Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1431 - 1431 Abstract: Recently, I came across an article on the history of the Journal of AOAC INTERNATIONAL (J. AOAC Int.) in the March–April 2023 issue of Inside Laboratory Management (ILM), a bimonthly magazine of AOAC INTERNATIONAL available exclusively to its members. Information like this is not readily available, and this is the first and only article I have read offering a systematic and comprehensive overview on the history of J. AOAC Int. since being a member of AOAC for more than 20 years. Because many of the authors and readers of J. AOAC Int. may not be members of AOAC International but are likely interested in the history of J. AOAC Int., I decided to relay and share some of the information from that article in this editorial, and I hope everyone will find it as informative as I did. However, I do encourage everyone to join AOAC to ensure you don’t miss information on news and updates on AOAC initiatives, events, meetings, trainings, Official MethodsSM and Performance Tested MethodsSM, and much more. To join, visit https://www.aoac.org/membership/join-aoac-info/. PubDate: Mon, 31 Jul 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad089 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1432 - 1437 Abstract: AbstractBackgroundMarbofloxacin (MAR) is a veterinary antimicrobial, marketed in injectable solution, oral suspension, and tablets. MAR has no monograph for tablet evaluation in official compendiums. High Performance Liquid Chromatography (HPLC) methods present in the literature for evaluating MAR in tablets do not follow the principles of green and sustainable analytical chemistry.ObjectiveA green, clean, and sustainable method by HPLC was developed and validated to evaluate the content and stability of MAR in tablets, in addition to comparing it with other methods available in the literature.MethodA C8, 5 µm, 4.6 × 150 mm (ACE®) column, purified water with 0.2% formic acid–ethanol (70:30, v/v) as the mobile phase, and a flow rate of 0.7 mL/min at 296 nm were used.ResultsThe method was linear over a concentration range of 1–10 μg/mL, selective for tablet matrix and forced degradation, precise with relative standard deviations (RDS) less than 5%, accurate with recovery of 99.99%, and robust to changes in the mobile phase, flow rate, wavelength, equipment, and column brand. The retention time for MAR was approximately 3.1 min.ConclusionsThe method can be used in routine analysis of MAR in tablets in chemical-pharmaceutical laboratories. Furthermore, it can be used to verify the stability of MAR-based products and proved to be interchangeable with spectrophotometric method in the UV region and turbidimetric microbiological method.HighlightsA green method for evaluation of marbofloxacin tablets by HPLC was developed and validated. Additionally, it has been shown to be interchangeable with UV and turbidimetric methods. PubDate: Thu, 07 Sep 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad102 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1438 - 1442 Abstract: AbstractBackgroundHypericin (HYP) is a natural compound widely used as a food supplement. The encapsulation of HYP into nanosystems, such as nanostructured lipid carriers (NLC), is a promising strategy for delivering this lipophilic molecule and protecting it from degradation.Objective This study aims to develop and validate an analytical method to quantify the encapsulation efficiency of HYP in NLC.MethodA reverse-phase high-performance liquid chromatography (HPLC) method was developed and validated according to the International Conference on Harmonization (ICH) guide Q2 (R1). NLC was prepared through the ultrasonication method, and HYP encapsulation efficiency was evaluated using the validated method.ResultsSeparation was achieved using an isocratic mobile phase composed of acetonitrile, methanol, and ammonium acetate buffer (10 mM, pH 5.0) (54:36:10, v/v/v) and a reverse stationary phase. The specificity, linearity, precision, accuracy, and robustness of the method were assessed and confirmed during the validation. Furthermore, the validated method was able to determine the encapsulation efficiency of HYP in NLC.ConclusionsThe HPLC method was validated, and the results indicated the ability of NLC to deliver HYP compounds for further application as a food supplement.HighlightsHYP is used as a food supplement and for photodynamic therapy (PDT). The developed method was specific, linear, precise, accurate, and robust. NLCs showed a high ability to encapsulate HYP. PubDate: Wed, 06 Sep 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad100 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1443 - 1454 Abstract: AbstractBackgroundMonitoring impurities in drug products is a principal requirement of pharmaceutical regulatory authorities all over the world to ensure drug safety. For this reason, there is a great need for analytical QC of dugs products.ObjectiveIn this study, a simple, efficient, and direct HPLC method was developed for the determination