Dispersive Solid-Phase Extraction Clean-up Combined with Dispersive Liquid�CLiquid Microextraction for the Determination of Neonicotinoid Insecticides in Vegetable Samples by High-Performance Liquid Chromatography

Dispersive solid-phase extraction (DSPE) clean-up combined with dispersive liquid–liquid microextraction (DLLME) has been developed as a new approach for the extraction of neonicotinoid insecticides in vegetable samples prior to high-performance liquid chromatography with diode array detection. In the DSPE–DLLME method, neonicotinoid insecticides were first extracted with acetonitrile from vegetable samples, followed by clean-up by a DSPE with primary secondary amine and multi-walled carbonnanotubes as sorbents. A 2.5-mL aliquot of the resulting extract was then added into a centrifuge tube containing 10 mL of water, 0.8 g NaCl, and 200-μL chloroform (as the extraction solvent) for DLLME procedure. Under the optimum conditions, the enrichment factors for the compounds were in the range between 110 and 243. The linearity of the method was in the range from 5.0 to 300 ng g⁻¹ with the correlation coefficients (r) ranging from 0.9989 to 0.9998. The detection limits of the method were 0.5–1.0 ng g⁻¹. The repeatability of the method expressed as the relative standard deviations by five parallel experiments at the concentration levels of 10 and 50 ng g⁻¹ each of the neonicotinoid insecticides in tomato or cucumber samples varied from 3.6% to 5.8%. The developed method has been successfully applied for the analysis of target neonicotinoid insecticides (acetamiprid, imidacloprid, thiacloprid, and thiamethoxam) in tomato and cucumber samples. The recoveries of the method for the target neonicotinoid insecticides from the vegetable samples at spiking levels of 10.0 and 50.0 ng g⁻¹ were in the range between 84.6% and 97.5% (n = 5).     

Micelle-Mediated Extraction and Flame Atomic Absorption Spectrometric Method for Determination of Trace Cobalt Ions in Beverage Samples

A new method has been developed for preconcentration of cobalt at trace levels in beverage samples using calcon carboxylic acid as chelating agent and cetyl pyridinium chloride as an auxiliary ligand and entrapped into Triton X-114 prior to its determination by flame atomic absorption spectrometry (FAAS). The main parameters affecting cloud point extraction (CPE) efficiency such as pH, concentration of the complexing agent, cationic and nonionic surfactant concentration, salt effect, the equilibrium time, and temperature were investigated and optimized. After optimization of the CPE conditions, a preconcentration factor of 60, an enhancement factor of 106, and a detection limit of 0.20 μg L⁻¹ by (R ² = 0.9978) were obtained from a calibration curve constructed in the range of 0.7–100 μg L⁻¹. The proposed preconcentration procedure was successfully applied to the determination of cobalt ions in some real samples including natural drinking water, tap water, and beer and wine samples. The accuracy and validity of the proposed CPE/FAAS method was tested by means of five repeated analysis of reference standard materials (TM-253, a low level fortified water standard for trace elements). A good agreement between analytical results (28.8 and 28.5 μg L⁻¹ with calibration curve and standard addition curve method, respectively) and certified value (27.9 μg L⁻¹) for Co (p < 0.05) were obtained and verified by means of calibration curve and standard addition curve method using CPE procedure.     

Extraction of Bioactive Compounds from Milled Grape Canes (Vitis vinifera) Using a Pressurized Low-Polarity Water Extractor

Trans-resveratrol and trans-ε-viniferin were extracted from milled grape canes using pressurized low-polarity water. The effects of temperature were significant for both compounds (p ≤ 0.05): extraction at 160 °C resulted in a 40% loss of trans-resveratrol compared to 95 °C while reduction of trans-ε-viniferin at both temperatures remained at 30%. Increasing ethanol concentration from 0% to 25% increased the extraction of total phenolics and trans-ε-viniferin by 44% and 489%, respectively. Solvent flow rate also influenced trans-ε-viniferin extraction. Antioxidant activity showed a strong correlation with total phenolic content of the extracts, and the two target phenolic compounds. Except for the modifier concentration, the extraction parameters studied were not statistically significant with respect to the antioxidant activity of extracts (p > 0.05). Effective diffusivities of trans-resveratrol multiplied from 3.3 × 10⁻¹¹ to 10.4 × 10⁻¹¹ m²/s by three times with increasing temperature. The modified Gompertz equation satisfactorily explained the extraction of the stilbenes investigated.     

