Official Method Research Articles

Morpho-Phytochemical Composition of Sesame (<i>Sesamum</i> <i>indicum</i> L.) Varieties Grown in Lafia, Nasarawa State, Nigeria

The study, Morpho-phytochemical composition of sesame (Sesamum indicum) varieties grown in Lafia, Nasarawa state-Nigeria. The experiment was conducted at the Botanical Garden of the Federal University of Lafia, Nasarawa State. Sesame varieties were obtained from National Cereal Research Institute Baddegi, Niger State. The varieties obtained include: GUJ BLACK, CHI001, and NCRIBEN 04E, NCRIBEN 05E and E8. The experiment was laid out in a randomized complete block design with three replications. Data were collected on the basis of Number of days for germination, Number of days to flowering, Plant height at flowering, Number of leaves per plant, Number of branches per plant, Number of branches at 50% flowering, Plant height at maturity, Number of pods per plant, Number of seeds per plant and 1000 seed weight. 30 g of sesame seeds from each varieties were grounded and analyzed for six proximate traits. Data were recorded for crude protein, crude fat/oil, fibre, mineral ash, moisture content and carbohydrate content. All proximate analyses were done according to Official methods of Associations of Analytical Chemist (AOAC). Data collected were subjected to ANOVA P ≤ 0.5. The varieties GUJBLACK and E8 performed very well in most of the morphological characterization such as days to germination, germination percentage, number of leaves, plant height, number of branches and 100 seed weight. Phytochemical composition of different varieties revealed that the variety GUJBLACK has the highest concentration of alkaloid, flavonoid, phenols, glycosides and saponin. The least varieties performance were observed in NCRIBEN 05E and NCRIBEN 04E.

Fourier‐transform mid‐infrared spectroscopy for high‐throughput phenotyping of total dietary fiber in pulse crops

AbstractThis study uses Fourier‐transform mid‐infrared (FT‐MIR) spectroscopy as a high‐throughput phenotyping tool to quantify total dietary fiber (TDF) in chickpea (Cicer arietinum L.), dry pea (Pisum sativum L.), and lentil (Lens culinaris Medik.) for pulse crop breeding purposes. The standard analytical approach for TDF analysis is based on the Association of Official Analytical Collaboration method 985.29, which requires extensive sample preparation with extended analysis times of up to 30 h. The FT‐MIR approach was developed to enhance rapid and non‐destructive analysis and minimize the traditional workload associated with phenotyping TDF in pulse crops by accomplishing the same task in a shorter time and at minimal cost. Partial least squares regression (PLSR) was applied with chemometric modeling in MIR regions (650–1480 and 2771–3700 cm−1), encompassing spectral bands associated with undigested polysaccharides and partially or undigested protein and fatty acid methyl ester fractions that fingerprint TDF. K‐fold cross‐validation was used for PLSR modeling to enhance computational speeds with large‐scale data processing. These PLSR models for chickpea, dry pea, and lentil have coefficients of determination (R2) as 0.91, 0.96, and 0.94 with root mean square errors of prediction in the range of 0.05–0.5 g/100 g. This technique supports rapid phenotyping of TDF from raw flour in <1 min. The FT‐MIR technique can relieve the phenotyping bottleneck in pulse breeding and pulse‐based food and feed industries, targeting the measurements of TDF and ensuring a rapid and high‐throughput pipeline for plant breeding and cultivar development.

What's up ducks? - Antimicrobial resistance of Escherichia coli isolated from duck farm environment in Poland extended with genomic characteristics of cephalosporin-resistant strains.

What's up ducks? - Antimicrobial resistance of Escherichia coli isolated from duck farm environment in Poland extended with genomic characteristics of cephalosporin-resistant strains.

