation effectively stabilizes the wheat germ. In the next step, after the preparation of the solutions for drying process and investigating the physical properties (surface tension, electrical conductivity, and viscosity) of the solutions, the electrosprayability of the samples was evaluated at different conditions and revealed that 18 kV applying voltage, 0.3 flow rate, and 12 cm distance between tip to collector was the best for electrospraying the 20% solution of fermented wheat germ with morphologically most semi-uniform particles. Finally, the viability of the probiotics after drying process and during the storage at 25°C was examined. The number of initial cells counted as 14.48 ± 0.2 log cfu/g and the viability studies showed 0.55 log cfu/g decrease in the number of viable bacteria from initial count as a result of the electrospraying process. Furthermore, 7.86 ± 0.03 log cfu/g in freeze-dried and 9.05 ± 0.45 log cfu/g in electrosprayed samples survived after 70 days of storage.

Optimization and characterization of pullulan produced by a newly identified strain of Aureobasidium pullulans.

In this study, a new strain suspected to be Aureobasidium pullulans was isolated from trees leaves. The molecular characterization and the resulting phylogenetic tree showed that the isolated strain was A. pullulans. Also, the results of methylation analysis, monosaccharide composition, FTIR, NMR and XRD confirmed that the obtained exo-polysaccharide from the mentioned strain was pullulan. The pullulan production optimization by central composite design (CCD) indicated that the maximum yield obtained under optimum conditions (pH of 6.5, sucrose concentration of 5.5% (w/v) and yeast extract concentration of 0.1% (w/v)) was 51.4 ± 0.50 g/L. The produced pullulan had an average molecular weight (Mw) of 2.07 × 105 g.mol-1 based on gel permeation chromatography results. The decomposition temperature (Td) of the produced pullulan was ~300 °C and also, the resulting pullulan had a Newtonian flow behavior in a wide range of concentrations.

Fast Quantitation of Target Analytes in Small Volumes of Complex Samples by Matrix-Compatible Solid-Phase Microextraction Devices.

Herein we report the development of solid-phase microextraction (SPME) devices designed to perform fast extraction/enrichment of target analytes present in small volumes of complex matrices (i.e. V≤10 µL). Micro-sampling was performed with the use of etched metal tips coated with a thin layer of biocompatible nano-structured polypyrrole (PPy), or by using coated blade spray (CBS) devices. These devices can be coupled either to liquid chromatography (LC), or directly to mass spectrometry (MS) via dedicated interfaces. The reported results demonstrated that the whole analytical procedure can be carried out within a few minutes with high sensitivity and quantitation precision, and can be used to sample from various biological matrices such as blood, urine, or Allium cepa L single-cells.

Rapid analysis of Origanum majorana L. fragrance using a nanofiber sheet, gas chromatography with mass spectrometry, and chemometrics.

Headspace nanofiber sheet microextraction together with GC-MS and chemometrics resolution techniques were implemented to separate and identify the volatiles emitted by intact marjoram (Origanum majorana L.) and their relative concentrations. A novel polyaniline-nylon-6 nanofiber composite was applied for headspace microextraction. Characteristics such as high surface-to-volume ratio and π-π functional groups in polyaniline together with the NH and C=O functional groups in nylon-6 make the polyaniline-nylon-6 nanofiber composite a suitable candidate for the extraction of volatiles and semivolatiles. The extracted constituents were desorbed and injected into the GC-MS system under the optimum conditions. Chemometric resolution techniques were utilized to solve the baseline offset, asymmetric peaks, and overlapped peaks problems that arise from GC-MS analysis. By means of these techniques and resolving the overlapped peak clusters, the number of identified constituents was increased to 67 compounds. The major released constituents from the intact marjoram leaves are 4-terpineol, ß-linalool, cis-sabinol, and trans-geraniol.

A highly thermal-resistant electrospun-based polyetherimide nanofibers coating for solid-phase microextraction.