Physicochemical and Enzymatic Properties of Five Kiwifruit Cultivars during Cold Storage

Samples of Abbot, Alison, Bruno, Monty, and Hayward cultivars of kiwifruit (Actinidia deliciosa) were obtained from the Iran Research Center of Citrus (Tonekabon, located in north of Iran) and their physicochemical properties were studied during cold storage (at T = 1 ± 1 °C, RH = 80 ± 5%) at 0-, 9-, and 18-week intervals. The mean chemical composition of the fruits were as follows: ash = 0.66–0.96%, moisture = 75.2–84.7%, starch = 0.3–7.0%, and ascorbic acid = 54.8–261.0; K = 125.0–372.0 mg 100 g⁻¹ fresh weight, Mg = 18.0–32.0 mg 100 g⁻¹ fresh weight, Na = 1.4–3.1 mg 100 g⁻¹ fresh weight, Fe = 0.17–0.52 mg 100 g⁻¹ fresh weight, Cu = 0.04–0.24 mg 100 g⁻¹ fresh weight, Zn = 0.16–0.49 mg 100 g⁻¹ fresh weight, Mn = 0.04–0.10 mg 100 g⁻¹ fresh weight, and P = 25.2–49.3 mg 100 g⁻¹ fresh weight; glucose = 0.7–2.39%, fructose = 1.20–3.13%, and sucrose = 0.0–5.8%. At the same time, the values of the parameters °Brix = 6.5–14.8% and acidity = 1.8–2.5% of the studied cultivars (mutual effects of cultivar and storage time) were investigated. The increase in peroxidase (POX = 0.0–6.65 U ml⁻¹) and the decrease in pectinesterase (PE; poor activity to 0) activities were also determined. The statistical analysis showed that the Bruno cultivar had the highest content of ascorbic acid (115.0–261.0 mg 100 g⁻¹ fresh weight), which is an important compound in fruits during storage, while Hayward had the best overall quality particularly with regards to its resistance to softening. This study confirms that long-term cold storage at 1 ± 1 °C and 80 ± 5% RH is suitable for maintaining the highest quality of Iranian grown cultivars of kiwifruit.     

Co-production of Lactic Acid and <Emphasis Type="Italic">Lactobacillus rhamnosus</Emphasis> Cells from Whey Permeate with Nutrient Supplements

Lactic acid and cell production from whey permeate by Lactobacillus rhamnosus with different nutrient supplements were investigated in this study. Yeast extract was identified as the most effective nutrient affecting lactic acid production. Increase in inoculum size from 0.05% to 1% (v/v) resulted in a substantial increase in lactic acid productivity from 0.66 to 0.83 g L⁻¹ h⁻¹ (P < 0.001). The optimal temperature for lactic acid production was 37 °C, while the highest cell production was obtained at 42 °C. When whey permeate and yeast extract concentrations were 6.8% (w/v) and 3 g L⁻¹, respectively, lactic acid productivity reached 0.85 g L⁻¹ h⁻¹ after 48-h cultivation, which is 3.40 times of those without nutrient supplements.     

Evaluation of Protease-producing Ability of Fish Gut Isolate Bacillus cereus for Aqua Feed