Spatial Representativeness of Air Quality Monitoring Networks in China From 2013 to 2022: Implications for Exposure Assessment

AbstractThe spatial representativeness (SR) of air quality monitoring sites is critical for ensuring that gathered data accurately reflect the broader area's air quality. Evaluating the SR of sites at a national scale and its long‐term trends is particularly important for countries like China, where both air quality and monitoring networks have changed dramatically over time. Here, we used 1‐km daily air pollutant concentrations from the China High Air Pollutants dataset to assess the yearly SR of state‐controlled sites in China from 2013 to 2022 for multiple pollutants. With the number of sites increasing from 460 in 2013 to 1,590 in 2022, our results showed that the total SR area of sites increased by 89% for PM2.5, 149% for PM10, and 2,190% for O3. While the number of sites mainly drove these increases, its impact varied at different phases. Interestingly, the rise in sites from 2020 to 2022 actually led to a decrease in the total SR area for PM2.5 (−18,300 km2) and PM10 (−14,200 km2). Additionally, we found that applying SR to pollution exposure assessments did not improve their accuracy at national and city levels when compared to the official method, which involves exposure calculation using arithmetic mean aggregation of monitoring sites. This was related to poor SR performance, with more than half of the population being uncovered by SR areas in more than 85% of Chinese cities. Nevertheless, we demonstrated the benefits of applying SR for city‐level air quality attainment.

A review on validated analytical methods for Ramipril

Ramipril is the drug is official in British Pharmacopoeia used to treat high blood pressure (hypertension) and heart failure. The official method of analysis of Ramipril is potentiometric method. Several UV spectrophotometric, HPLC methods in pure form, pharmaceutical formulation and HPTLC methods have been reported to determine. This review provides an overview of various analytical techniques used for Ramipril determination both in a single preparation and in combination.

The Mobile Divider Method: An Effective Strategy to Detect Small Hive Beetle (Aethina tumida) Adults in Honey Bee Colonies (Apis mellifera) in Calabria, Italy

Aethinosis, the honey bee disease caused by small hive beetle, is listed in the Animal Health Law and requires mandatory surveillance and control measures. The Mobile Divider (MD) method has been proposed as a time-saving alternative to the official surveillance method outlined by the Ministry of Health (MoH). The current study aimed to evaluate the efficacy of the MD method in concentrating SHBs behind the MD and optimizing the number of SHBs detected during hive inspections, thereby improving the surveillance strategies required by European regulations and the WOAH. In late winter and autumn 2022, we conducted 431 hive inspections across six apiaries in the province of Reggio Calabria, Italy. A total of 379 adult SHBs were collected and killed; no larvae were detected. Using the MD method, 238 SHBs were found behind the MD, while 141 SHBs were found in the remaining volume of the hive. Chi-square analysis confirmed the effectiveness of the MD method, showing that the SHB distribution behind the MD and in the remaining volume of the hive was not random (p < 0.0005). Further studies are needed to assess the effectiveness and potential benefits of the MD method in regions with higher SHB infestation levels.

SPE-HPLC-DAD Dosage of Seven Neonicotinoids in Green Coffee.

Green coffee is essential in many tropical economies. Its cultivation often necessitates using pesticides that can leave behind residues harmful to human health. To ensure consumer safety, the European Community has set strict maximum residue limits (ranging from 0.01 to 1.0 mg/kg) for pesticides in green coffee sold within Europe. However, the lack of official testing methods for neonicotinoids (NEOs) is a problem, as laboratories must spend resources and time developing and validating suitable analytical methods. This study developed and validated a method for the simultaneous analysis of seven NEOs frequently used in coffee cultivation: acetamiprid, clothianidin, dinotefuran, imidacloprid, nitenpyram, thiacloprid, and thiamethoxam. The proposed methodology uses Strata®-X PRO cartridges (solid-phase extraction) to remove interfering compounds present in the food matrix and high-performance liquid chromatography (HPLC), equipped with a diode array detector (DAD), to determine NEOs. The accuracy profile strategy validated the method's suitability for the intended application. NEO recovery rates above 97%; negligible matrix effects (>93%); the linearity of the quantification method (R2 values above 0.99); relative biases and standard deviations below 5% and 6%, respectively; and an expected error rate less than 8% allowed to consider the method reliable for the intended objectives. Because of its low ecological impact and simple execution, this method can be used in routine analyses.