A high-temperature-resistant solid-phase microextraction (SPME) fiber was prepared based on polyetherimide (PEI) by the electrospinning method. The PEI polymeric solution was converted to nanofibers using high voltages and directly coated on a stainless steel SPME needle. The scanning electron microscopy images of PEI coating showed fibers with diameter range of 500-650 nm with a homogeneous and smooth surface morphology. The SPME nanofibers coating was optimized for PEI percentage, electrospinning voltage, and time. The extraction efficiency of the coating was investigated for headspace SPME of some environmentally important polycyclic aromatic hydrocarbons from aqueous samples followed by gas chromatography-mass spectrometry measurement. In addition, the important extraction parameters including extraction temperature, extraction time, ionic strength, as well as desorption temperature and time were investigated and optimized. The detection limits of the method under optimized conditions ranged from 1 to 5 ng L(-1) using time-scheduled selected ion monitoring mode. The relative standard deviations of the method were between 1.1 and 7.1 %, at a concentration level of 500 ng L(-1). The calibration curves of polycyclic aromatic hydrocarbons showed linearity in the range of 5-1000 ng L(-1). The developed method was successfully applied to real water samples and the relative recovery percentages obtained from the spiked water samples were from 84 to 98 % for all the selected analytes except for acenaphthene which was from 75 to 106 %.

Novel polyamide-based nanofibers prepared by electrospinning technique for headspace solid-phase microextraction of phenol and chlorophenols from environmental samples.

A novel solid phase microextraction (SPME) fiber was fabricated by electrospinning method in which a polymeric solution was converted to nanofibers using high voltages. A thin stainless steel wire was coated by the network of polymeric nanofibers. The polymeric nanofiber coating on the wire was mechanically stable due to the fine and continuous nanofibers formation around the wire with a three dimensional structure. Polyamide (nylon 6), due to its suitable characteristics was used to prepare the unbreakable SPME nanofiber. The scanning electron microscopy (SEM) images of this new coating showed a diameter range of 100-200 nm for polyamide nanofibers with a homogeneous and porous surface structure. The extraction efficiency of new coating was investigated for headspace solid-phase microextraction (HS-SPME) of some environmentally important chlorophenols from aqueous samples followed by gas chromatography-mass spectrometry (GC-MS) analysis. Effect of different parameters influencing the extraction efficiency including extraction temperature, extraction time, ionic strength and polyamide amount were investigated and optimized. In order to improve the chromatographic behavior of phenolic compounds, all the analytes were derivatized prior to the extraction process using basic acetic anhydride. The detection limits of the method under optimized conditions were in the range of 2-10 ng L(-1). The relative standard deviations (RSD) (n=3) at the concentration level of 1.7-6.7 ng mL(-1) were obtained between 1 and 7.4%. The calibration curves of chlorophenols showed linearity in the range of 27-1330 ng L(-1) for phenol and monochlorophenols and 7-1000 ng L(-1) for dichloro and trichlorophenols. Also, the proposed method was successfully applied to the extraction of phenol and chlorophenols from real water samples and relative recoveries were between 84 and 98% for all the selected analytes except for 2,4,6 tricholophenol which was between 72 and 74%.

Polyaniline-nylon-6 electrospun nanofibers for headspace adsorptive microextraction.

A headspace adsorptive microextraction technique was developed using a novel polyaniline-nylon-6 (PANI-N6) nanofiber sheet, fabricated by electrospinning. The homogeneity and the porosity of the prepared PANI-N6 sheet were studied using the scanning electron microscopy (SEM) and nanofibers diameters were found to be around 200 nm. The novel nanofiber sheet was examined as an extracting medium to isolate some selected chlorobenzenes (CBs), as model compounds, from aquatic media. The extracted analytes were desorbed using µL-amounts of solvent and eventually an aliquot of extractant was injected into gas chromatography-mass spectrometry (GC-MS). Various parameters affecting the extraction and desorption processes were optimized. The developed method proved to be convenient and offers sufficient sensitivity and a good reproducibility. Limits of detection achieved for CBs with the developed analytical procedure ranged from 19 to 33 ng L(-1), while limits of quantification were from 50 to 60 ng L(-1). The relative standard deviations (RSD) at a concentration level of 0.1 ng mL(-1) and 1 ng mL(-1) were in the range of 8-14% and 5-11% (n=3), respectively. The calibration curves of analytes were investigated in the range of 50-1000 ng L(-1) and R(2) between 0.9739 and 0.9932 were obtained. The developed method was successfully applied to the extraction of selected CBs from tap and river water samples. The relative recovery (RR) percentage obtained for the spiked real water samples at 0.1 ng mL(-1) and 1 ng mL(-1) level were 93-103% and 95-104%, respectively. The whole procedure showed to be conveniently applicable and quite easy to handle.