Extracellular protease production by Bacillus cereus isolated from the intestine of fish Mugil cephalus has been investigated in shake-flask experiment using different preparations of tuna-processing waste such as raw fish meat, defatted fish meat, alkali hydrolysate, and acid hydrolysate as nitrogen source. Among the tuna preparations tested, defatted fish meat supported the maximum protease production (134.57 ± 0.47 U ml⁻¹), and 3% concentration of the same was found to be optimum for maximizing the protease production (178.50 ± 0.28 U ml⁻¹). Effect of carbon sources on protease production in the optimized concentration of defatted tuna fish meat revealed that galactose aided the higher protease production (259.83 ± 0.04 U ml^–1) than the other tested carbon sources and a concentration of 1.5% galactose registered as optimum to enhance the protease production (289.40 ± 0.16 U ml⁻¹). The halotolerancy of B. cereus for protease production indicated that 3% of sodium chloride was optimum to yield maximum protease (301.63 ± 0.20 U ml⁻¹). Among the surfactants tested, protease production was high in Triton X 100-added medium (298.63 ± 0.12 U ml⁻¹) when compared to other surfactants, and its optimum concentration recorded was 0.8% (320.57 ± 0.17 U ml⁻¹) for more protease production. Partial characterization of crude enzyme revealed that pH 7.0 (278.90 ± 0.08 U ml⁻¹) and 60°C temperature (332.37 ± 0.18 U ml⁻¹) were optimum for better protease activity by B. cereus.     

Supercritical CO<Subscript>2</Subscript> extraction of <Emphasis Type="Italic">Alkanna</Emphasis> species and investigating functional characteristics of alkannin-enriched yoghurt during storage

Alkannin is a potent pharmaceutical substance with a wide spectrum of biological activities. In the scope of this study, supercritical CO₂ extraction and sonication with hexane were applied to various Alkanna species, which were then subjected to hydrolysis. Total alkannins were quantified by HPLC/DAD and incorporated into yoghurt. Viscosities, pH values and microbial analyses were reported at 7 days of intervals for 21 days of storage. A. tinctoria possessed the highest amounts of alkannins and total phenols (686.3 mg GAE/g extract). The results revealed no significant changes in pH values (4.1–4.0), viable counts of Streptococcus salivarius ssp. thermophilus (80–150 × 10⁶ cfu g⁻¹) and slightly lower viscosities of enriched yoghurts (8,250–6,750 cPs) compared with the control (4.15–4.0; 110–105 × 10⁶ cfu g⁻¹; 12,600–11,310 cPs) during storage. However, viable counts of Lactobacillus delbrueckii ssp. bulgaricus of enriched yoghurts (87 × 10³ cfu g⁻¹) were much better than the control (191 × 10³ cfu g⁻¹), indicating a significant decrease in post acidification and generation of bitter peptides. Among the species investigated, A. tinctoria is the most promising source, obtained at higher yields via supercritical fluid extraction technology as a green alternative to solvent extraction and thus can be utilized at industrial scale in order to develop yoghurt products with improved health benefits.     

Analysis of Flavonoids in <Emphasis Type="Italic">Portulaca oleracea</Emphasis> L. by UV–Vis Spectrophotometry with Comparative Study on Different Extraction Technologies

Portulaca oleracea L. is a traditional edible and medicinal plant in China. Flavonoids are one of the main active ingredients of this plant. Five extraction technologies of flavonoids from P. oleracea L. were investigated and compared, including microwave-assisted extraction, ultrasonic extraction, reflux extraction, Soxhlet extraction, and marinated extraction. The results showed that microwave-assisted extraction was most suitable for the extraction of flavonoids from P. oleracea L. because of its high effect and short extraction time. The found optimum extraction conditions were that the ethanol concentration was 70% (v/v), solid–liquid ratio was 1:50, extracting temperature was 50 °C and irradiation time was 9 min. Quantification was performed by means of UV–Vis spectrophotometry with chromogenic system of NaNO₂–Al (NO₃)₃–NaOH. Under the optimum conditions, the calibration curve for the analyte was linear with the correlation coefficients greater than 0.9999. The average recovery was 102.6%, and its RSD was 1.13%(n = 5). Eight types of P. oleracea L. according to different habits were investigated. The total content of flavonoids was 7.16, 7.10, 9.38, 6.82, 6.78, 11.36, 5.12, and 1.76 mg g⁻¹, respectively.     