Validation of Enzytec™ Liquid D-Lactic acid for Enzymatic Determination of D-Lactic acid in Selected Foods and Beverages: Official Method 2024.06 First Action.

D- and L-lactic acid are produced naturally by lactic acid bacteria and are found in fermented milk products, pickled vegetables, and cured meats. D-lactic acid is formed by some microorganisms only, e.g., Lactobacillus lactis, and Leuconostoc cremoris. D-Lactic acid is not formed or only in traces by "higher organisms", e.g., by animals. Therefore the presence of D-lactate may serve as an indicator for microbial contamination or spoilage, assuming that fermentation techniques have not been used. To validate the performance of the Enzytec™ Liquid D-Lactic acid for the determination of D-lactic acid in food and beverages such as milk and (fermented) milk products, fermented vegetable products, wines, beer, fruit and vegetable juices, egg and egg powder. The kit contains two ready-to-use components which makes handling easy and suitable for automation. D-lactic acids react in the presence of NAD and D-lactate dehydrogenase to pyruvate and NADH. The NADH formed is equivalent to the amount of D-lactic acid converted. Ascorbic acid, 3-hydroxybutyric acid, and sulfite interfere at concentrations higher than 0.2, 0.2, and 0.05 g/L, respectively. Oxaloacetic acid, pyruvic acid and D-fructose do not interfere at or below concentrations of 0.2, 1, and 10 g/L, respectively. The calculated LOD when using a test volume of 100 µL is 5.4 mg/L and the LOQ is 15 mg/L. The practical upper measurement range is 600 mg/L. Relative intermediate precision was between 3.5 and 5.7% for pineapple juice, sauerkraut juice, wine and liquid egg. A reference material (wine) showed recoveries of 108%. For automation, three applications with different test volumes were validated. Linearity is given from 0.75 up to 3125 mg/L. The method is robust and accurate and was approved as AOAC Official Method of Analysis℠. The ready-to-use components of the test kit have a shelf life of at least 24 months.

Validation of Enzytec™ Liquid D-Glucose for Enzymatic Determination of D-Glucose in Selected Foods and Beverages: Official Method 2024.03 First Action.

Glucose is the most abundant monosaccharide. Glucose is mainly made by plants during photosynthesis from water and carbon dioxide, using energy from sunlight. It is therefore contained in many foodstuffs naturally or added later as an ingredient. To validate the performance of the Enzytec™ Liquid D-Glucose for the determination of D-glucose in food and beverages such as fruit and vegetable juices, soft drinks, wines, and beer. The kit contains two ready-to-use components which makes handling easy and suitable for automation. D-Glucose is phosphorylated to glucose-6-phosphate (G-6-P) by a hexokinase and ATP. In the presence of glucose-6-phosphate dehydrogenase and NAD, G-6-P reacts to gluconate-6-phosphate, whereby NADH is formed and measured at a wavelength of 340 nm within 20 minutes. Mannose and D-fructose interfere at 5.1 and 12.5 g/L (or more), respectively. Sulfite does not interfere up to 1.25 g/L. The calculated LOD and LOQ when using a test solution volume of 100 µL are 1.4 and 4 mg/L, respectively. The linear measurement range is from 4 to 2000 mg/L D-glucose. Trueness was checked by using materials from NIST (cranberry juice) and one reference wine from the German Wine Analysts. Spiking of wine, beer, and juices resulted in recoveries between 93 and 101%. Analysis of NIST SRM 3282 resulted in an intermediate precision of 4.1%. For automation, three applications with different test solution volumes and different but overlapping measurement ranges were validated. Linearity is given from 2.4 up to 10000 mg/L. The method is robust and accurate for manual and automated applications. The method was approved as AOAC Official Method of Analysis℠. The ready-to-use components of the test kit have a shelf life of at least 29 months from date of manufacture.

Validation of Enzytec™ Liquid D-/L-Lactic Acid for Enzymatic Determination of D- and L-Lactic Acid in Selected Foods and Beverages: Official Method 2024.08 First Action.