Reinforced polydiphenylamine nanocomposite for microextraction in packed syringe of various pesticides.

Reinforced polydiphenylamine (PDPA) nanocomposite was synthesized by oxidation of diphenylamine in 4 molL(-1) sulfuric acid solution containing a fixed amount of carbon nanotubes (CNTs) in the presence of cetyltrimethylammonium bromide (CTAB). The surface characteristic of PDPA and PDPA/CNT nanocomposites was investigated using scanning electron microscopy (SEM). The prepared PDPA/CNT nanocomposite was used as an extraction medium for microextraction in packed syringe (MEPS) of selected pesticides from aquatic environment. The effect of CNT doping level and the presence of surfactant on the extraction capability of nanocomposite was investigated and it was revealed that when 4% (w/w) of CNT in the presence of CTAB is being used, the highest extraction recovery could be achieved. Eventually, the developed MEPS technique in off-line combination with gas chromatography-mass spectrometry (GC-MS) was applied to the analysis of some pesticides including triazine, organophosphorous, organochlorine and aryloxyphenoxy propionic acid pesticides. Important parameters influencing the extraction and desorption processes were optimized and a 25 cycles of draw-eject gave maximum peak area, when desorption was performed using 200 µL of n-hexane. Limits of detection (LODs) were in the range of 0.01-0.1 ngmL(-1) and 0.02-0.1 ngmL(-1) for distilled water and river water respectively, using time scheduled selected ion monitoring (SIM) mode. The method precision (RSD %) with four replicates was in the range of 1.6-14.6% for distilled water and 1.5-16.2% for river water at the concentration level of 5 ngmL(-1) while the linearity of method was in the range of 0.15-100 and 0.5-500 ngmL(-1). The developed method was successfully applied to different river water samples and the matrix factor for the spiked river water samples were found to be in the range of 0.74-1.09.

Polypyrrole/polyamide electrospun-based sorbent for microextraction in packed syringe of organophosphorous pesticides from aquatic samples.

A novel method based on microextraction in packed syringe (MEPS) as sample preparation technique coupled off-line with gas chromatography-mass spectrometry was developed using electrospun nanofibers as sorbent. For electrospinning of polypyrrole/polyamide-based nanofiber, a homogeneous solution containing nylon 6, ferric chloride and pyrrole monomer was prepared and then was drawn into a 2.5-mL syringe. By applying a voltage of 13 kV between the needle of the syringe and an aluminum-foil collector, the nanofibers could be formed on the surface of the collector. The prepared sheet was used as the sorbent for MEPS to analyze some selected organophosphorous pesticides. Important parameters influencing the extraction and desorption processes were optimized. Limits of detection were in the range of 0.04-0.1 ng/mL using time scheduled selected ion monitoring mode, and the relative standard deviation (RSD %) values with four replicates were in the range of 3.7-11.8% at a concentration level of 5 ng/mL. The linearity of the method was in the range of 0.5-500 ng/mL for diazinon and fenithrothion and 0.5-200 ng/mL for the rest of the analytes. The developed method was successfully applied to Zayandeh-roud river water samples, whereas the matrix factors were in the range of 0.87-0.98.

Electrospun composite of polypyrrole-polyamide as a micro-solid phase extraction sorbent.