Determination of Nitrite and Nitrate in Brazilian Meats Using High Shear Homogenization

Nitrate and nitrite are usually added to processed meat products to protect against the growth of microorganisms. Two sample preparation methodologies using either manual grinding (with a mortar and pestle) or mechanical high shear homogenization were investigated and compared. The results showed that high shear homogenization was the most suitable for the extraction of nitrite and nitrate from ham, salami, and bacon samples, achieving high extraction recoveries (>98%) together with low relative standard deviations (RSDs) for the samples analyzed. Analyses were performed using capillary electrophoresis. A running buffer consisting of 60 mmol L⁻¹ tetraborate and 0.2 mmol L⁻¹ cetyltrimethylammonium bromide enabled separation of the analytes in <5 min. In validation experiments, good repeatability was obtained for both migration times (<0.8% RSD) and peak areas (<1.1% RSD). Analytical curves for nitrite and nitrate were linear (r > 0.998) in the 0.2- to 2.5-mg L⁻¹ and 0.5- to 5-mg L⁻¹ concentration ranges, respectively. The limits of detection were 0.15 mg L⁻¹ for nitrite and 0.17 mg L⁻¹ for nitrate. The method developed was applied to the analysis of different kinds of meats (sausage, ham, salami, bacon, and others) produced in Brazil. The ranges of concentration found were 17.3–46.4 mg kg⁻¹ (nitrite) and 69.9–198.1 mg kg⁻¹ (nitrate). The contents of nitrate and nitrite in the samples were below the Brazilian legislation limit values (150 and 300 mg kg⁻¹ for nitrite and nitrate, respectively).     

Optimization of Microwave-Assisted Extraction Procedure to Determine Metal in Fish Muscles Using Box–Behnken Design

This study describes the application of response surface methodology (RSM) to develop a method for zinc, lead, manganese, nickel, iron, and copper determination by flame atomic absorption spectrometry in Snow trout (Schizothorax zarudnyi) samples after extraction by a microwave system. The effects of various parameters such as irradiation power, temperature, extraction time, and concentration of nitric acid were investigated by a fractional factorial design (2⁴⁻¹) to determine the significant parameters and their interactions. The results showed that all of the parameters were significant (p < 0.05). The RSM, based on Box–Behnken design, was employed to obtain the optimum conditions of the significant parameters. The optimal conditions could be obtained at a power of 685.0 W, temperature of 116 °C, extraction time of 38.0 min, and 2.5 (mol L⁻¹) for nitric acid concentration. The method was applied for determination of zinc, lead, manganese, nickel, iron, and copper in Snow trout (Schizothorax zarudnyi) samples.     

Determination of Histamine in Some Foods by Isotachophoretic Method with Simple Sample Preparation

A one-dimensional capillary isotachophoretic method in cationic system of the separation has been applied for histamine determination in food samples. The proposed electrolyte system consisted of 0.01 M potassium hydroxide with l-valine to pH = 9.9 as the leading electrolyte and 0.02 M 2-amino-2-hydroxymethyl-propane-1,3-diol adjusted to pH = 8.3 with 0.1 M hydrochloric acid as terminating electrolyte. Proposed method was characterized by linearity range 5–50 mg L⁻¹ and R ² = 0.9982, accuracy (recoveries ranged from 95% to 102%), detection (2.10 mg L⁻¹), and quantification (7.01 mg L⁻¹) limits. The sample preparation for proposed electrophoretic method included only simple extraction with trichloroacetic acid with filtration and derivatisation stage are avoided. The histamine concentration was determined in meat (turkey, chicken, beef and pork) and meat products (ripened sausage and dry-cured ham), fish (smoked salmon and mackerel), and different kind of mildew and mold ripened cheeses samples. The histamine content ranged from not detected level for fresh meat to 29.63 mg 100 g⁻¹ for cheese samples. The reversed phase HPLC was applied as reference method and the F-Snedecor test and the t test were employed to compare the precision and accuracy of the both methods. Positive correlations were found between the two analytical methods for histamine determination in food products. The obtained results indicate that the proposed electrophoretic method is simple, precise, accurate, and convenient.     