Produced naturally by lactic acid bacteria, L-lactic acid is found in many fermented milk products such as yogurt, and also in pickled vegetables, cured meats and fish. It also serves as a quality parameter in wine, beer, whole egg, whole egg powder, and juices. To validate the performance of the Enzytec™ Liquid D-/L-Lactic acid for the determination of the sum of D- and L-lactic acid in food and beverages such as milk and (fermented) milk products, fermented vegetable products, wines, beer, fruit and vegetable juices, egg and egg powder. The kit contains two ready-to-use components which makes handling easy and suitable for automation. Both lactic acids react in the presence of NAD and D- or L-Lactate dehydrogenase to pyruvate and NADH. The NADH formed is equivalent to the amount of D-/L-lactic acid converted. Ascorbic acid, 3-hydroxybutyric acid, and sulfite were found to have a low activity at concentrations higher than 0.5, 0.05, and 0.1 g/L, respectively. Oxaloacetic acid and D-fructose do not interfere at concentrations at or below 0.2 and 20 g/L, respectively. The calculated LOD when using a test solution volume of 100 µL is 3 mg/L and the LOQ is 10 mg/L. The practical upper measurement range is 600 mg/L. Relative intermediate precision was between 3.8 and 5.3% for pineapple juice, sauerkraut juice, wine and liquid egg. Cream cheese Certified Reference Materials showed a recovery between 98 and 103%. A reference wine was found with a recovery of 104%. For automation, three applications with different test solution volumes were validated. Linearity is given from 4 up to 3125 mg/L. The method is robust and accurate and was approved as AOAC Official Method of Analysis℠. The ready-to-use components of the test kit have a shelf life of at least 24 months.

Development of an Accurate Method based on MAD-SRC for the Determination of Metals and Sulfur in Crude Oil Atmospheric and Vacuum Residues by ICP OES

The present study proposes for the first time a microwave-assisted digestion in an ultra-high pressure single reaction chamber (MAD-SRC) method for the digestion of atmospheric residue (AR) and vacuum residue (VR) from crude oil distillation. The determination of metals and sulfur was performed by inductively coupled plasma optical emission spectrometry (ICP OES). The type of digestion solution (HNO3 or HNO3 + H2O2), the volume of digestion solution (6 to 10 mL), maximum temperature (200 ºC and 270 ºC), and sample mass (up to 1000 mg) were evaluated. Using 1000 mg, 8 mL of HNO3, and 270 °C the final digests presented carbon concentrations lower than 2500 mg L-1 for both crude oil AR and VR. The accuracy of MAD-SRC was evaluated by using a certified reference material, recovery tests, and comparison with results obtained by using microwave-induced combustion (MIC). No statistical difference was observed between the results obtained after the proposed MAD-SRC method and the certified values and recoveries higher than 95% were obtained for all analytes. Comparing the results obtained by the MAD-SRC method with those obtained by MIC, an agreement higher than 95% was achieved for all analytes. The relative standard deviation was always lower than 7%. The quantification limits ranged from 0.06 µg g-1 for Ba to 3.13 µg g-1 for S enabling metals and sulfur determination in crude oil distillation residues virtually free of interferences. The main advantages of the proposed method is the possibility to digest up to 1000 mg of crude oil AR and VR without the use of relatively long processing time and with lower risks of contamination and volatilization of analytes when compared to an official method using open vessels (about 240 min). In addition, it was possible to obtain digests fully compatible with the determination technique making this method a suitable option for the routine quality control of crude oil AR and VR.

Evaluation of Modified QuEChERS Using Small-Scale SPE for the Analysis of Organophosphorus Pesticides in Spinach.

The Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method has been widely applied to various compounds and matrices. However, the clean-up process of QuEChERS with dispersive solid-phase extraction (d-SPE) is considered to be not always sufficient. Therefore, a modified QuEChERS using small-scale SPE (abbreviated as "modified QuEChERS") for the clean-up process has seen an increasing number of users in Japan; it is therefore necessary to evaluate its performance. To evaluate the performance of modified QuEChERS for the analysis of nine organophosphorus pesticides (OPPs) in spinach, and to compare the various parameters among modified QuEChERS, QuEChERS, and the Japanese official multiresidue method (JOMM). The modified QuEChERS was evaluated by a recovery test using blank spinach samples and quantification using a pesticides-containing quality control spinach sample. A matrix effect was also evaluated for gas chromatography with mass spectrometry (GC/MS) with the stomach-shaped spiral large volume injection (LVI). Various parameters including accuracy, time, cost, and clean-up effect were compared among modified QuEChERS, QuEChERS, and JOMM. The mean recoveries, the intra-day repeatability, and the inter-day reproducibility for modified QuEChERS were acceptable according to the validation guideline. The concentration of fenitrothion in the pesticides-containing quality control spinach sample obtained by modified QuEChERS was comparable that obtained by QuEChERS and JOMM. It was found that the clean-up of the blank spinach sample by modified QuEChERS using small-scale SPE can be more effective than that by QuEChERS using d-SPE. A matrix effect was newly evaluated in our analysis by GC/MS with the stomach-shaped spiral LVI. The modified QuEChERS is an accurate and simple method of analyzing OPPs in spinach. The modified QuEChERS is not only accurate but also a fast, cost-effective, and environment-friendly method for analyzing OPPs in spinach.

Authentication of Indian Honey Based on Carbon Stable Isotope Ratio Analysis—Verification of Indian Regulatory Criteria

The present study was undertaken for the first time in India to generate a database of isotopic signatures of authentic Indian honey to verify the regulatory criteria laid down by the Food Safety and Standards Authority of India (FSSAI). In this study, ninety-eight (98) authentic honey samples from nineteen (19) different botanical sources were collected from five (05) geographical regions of India and analyzed to generate a database of stable carbon isotope ratios (13C/12C) by Elemental Analyzer/Liquid Chromatography–Isotopic Ratio Mass Spectrometry (EA/LC-IRMS). The samples were analyzed for the parameters δ13CHoney(δ13CH), δ13CProtein(δ13CP), δ13C individual sugars, ∆δ13CProtein-Honey(δ13CP-H), C4 sugar, ∆δ13CFructose-Glucose(δ13CFru-Glu), ∆δ13Cmax, and foreign oligosaccharides (FOs), as per the official methods of analysis of the Association of Official Analytical Chemists (AOAC 998.12) and the FSSAI. The results were evaluated against the published literature and Indian regulatory criteria for authentic honey. The δ13C value for honey (δ13CH) ranged from −22.07 to −29.02‰. It was found that 94% of Indian honey samples met the criteria for Δδ13CP-H (≥−1.0‰), Δδ13CFru-Glu (±1.0‰), and C4 sugar content (7% maximum), with negative C4 sugar values treated as 0% as prescribed by the AOAC method. Further, 86% of samples met the FO criteria (maximum 0.7% peak area). Thus, the data of this study provide scientific backing for these four (04) parameters as per the FSSAI regulation. However, the non-compliance of a high number (47%) of authentic honey samples for Δδ13Cmax (±2.1‰) compels further systematic investigation with a special focus on bee feeding practices. Further, in the present study, it was found that honey samples with a Δδ13CP-H greater than +1‰ and a C4 sugar content more negative than −7% also did not comply with the Δδ13Cmax criteria. Hence, Δδ13CP-H values (>+1‰ equivalent to C4 sugar < −7%) could be an indicator of C3 adulteration to some extent.

