Development of plant-based products faces challenges like raw material standardization and time-consuming functionality measurements. Fourier Transform Infrared (FTIR) spectroscopy provides a quick, non-destructive way to analyze protein molecular characteristics. This study explored the classification capability of FTIR in analyzing five plant protein isolates-soy, mung bean, pea, fava bean, and lentil-and assessed its predictive ability for functional property measurement such as water absorption capacity (WAC), oil absorption capacity (OAC), Solubility (SOL), foaming, and emulsification. Functional properties were calculated using traditional methods of measurements. Principal Component Analysis (PCA) and Partial Least Square (PLS) Regression Analysis were used to study FTIR spectra and its correlation with functional properties. PCA revealed distinct clusters for each protein source based on their FTIR spectra, indicating molecular differences. WAC and OAC prediction models showed strong correlations, with prediction correlation coefficients (Rp) of more than 0.99 and cross-validation correlation coefficients (Rcv) ranging from 0.85 to 0.92. As sample size increases, SOL, emulsifying, and foaming properties display promising potential. Moreover, WAC and OAC predictions exhibited robust results with protein blends of various ratios. The expanded WAC model predicted with an Rp of 0.99 and an Rcv of 0.95, while the expanded OAC model had an Rp of 0.99 and an Rcv of 0.84. The results underscore FTIR has the potential to identify plant proteins aiding in raw material verification and quality control as well as being an alternative to analyzing functional properties of plant proteins.

Analytical validation is a sequence of operations aiming to evaluate the accuracy, reliability, and cost of analytical results for making informed decisions in method selection and meeting the requirements of regulatory institutions. This study aims to perform an analytical validation by comparing three different approaches: the accuracy profile, the uncertainty profile, and the conventional validation to assess the capability of each method in confirming the robustness of the results. The accuracy profile offers a comprehensive assessment of analytical performance and integrates systematic and random errors to determine if future results will satisfy the predefined acceptance limits. Meanwhile, the uncertainty profile, which is complementary and innovative, allows the uncertainty estimation from validation data. These approaches were developed after conventional validation that relies on statistical methodologies based on separate evaluations of method criteria to provide a comparative framework for evaluating new methods. This comparison will give recommendations for best practices related to analytical validation. The uncertainty profile is a graphical decision-making tool for determining full validation by integrating analytical validation and the estimation of measurement uncertainty, evaluating two statistical methods: β-expectation tolerance intervals and β-content, γ-confidence tolerance intervals, using a formula introduced by Saffaj δ Ihssane, predicting that 95% of future results will fall within the acceptance limits of ± 5%, revealing that the tolerance intervals for β-expectation are smaller than β-content, γ-confidence. The total error approaches offer robust recommendations for optimal methods for routine application. This study highlights the critical need for appropriate analytical validation and the challenges arising from the absence of clear guidelines for that purpose. Different approaches emphasize the significant impact of the choice of an adequate method, which remains pivotal for providing accurate results under real-world scenarios. Concrete examples and simulations illustrate the viewpoints associated with different approaches to making decisions.

Per- and polyfluoroalkyl substances (PFAS) comprise thousands of fluorinated chemicals. They are of growing concern because many PFAS compounds are persistent and toxic. Food contact materials (FCM) containing PFAS pose multiple exposure pathways to humans, prompting twelve states to enact laws banning FCM with PFAS levels exceeding 100 ppm of TOF. While LC-MS is often used to measure targeted PFAS compounds, much of the total PFAS content in the sample may be missed. To understand organic fluorine content in samples more comprehensively, we developed a method using combustion ion chromatography (CIC) to measure TOF and extractable organic fluorine (EOF) in FCM. This technology utilizes combustion under an oxygen and argon atmosphere. All gaseous, acidic combustion products are collected in water, with ions separated on an ion exchange column and detected by conductivity. Total fluorine (TF) was measured by combusting 10-50 mg of FCM. Total inorganic fluorine (TIF) was measured by extracting cryo-ground FCM with water followed by direct injection to the IC system. TOF was then calculated by subtracting TIF from TF. EOF was determined by CIC after extracting analytes from the ground FCM using 80% methanol/20% acetonitrile. The Method detection limit (MDL) for TOF is 0.51 ppm, exceeding the sensitivity requirements of current state regulations. A comparison of EOF to TOF revealed that EOF constitutes less than 15% of the TOF in the FCM samples. TOF is a critical metric for assessing PFAS contamination in FCM, as targeted LC-MS approaches may miss much of the PFAS in the samples. We developed a sensitive and automated method to determine TOF and EOF in FCM. The method can be used to screen for PFAS in FCM, ensuring compliance with current regulations on PFAS contamination.