A micro-solid phase extraction technique was developed using a novel polypyrrole-polyamide nanofiber sheet, fabricated by electrospinning method. The applicability of the new nanofiber sheet was examined as an extracting medium to isolate malathion as a model pesticide from aqueous samples. Solvent desorption was subsequently performed in a microvial, and an aliquot of extractant was injected into gas chromatography-mass spectrometry. Various parameters affecting the electrospinning process including monomer concentration, polyamide content, applied voltage, and electrospinning time were examined. After fabricating the most suitable preparation conditions, influential parameters on the extraction and desorption processes were optimized. The developed method proved to be rather convenient and offers sufficient sensitivity and good reproducibility. The limit of detection (S/N = 3) and limit of quantification (S/N = 10) of the method under optimized conditions were 50 and 100 ng L(-1), respectively. The relative standard deviation at concentration level of 1 ng mL(-1) was 2% (n = 3). The calibration curve of analyte showed linearity in the range of 0.1-1 ng mL(-1) (R (2) = 0.9975). The developed method was successfully applied to tap and Zayanderood river water samples, while the relative recovery percentages of 98% and 96% were obtained, respectively. The whole procedure showed to be conveniently applicable and quite easy to be manipulated.

Extraction of fluoxetine from aquatic and urine samples using sodium dodecyl sulfate-coated iron oxide magnetic nanoparticles followed by spectrofluorimetric determination.

A new method based on the combination of magnetic solid phase extraction (MSPE) and spectrofluorimetric determination was developed for isolation and preconcentration of fluoxetine form aquatic and biological samples using sodium dodecyl sulfate (SDS) coated Fe(3)O(4) nanoparticles (NPs) as a sorbent. The unique properties of Fe(3)O(4) NPs including high surface area and strong magnetism were utilized effectively in the MSPE process. Effect of different parameters influencing the extraction efficiency of fluoxetine including the amount of Fe(3)O(4) and SDS, pH value, sample volume, extraction time, desorption solvent and time were optimized. Under optimized condition, the method was successfully applied to the extraction of fluoxetine from water and urine samples and absolute recovery amount of 85%, detection limit of 20 µg L(-1) and a relative standard deviation (RSD) of 1.4% were obtained. The method linear response was over a range of 50-1000 µg L(-1) with R(2)=0.9968. The relative recovery in different aquatic and urine matrices were investigated and values of 80% to 104% were obtained. The whole procedure showed to be conveniently fast, efficient and economical for extraction of fluoxetine from environmental and biological samples.

A novel needle trap sorbent based on carbon nanotube-sol-gel for microextraction of polycyclic aromatic hydrocarbons from aquatic media.

A new type of composite material based on carbon nanotubes (CNTs) and sol-gel chemistry was prepared and used as sorbent for needle trap device (NTD). The synthesized composite was prepared in a way to disperse CNTs molecules in a sol-gel polymeric network. CNT/silica composites with different CNT doping levels were successfully prepared, and the extraction capability of each composite was evaluated. Effects of surfactant and the oxidation duration of CNTs on the extraction efficiency of synthesized composites were also investigated. The applicability of the synthesized sorbent was examined by developing a method based on needle trap extraction (NTE) and gas chromatography mass spectrometry detection (GC-MS) for the determination of polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. Important parameters influencing the extraction process were optimized and an extraction time of 30 min at 50 °C and sampling flow rate of 2.5 mL min(-1) gave maximum peak area, when NaCl (15%, w/v) was added to the aqueous sample. The linearity for acenaphthene, acenaphthylene and fluorene was in the concentration range of 0.01-20 ng mL(-1) and for naphthalene and anthracene was in the range of 0.1-50 ng mL(-1). Limits of detection was 0.001 ng mL(-1), for acenaphthene, acenaphthylene and fluorene, and 0.01 ng mL(-1), for naphthalene and anthracene using time-scheduled selected ion monitoring (SIM) mode, and the RSD% values (n=3) were all below 11.2% at the 1 ng mL(-1) level. The developed method was successfully applied to real water samples while the relative recovery percentages obtained for the spiked water samples were from 73.8 to 113.8%.