DEVELOPMENT AND VALIDATION OF RELATED SUBSTANCE BY HPLC FOR DIPHENHYDRAMINE HYDROCHLORIDE SOFT GEL CAPSULE

Objective: Many over-the-counter drug products does not have official compendial analytical methods for the analysis of the drug product. Thus, the United States Pharmacopeia (USP) are seeking to develop and validate new methods to establish analysis standards for the assessment of pharmaceutical over-the-counter drug products. One such method is the related substances by high-performance liquid chromatographic (HPLC) of diphenhydramine hydrochloride capsule. Methods: A reversed-phase high-performance liquid chromatographic method for related substances of diphenhydramine hydrochloride capsule was developed comprising of YMC pack pro C8 column 250×4.6 mm, S-5µm, 12 nm HPLC column using waters Alliance 2690 HPLC system with a mobile phase of 65% of pH 3 monobasic potassium phosphate buffer and 35% of acetonitrile. The flow rate was 1.2 ml/min, 10 µl injection volume, at 220 nm wavelength with the column temperature of 25 °C. The method was validated as per International Council for Harmonisation of Technical Requirements for Pharmaceuticals (ICH) Q2R2 guidelines for specificity, precision (system precision, method precision), linearity, accuracy, solution stability and robustness (filter study). Results: The method found to be specific without any interference from placebo and spiked sample with the retention time of 5.2 min, 5.5 min, 7.0 min, 23.2 min and 46.1 min for Diphenhydramine Related Compound-A (DRC-A), diphenhydramine hydrochloride, Diphenhydramine N-Oxide (DNO), benzhydrol and benzophenone respectively. The % Relative Standard Deviation (RSD) for DRC-A, DNO, benzhydrol and benzophenone was observed to be as 6.2, 5.9, 6.3 and 5.5, respectively. The accuracy ensures the detection and quantification at a very low level for all impurities [Limit Of Quantification (LOQ) 0.03%] with coefficient correlation of 0.9999, 0.9977, 0.9992, 0.9995,0.9990 and % RSD for LOQ precision was determined as 0.9, 2.1, 0.8, 1.9 and 8.0 for DRC-A, diphenhydramine hydrochloride, DNO, benzhydrol and benzophenone respectively. Since, DNO impurity is degradation impurity and vital in drug products and required to address its consistency and assurance towards the safety of patient, this method ensures to quantitate it at low level with precision and accuracy. Thus, the consistent, linear, precise, accurate and stability indicating results makes it more suitable for quantification of related substances in finished product and stability analysis. Conclusion: The study findings shows that the method is quite simple and applicable for release of finished product for the related substance analysis of diphenhydramine hydrochloride soft gel capsule.

Effect of sediment on fluvial phosphorus and aquatic water quality.

Effect of sediment on fluvial phosphorus and aquatic water quality.

A systematic review of zinc, iron and vitamin B12 content of edible insects and comparison with dietary reference values.

Entomophagy (eating edible insects) could potentially address human deficiencies of iron, zinc and vitamin B12. This article aims to summarize available evidence about iron, zinc and vitamin B12 content of raw and processed edible insects and these contents compared with nutritional needs of different human life stages. A systematic literature search using specific key words (edible insects, iron content, zinc content, vitamin B12 content, and nutritional composition) in Web of Science and Scopus databases was performed. Forty six studies were reviewed. To ensure standardized comparisons, articles with nutrient-enriched edible insects were excluded. The quality of records was assessed using standardized protocols. Results indicate that edible insects are generally either "sources of" or "rich in" iron, zinc and vitamin B12 required for optimal nutrition and health of different human life stages. Moreover, iron, zinc and vitamin B12 content of edible insect species were generally either comparable to or higher than that of lean (beef, pork), poultry and kidney beans. Most insect species were oven processed with little/no species specific data for other processing methods. Variations in micronutrient content existed between processing methods and among oven processed edible insects. Data inaccuracies, poor data quality control and lack of insect-specific official analytical methods contributed to fairly high variations and made comparisons difficult. Based on available data, edible insects can potentially address human deficiencies of iron, zinc and vitamin B12, despite the observed variations, data gaps, lack of edible insect matrix-specific official methods in addition to limited human bioavailability and efficacy studies.