Yogurt has emerged as an essential nutritional food in contemporary diets, and the development of new multi-component yogurt formulations has become a focal point of current research. In this study, the effects of fermentation compounds and the addition of sugar, soy milk on the quality and probiotic activity of milk-soy mixed yogurt were studied to determine the optimal formation of mixed yogurt. The various fermentation compounds (YO-MIX 883, Lactobacillus Casei complex starter cultures, Lactobacillus Paracasei compound starter cultures), different concentrations of milk-soy additions (0, 25, 50, 75, 100%) and sugar (2, 4, 6, 8%) were tested within each experimental group, and the pH, appropriate acidity, and total viable bacterial count of the fermented milk-soy mixed yogurt were determined throughout the fermentation and refrigeration processes. The obtained results showed that the Lactobacillus Paracasei complex was particularly effective for the fermentation of soy milk. The mixed yogurt formulation, comprising 50% soy milk and 4∼6% sucrose, exhibited enhanced acidity, superior sensory evaluation scores, and overall improved product quality. It was observed that during refrigeration, an increase in the milk content of yogurt corresponded to a more pronounced post-acidification effect. The optimal formulation for the milk-soy mixed yogurt identified in this research consisted of 0.3% Lactobacillus Paracasei compound fermenter, 6% sucrose, and 40% soy milk. Under these optimal conditions, the mixed yogurt achieved an acidity level of 76°T, a sensory score of 92 points, and a survival rate index of 1.25. Additionally, the yogurt exhibited a distinctive soybean aroma in its aftertaste, contributing to its overall quality. Furthermore, the probiotic survival index of the mixed yogurt containing 40% soy milk, following simulated gastrointestinal fluid digestion, was recorded at 0.767, indicating that the probiotic activity in this yogurt was significantly higher than that of other yogurts. The obtained results provide a theoretical foundation for the future industrial production of milk-soy mixed yogurt products.

Hemodialysis solutions are liquid concentrates used during hemodialysis sessions. They are commonly used as a renal replacement therapy. This study aimed to develop a method to determine Na, K, Ca, and Mg in hemodialysis solutions by high-resolution continuum source flame atomic absorption spectrometry (HR-CS F AAS) using Design of Experiments (DOE). The combination of the Doehlert Matrix with the desirability function was used to establish a compromise condition in the optimization of the significant variables studied: 60 L/h for acetylene flow rate, 8 mm for burner height, and 0.25% (w/v) and 0.60% (w/v) for Cs and La concentrations. The method was validated by following the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) guidelines and parameters, and, as such, the selectivity, linearity, precision, accuracy, and robustness were evaluated. Calibration curves with the ranges of 25-130 mg/L for Na, 1.0-5.0 mg/L for K and Ca, and 0.30-0.70 mg/L for Mg were employed. The method proved to be precise (RSD lower than 2.7%) and accurate (mean recovery data, contemplating the three levels added, were 103.0% for Na, 100.5% for K, 101.3% for Ca, and 101.5% for Mg). The developed method enables the sequential multielement determination of Na, K, Ca, and Mg in a single run. Requiring only one dilution step, this method significantly reduces analysis time for both sample and standard solution preparation and measurement. This study presents the first method reported in the literature for multielement determination in hemodialysis solutions, offering an alternative approach to the current European Pharmacopeia method.