Application of Catalytic Hydrogen Evolution in the Presence of Neonicotinoid Insecticide Clothianidin

Clothianidin, a new generation of pesticide, was determined in spiked tap water, apple juice, and soil by square-wave adsorptive stripping voltammetry. The method of determination is based on the hydrogen evolution reaction catalyzed by clothianidin at the hanging mercury drop electrode. The optimal signal was detected at −1.4 V versus Ag/AgCl in citrate buffer at pH 2.2. Various parameters such as pH, buffer concentration, frequency, amplitude, step potential, accumulation time, and potential were investigated to enhance the sensitivity of the determination. The optimal results were recorded at an accumulation potential of −0.35 V, accumulation time of 7 s, amplitude of 100 mV, frequency of 200 Hz, and step potential of 7 mV. The mechanism of catalytic hydrogen evolution was considered under experimental and theoretical conditions. This electroanalytical procedure enabled to determine clothianidin in the concentration range 9 × 10⁻⁹–4 × 10⁻⁶ mol L⁻¹ in supporting electrolyte and tap water, 1 × 10⁻⁷–4 × 10⁻⁶ mol L⁻¹ in diluted apple juice, and 2 × 10⁻⁷–1 × 10⁻⁶ mol L⁻¹ in soil. The detection and quantification limits in supporting electrolyte and diluted apple juice were found to be 2.6 × 10⁻⁹, 8.6 × 10⁻⁹ and 3 × 10⁻⁸, and 1 × 10⁻⁷ mol L⁻¹, respectively. A standard addition method was successfully used to determine clothianidin in spiked tap water, spiked apple juice, and spiked soil.     

Optimization of supercritical CO2 extraction of phytosterol-enriched oil from Kalahari melon seeds

Supercritical carbon dioxide (SC-CO₂) extraction of oil from Kalahari melon seeds was investigated in this study. Response surface methodology was applied to model and optimize the extraction, namely pressure (200–400 bar), temperature (40–80 °C), and supercritical fluid flow rate (10–20 mL/min). Well-fitting models were successfully established for oil recovery (R ² = 0.9672) and phytosterol concentration (milligrams per 100 g; R ² = 0.8150) through multiple linear regressions with backward elimination. The effect of supercritical fluid flow rate was the most significant (P < 0.05) factor that affected oil recovery but this factor had no significant (P > 0.05) effect on phytosterol concentration. The optimal processing conditions for oil recovery and phytosterol concentration were pressure of 300 bar, temperature at 40 °C, and supercritical fluid flow rate of 12 mL/min. These optimal conditions yielded a 76.3% oil recovery and 836.5 mg/100 g of phytosterol concentration. The oil content in the Kalahari melon seeds as estimated by Soxhlet extraction was around 30.5/100 g. The phytosterol concentration in the oil extracted with SC-CO₂ extraction was 94% higher than that obtained with solvent extraction.     

Simple Phosphate Buffer Extraction for the Determination of Fumonisins in Masa,Maize, and Derived Products

An accurate determination of fumonisins in masa can be troublesome because of difficulties often experienced in obtaining satisfactory recoveries. In this study, a new extraction method, effective both for masa and for maize and derived products, has been developed. The method extracts fumonisins using a 0.4 M phosphate buffer (PB) at pH 7.5, without any organic solvent; the purification of the extract is performed by an immunoaffinity column and the quantification by HPLC–MS/MS. The average recovery percentages were 95.5 ± 1.9% and 96.7 ± 2.1% for fumonisin B₁ and B₂, respectively. The limit of detection and of quantification for both fumonisins were 10 and 30 μg kg⁻¹, respectively. For masa and tortillas, PB pH 7.5 gave significantly higher results when compared with AOAC and other published extraction methods; for maize flour, PB gave generally higher results, even if the difference with the other extraction methods was not always significant.     