Physicochemical and functional properties of bulla from Ensete ventricosum for food applications

IntroductionEnset (Ensete ventricosum) is, a perennial crop native to Ethiopia, yields a variety of starch-based foods. It serves as a staple food for approximately 24 million people, which is roughly 20% of the Ethiopian population. This study aimed to investigate the impacts of different parts of Ensete ventricosum and pressing cycles on the proximate composition, functional properties, and mineral content of bulla extracted from the pseudostem and corm, across multiple processing stages.MethodsThe proximate composition including moisture content, ash, fat, fiber, and Crude protein were determined using the official AOAC method 920.87. Carbohydrates were measured according to the method outlined by FAO and World Health Organization, while gross energy content was calculated based on the Atwater conversion factors. The functional properties of bulla extracted from Enset (Ensete ventricosum) such as bulk density, water absorption capacity, oil absorption capacity Swelling power and solubility were also analyzed using different standard analytical methods. Mineral contents were analyzed using Scanning Electron Microscopy (SEM) coupled with Energy-Dispersive X-Ray Spectroscopy (EDS).ResultsThe yield of Bulla from the first, second, and third pressings of the pseudostem was 89.1 grams (25.86%), 20 grams (5.80%), and 14 grams (4.06%), respectively. The proximate composition revealed moisture content ranging from 15.35 to 16.10%, ash content from 0.205 to 0.335%, crude fiber from 0.405 to 0.300%, protein from 0.595 to 0.760%, and carbohydrate content from 0.570 to 0.760%. The functional properties of Bulla, including bulk density (BD), water absorption (WA), solubility index (SI), oil absorption (OA), and swelling power (SWP), ranged from 0.645 ± 0.006 to 0.813 ± 0.009 (g/mL), 1.803 ± 0.077 to 4.413 ± 0.286 (%), 3.100 ± 0.424 to 6.391 ± 0.136 (%), 1.752 ± 0.011 to 2.043 ± 0.003 (mL/g), and 4.945 ± 1.133 to 7.430 ± 0.940, respectively. All values represent the mean ± SD of replicate analyses. The elemental composition of Bulla showed ranges for oxygen from 53.05 to 91.1, sodium from −2.45 to 2.33, magnesium from −0.99 to −0.02, potassium from 0.47 to 4.91, copper from −3.73 to 11.94, zinc from −1.87 to 3.96, selenium from −1.24 to 0.95, calcium from 0.02 to 0.43, and iron from −0.55 to 4.06. All mineral content results are presented in weight% and atomic %.DiscussionThe study revealed significant impacts of enset pressing cycles and fractions on the physicochemical, functional, and mineral composition of bulla derived from the pseudostem and corm of the yeshraqinqey enset plant. The carbohydrates dominate the composition, with moderate levels of fiber, protein, and fat contributing to its functionality as a food stabilizer and thickener. The corm was identified as a rich source of calcium and iron, enhancing its gelling and stabilizing properties, while the pseudostem bulla exhibited high potassium, supporting its viscosity-modifying potential. The pseudostem bulla showed a particular affinity for viscosity enhancement, while the corm-derived bulla excelled in gelling and stabilizing functions. The study contributes to a deeper understanding of the effects of different processing methods on the properties of bulla, paving the way for enhanced utilization of enset Bulla in various food applications.

Simultaneous Measurements of Nanotrace Amounts of Lead and Cadmium Using an Environmentally Friendly Sensor (An Activated Glassy Carbon Electrode Modified with a Bismuth Film).

This paper shows the fabrication of a new environmentally friendly sensor, an activated glassy carbon electrode with an in situ deposited bismuth film (aGCE/BiF), to determine Cd(II) and Pb(II) at the nanotrace level. The electrochemical activation of the GCE surface was achieved in a solution of 0.1 M phosphate-buffered saline (PBS) of pH = 7 by performing five cyclic voltammetric scans in the range of -1.5-2.5 V at ν of 100 mV/s. The newly developed electrode provides several advantages, such as an increased electron active surface (compared to the glassy carbon electrode) and improved electron transfer kinetics. As a result, the new voltammetric procedure (square-wave anodic stripping voltammetry, SWASV) was established and optimized. With the SWASV method, the following calibration curves and low detection limits (LODs) were obtained for Cd(II) and Pb(II), respectively: 5-100 nM, 0.62 nM, 2-200 nM, and 0.18 nM. The newly prepared method was used to determine the amounts of Pb(II) and Cd(II) in the certified reference material, and the results agreed with the certified values. Moreover, the procedure was successfully applied to determine the Cd(II) and Pb(II) in river samples. The official and standard addition methods validated the measurement results.