The 11+Myco MS-PREP® Immunoaffinity Column (IAC) contains a gel suspension of monoclonal antibodies specific to the toxins of interest. Following sample extraction, the IAC is used for cleanup and concentration of mycotoxins prior to analysis by Liquid Chromatography with Tandem Mass Spectrometry (LC-MS/MS). This study evaluated the IAC with LC-MS/MS method for Performance Tested Methods SM certification for simultaneous determination and confirmation of Aflatoxins B1, B2, G1, G2, and M1; Deoxynivalenol, Fumonisins B1, B2, and B3; Ochratoxin A; T-2; HT-2; and Zearalenone from corn, wheat, cereal-based baby food (with and without dairy ingredients), paprika, chili powder and animal feed. A single extraction method using 50% Acetonitrile and water was used for all matrixes. The Method Developer validated all matrixes and an independent laboratory verified method performance on corn and animal feed. Data were analyzed for recovery, repeatability precision, LOD, LOQ, confirmation of identity, and method selectivity. Recovery (72%-138%) and repeatability (0.46%-24%), with the exception of sporadic data points, were within acceptance criteria. LOQ was estimated as AFB1 0.018-0.32 ꙡg/kg, AFB2 0.037-0.28 ꙡg/kg, AFG1 0.019-0.14 ꙡg/kg, AFG2 0.036-0.28 ꙡg/kg, DON 4.0-75 ꙡg/kg, Fumonisin B1 4.9-37 ꙡg/kg, Fumonisin B2 4.0-32 ꙡg/kg, Fumonisin B3 2.0-16 ꙡg/kg, OTA 0.15-4.4 ꙡg/kg, T-2 0.5-7.5 ꙡg/kg, HT-2 0.70- 7.5 ꙡg/kg), and ZON 1.3-7.2 ꙡg/kg), depending on matrix. Method performance was verified with reference and quality control materials. Selectivity and confirmation of identity were also demonstrated. The 11+Myco MS-PREP® IAC with LC-MS/MS method demonstrated acceptable performance for simultaneous determination of 12 mycotoxins in 7 matrixes. The data were reviewed by the AOAC Performance Tested Methods SM Program and approval was granted for certification of the 11+Myco MS-PREP® Method as PTM 112401.

White granulated sugar, a significant commodity in bulk trade and widely used raw material, plays a crucial role in the food, energy, and medicine industries. A certified reference material (CRM) of white granulated sugar provides a valuable tool for monitoring and maintaining the safety and quality of white granulated sugar and other related products. The colorimetric value, conductivity ash, sucrose content, and reducing sugar content serve as essential factors that determine the quality of white granulated sugar. Develop a CRM of grade one white granulated sugar, conduct a comprehensive study to assess its homogeneity and stability, and determine the designated property values. Collaborative certification across 11 laboratories was applied to validate its property values and evaluate corresponding uncertainties. The designated property values and expanded uncertainties (k = 2) determined to be 75.6 ± 2.8 IU, 0.0100 ± 0.0004 g/100g, 99.71 ± 0.08 g/100g, and 0.0226 ± 0.0024 g/100g for colorimetric value, conductivity ash, sucrose content, and reducing sugar content, respectively. The reference material (RM) was sufficiently homogeneous between and within bottles and remained stable for up to 20 months. The developed RM of the grade one white granulated sugar could be an effective support for method validation, capability validation, quality control, and metrological traceability in the sugar and food industries.

Melatonin supplements are often used to alleviate jetlag and other sleep-depletion related disorders. Recent studies found large inconsistencies between labeled values and actual contents of melatonin within products, which has led to concerns over the quality of melatonin supplements. In order to facilitate the quality control testing of melatonin supplements, an improved and more modern approach to the liquid chromatographic analysis of melatonin is required. In addition, growing public concern over the environmental footprint of analytical laboratories exacerbates the need to modernize legacy analytical procedures with more eco-friendly or greener approaches. This study aims to optimize the routine liquid chromatographic analyses that are prescribed in the US Pharmacopeia (USP) melatonin monograph on a High Performance Liquid Chromatography (HPLC) system without fundamentally modifying the methods. The melatonin assay and the melatonin related compounds (impurities) test were optimized on a C18 column packed with 2.5 µm particles. The column length and the gradient elution parameters were adjusted following the guidelines on Adjustment of Chromatographic Conditions in USP General Chapter <621>. The mobile phase compositions were optimized to meet the system suitability requirements that were specified in the USP melatonin monograph. The flow rate was optimized for better separation efficiency. The optimized HPLC methods not only met the USP system suitability requirements in relative retention time (RRT), resolution, and relative standard deviation (RSD), but also demonstrated excellent linearity, sensitivity, accuracy, precision (repeatability), and would have a lower environmental impact. The optimized HPLC methods for assay of melatonin and test of its related compounds achieved significantly increased throughput and a reduced environmental impact, without fundamentally modifying the methods. The optimized HPLC methods are significantly faster and more eco-friendly. These methods can be implemented on HPLC systems without a full re-validation.