Determination of Rosmarinic Acid by High-Performance Liquid Chromatography and Its Application to Certain Salvia Species and Rosemary

This study describes a method development for the determination of rosmarinic acid (RA) by using a gradient high-performance liquid chromatography (HPLC) and its application to certain plant materials. The analysis was performed by utilizing a two solvents system [A: methanol/water/formic acid (10:88:2; v:v:v); B: methanol/water/formic acid (90:8:2; v:v:v)] on a reverse-phase column. The flow rate and injection volume were 1 ml min⁻¹ and 10 μl, respectively. Signals were detected at 280 nm. In addition, an internal standard (IS) technique was applied for the analysis of RA to increase precision, and propylparaben was employed for this purpose. The repeatability results as RSD% were 1.66, 1.17 and 1.26 for intra-day and 1.38 was for inter-day with the employment of (3.67 × 10⁻⁵ M) RA. A limit of linearity (LOL) was observed in a wide (1.13 × 10⁻⁵–5.65 × 10⁻⁴ M) concentration range. Linearity parameters were also examined in the range of 5.95 × 10⁻⁶–7.14 × 10⁻⁵ M RA, and very good correlation was observed. The limit of detection (LOD) and limit of quantification (LOQ) (for inter-day) were 1.60 × 10⁻⁶ M (signal/noise [S/N] = 3.3) and 4.80 × 10⁻⁶ M (S/N = 10), respectively. The method was applied to the extracts of certain Lamiaceae plants (Salvia candidissima Vahl. subsp. candidissima, S. sclarea L., S. verticillata L. subsp. verticillata and R. officinalis L.), and reasonable results were obtained.     

A Sensitive, Selective New Analytical Reagent, 2, 6-Diacetylpyridine bis-4-phenyl-3-thiosemicarbazone for Extractive Spectrophotometric Determination of Mo(VI) in Food Samples

Synthesized a new reagent 2, 6-Diacetylpyridine bis-4-phenyl-3-thiosemicarbazone (2, 6-DAPBPTSC) characterized and is proposed as a sensitive and selective analytical reagent for the extractive spectrophotometric determination of molybdenum(VI) at pH 3.5 to form a yellowish orange colored 1:1 chelate complex. The absorbance was measured at a maximum wavelength, 500 nm. This method obeys Beer’s law in the concentration range 0.90–9.00 μg mL⁻¹ and the correlation coefficient of Mo(VI)–2,6-DAPBPTSC complex is 0.954, which indicates an adequate linearity between the two variables with good molar absorptivity and Sandell’s sensitivity, 1.212 × 10⁴ L mol⁻¹cm⁻¹, 0.0079 μg cm⁻², respectively. The precision and accuracy of the method is checked with calculation of relative standard deviation (n = 5), 0.894% and the detection limit value is 0.0056 μg mL⁻¹. The instability constant of the method has been calculated by Asmus’ method as 6.476 × 10^–5, at room temperature. The interfering effect of various cations and anions has also been studied. The method was successfully applied for the determination of Mo(VI) in food and water samples. The validity of the present method was evaluated in terms of Student ‘t’ test and Variance ‘f’ test, which indicates the significance of the present method an inter comparison of the experimental values, using atomic absorption spectrometer.     

A Biotin–Streptavidin Amplified Enzyme-Linked Immunosorbent Assay with Improved Sensitivity for Rapid Detection of Ractopamine in muscular tissue Development and Nonspecific Adsorption Reduction

An effective biotin–streptavidin amplified enzyme-linked immunosorbent assay (BA-ELISA) was optimized and characterized for the rapid detection of Ractopamine (RAC) residue in muscular tissue. Purification of the RAC antiserum by protein A-Sepharose 4B followed with bovine serum albumin (BSA)-Sepharose 4B affinity chromatography enhanced the sensitivity and reduce the background adsorption. Blocking with 0.5% skimmed milk power and diluting streptavidin–HRP conjugates with 0.5% BSA/phosphate-buffered saline (PBS) effectively remove the nonspecific adsorption in biotin–streptavidin amplified ELISA system. The established method allowed RAC determination with an IC₅₀ value of 0.3 ± 0.02 ng ml⁻¹ and a limit of detection of 0.02 ± 0.003 ng ml⁻¹, more sensitive than the other reported methods. The variation coefficients of intra-assay and inter-assay were all below 7%. RAC residue in pig muscular tissue could be quantified without matrix effects after a 5-fold extraction and 2-fold dilution with PBS. Recoveries of RAC in pig muscular tissue ranged from 75% to 82.75%. The results were also compared with those from HPLC and a good correlation was obtained (r ² = 0.9822). The characters show that the established biotin–streptavidin amplified ELISA could be potentially useful in rapid detection of RAC in animal-derived foods.     