Time dependence of the pre-chromatographic oxidation method for bivalves contaminated with paralytic shellfish poisoning toxins

The neurotoxins of the saxitoxin family can be the origin of the human neurological syndrome of paralytic shellfish poisoning via contaminated marine bivalve vectors. A pre-chromatographic oxidation method is the official testing method in the EU, also known as the ‘Lawrence method’. It involves several steps, including toxin extraction, solid-phase clean-up, and oxidation to produce fluorescent derivatives. Despite the manual peroxide oxidation involving four pipetting steps, high coefficients of determination were commonly obtained for the calibration curves of the respective toxin oxidation products. However, the 11-hydroxysulphate toxins dcGTX2 + 3, C1 + 2 and GTX2 + 3, often had slightly lower coefficients of determination (i.e. R 2 < 0.998) than their non-11-hydroxysulphate counterparts dcSTX, GTX5 and STX (i.e. R 2 > 0.998). Deviations of ±10 s from the respective standard reaction times, caused significant alterations in fluorescent yield for toxins quantified with peroxide but not for those quantified with periodate. The oxidation is an endothermal reaction, and its reaction rate is toxin-specific, with the N11-hydroxysulphate toxins having a slower reaction rate. This was confirmed by incubating GTX2 + 3 and STX at different reaction times. The incubation of toxins in a bivalve matrix also slows down the reaction in comparison with oxidation in dilute acetic acid, giving lower recoveries, as studied here in detail for dcGTX2 + 3. Circumventing the matrix effect by dilution is not possible, as 10% of matrix is enough to cause a reduction to half of the fluorescence yield of dcGTX2 + 3. When heating the N1-H toxins with peroxide, the increase in fluorescence yield is inversely proportional to the recovery values commonly found for each toxin.

Validation of Enzytec™ Liquid L-Lactic Acid for Enzymatic Determination of L-Lactic Acid in Selected Foods and Beverages: Official Method 2024.07 First Action.

Produced naturally by lactic acid bacteria, L-lactic acid is found in many fermented milk products and also in pickled vegetables, cured meats and fish. It serves as a quality parameter in wine, beer, whole egg, whole egg powder, and juices. To validate the performance of the Enzytec™ Liquid L-Lactic acid for the determination of L-lactic acid in food and beverages such as milk and (fermented) milk products, fermented vegetable products, wines, beer, fruit and vegetable juices, egg and egg powder. The method is based on enzymes which are part of a prepackaged kit that contains two ready-to-use components which are suitable for automation. L-lactic acids react in the presence of NAD and L-Lactate dehydrogenase to pyruvate and NADH. The NADH formed is equivalent to the amount of L-lactic acid converted. Ascorbic acid, 3-hydroxybutyric acid, and sulfite were found to interfere at concentrations higher than 0.2, 0.05, and 0.05 g/L in the test solution, respectively. Oxaloacetic acid and D-fructose do not interfere at concentrations at or below 0.2 and 10 g/L, respectively. The calculated LOD when using a test volume of 100 µL is 3.8 mg/L and the LOQ is 10 mg/L. The practical upper measurement range is 600 mg/L. Relative intermediate precision was between 3.0 and 7.3% for pineapple juice, sauerkraut juice, wine and liquid egg. Certified Reference Materials (cream cheese and wine) showed recoveries between 100 and 104%. For automation, three applications with different test volumes were validated. Linearity is given from 0.75 up to 3125 mg/L. The method is robust and accurate for manual and automated applications. The method was approved as AOAC Official Method of Analysis℠. The components of the test kit have a shelf life of at least 24 months.