Effect of Processing Methods on Physical,Chemical, Rheological,and Sensory Properties of Okra (<Emphasis Type="Italic">Abelmoschus esculentus</Emphasis>)

Effects of freezing/thawing, sun drying, solar drying, and foam-mat drying on physical, chemical, rheological, and sensory attributes of okra were investigated. Average poured bulk and tapped bulk densities of sun-dried, solar-dried, and foam-mat-dried okra were 800 and 950, 715 and 765, 355 and 367 kg/m³, respectively. Minimum and maximum porosity of sun-dried, solar-dried, and foam-mat dried okra were 55.70% and 62.60%, 50.06% and 53.30%, 60.90% and 62.87%, respectively. Sun-dried and solar-dried okra showed higher L*, a*, and chroma values than frozen/thawed and foam-mat-dried okra. Within a temperature range of 80–40 °C, viscosity of fresh, frozen/thawed, foam-mat-dried, solar-dried, and sun-dried okra were 0.055–0.080, 0.055–0.075, 0.050–0.073, 0.005–0.065, and 0.005–0.022 Nsm⁻², respectively. Sensory evaluation showed no significant difference (p < 0.05) between fresh, frozen/thawed, and foam-mat dried okra in color, aroma, and overall acceptability. Sun-dried and solar-dried okra were significantly poorer (p < 0.05) in color, aroma, taste, and overall acceptability.     

The Application of NIR FT-Raman Spectroscopy to Monitor Starch Retrogradation and Crumb Firmness in Semolina Bread

In this study, the potential application of near-infrared (NIR) Fourier-transform (FT)-Raman spectroscopy to monitor starch retrogradation in stored bread crumb was investigated. Semolina-based bread was made and cut into slices, which were stored under controlled conditions in sealed plastic bags. The aging of the bread crumb was monitored by both NIR FT-Raman spectroscopy and a texture analysis over a period of 20 days. Two-dimensional correlation analysis in the spectral range of 390–975 cm⁻¹ revealed characteristic differences among the spectra collected over time for bands that peaked at 480, 765, and 850 cm⁻¹. The band at 480 cm⁻¹ is studied here in detail. During the storage, the peak frequency of this band shifted towards lower wavenumbers, and its full width at half height decreased. Both of these parameters are highly correlated (R ² = 0.921 and R ² = 0.949, respectively) to crumb hardness measured by the texture analyzer.     

Sorption Isotherms of Barnyard Millet Grain and Kernel

The moisture sorption isotherms of grain and kernel of barnyard millet (Echinochloa frumentacea) were determined at 20, 30, 40, and 50 °C. A gravimetric static method was used under 0.112–0.964 water activity (a _w) range for the determination of sorption isotherms. The models were compared using the coefficient of determination (r ²), reduced chi-square (χ ²) values, and on the basis of residual plots. In grain, modified Chung–Pfost (r ² > 0.99; χ ² < 0.7) and modified Oswin (r ² > 0.99; χ ² < 0.55) models were found suitable for predicting the M _e –a _w relationship for adsorption and desorption, respectively. Modified Henderson model was found to give the best fit (r ² > 0.99 and χ ² < 0.55) for describing the adsorption and desorption of the kernel. The isosteric heat, calculated using Clausius–Clapeyron equation, was varied between 46.76 and 61.71 kJ g⁻¹ mol⁻¹ at moisture levels 7–21% (d.b.) for grain and 47.11–63.52 kJ g⁻¹ mol⁻¹ at moisture level between 4% and 20% (d.b.) for kernel. The monolayer moisture content values ranged from 4.3% to 6% d.b. in the case of adsorption of barnyard millet grain and 5.2–6.6% d.b. in the case of desorption at the temperature ranges of 50–20 °C. The monolayer moisture values of barnyard millet kernel ranged from 4.4% to 6.67% d.b. in adsorption and 4.6% to 7.3% d.b. in desorption in the temperature ranges of 50–20 °C.