of three impurities of diclofenac.MethodsThe HPLC method was developed using a mobile phase which consisted of an HPLC grade mixture, acetonitrile–0.01M phosphoric acid adjusted to pH 2.3 (1 + 3, by volume).ResultsThe separation was performed in 15 min. The calibration curves of the three impurities were linear; the correlation coefficients were 0.999 at concentrations of 0.00015–0.003 µg/mL.ConclusionThe validation of this method shows that it meets all validation criteria. This shows the reliability of this method for the routine control of diclofenac impurities.HighlightsThe validation of a robust HPLC method for the determination of diclofenac impurities is of great importance for the pharmaceutical industry to control its products. PubDate: Thu, 06 Jul 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad078 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1455 - 1463 Abstract: AbstractBackgroundThe global financial market is still highly threatened by bovine fasciolosis, a parasitic infection that targets cattle, mainly in tropical regions. Binary combination of ivermectin (IVER) and clorsulon (CLO), in challenging concentration ratios, is typically indicated for treatment and control of fasciolosis.ObjectiveThe present study aims at smart simultaneous spectrophotometric assay of both compounds at their high ratio in marketed formulation and synthetic mixtures, without any prior separation. Furthermore, their greenness profile was evaluated and compared with previous reported assay methods, including the official one.MethodsMathematical-based proposed methods are the dual-wavelength, induced dual-wavelength, and first derivative ratio methods. Each is developed, optimized, and applied to determine simultaneously IVER and CLO at linear ranges of 1–30 and 5–40 μg/mL, respectively. They have been validated according to ICH guidelines. Statistical Student t-tests and F-tests compared the proposed methods with a USP chromatographic technique. Ecological appraisal is accomplished using three independent metrics: Analytical Eco-Scale (AES), Green Analytical Procedure Index (GAPI), and Analytical GREEnness Metric Approach (AGREE).ResultsSatisfactory recoveries, ICH compliance, and adherence of proposed methods to the ecological safety margin are achieved.ConclusionsDeveloped methods are eco-friendly and cost-effective and can accomplish a routine quantitative quality control for concurrent determination of both drugs.HighlightsVeterinary antimicrobials need analytical quality control using safer and green methodologies. Data manipulated spectral analyses of IVER and CLO, in a ratio of 1:10% (v/v), are developed and optimized. AES, GAPI, and AGREE approaches illustrate the high green compliance in respect to assays reported in the literature. Furthermore, the United States Pharmacopeia (USP) assay for IVER and CLO in injectable dosage form depends on analysis of each drug separately in the presence of the other drug, but it cannot determine both drugs simultaneously. PubDate: Wed, 30 Aug 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad098 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1464 - 1470 Abstract: AbstractBackgroundRifaximin, a medication of the rifamycin family with two distinct strengths of 200 mg and 550 mg in tablet form, is useful for the treatment of travelers’ diarrhea. It has a solid yellow hue and is very hygroscopic in nature. It exhibits a variety of polymorphic forms such as α, β, γ, δ, and ε depending on bonded moisture. These polymorphs’ varying chemical and physical characteristics, such as solubility and water content, may have a big impact on in vivo absorption, which in turn affects efficacy and safety. Therefore, understanding the polymorphic stability of rifaximin is crucial for formulating rifaximin tablets.ObjectiveThe current effort focuses on the understanding of water vapor sorption properties to control the polymorphic stability of rifaximin in the tablet formulation using the appropriate selection of excipients and manufacturing process.MethodsThe dynamic vapor sorption method in the range of 0–90% relative humidity at 25°C is used for understanding the sorption properties of drug substances and drug excipient mixtures; the state-of-the-art techniques of the X-ray diffraction method are used to identify polymorph conversions; and dissolution procedures are used for in vitro correlation studies.ResultsThe sorption study data reveals that rifaximin is highly unstable at relative humidity conditions above 36%. When using excipients that have a low tendency to adsorb water in the formulation, the polymorphic results do not show any change in their intended form, and the in vitro dissolution data show an equivalency with the reference drug product.ConclusionThe study prompted a successful outcome-oriented development of the formulation processing environment conditions design to develop a test formulation that has adequate polymorphic stability and also similarity in in-vitro dissolution profiles, with the reference product with highest similarity.HighlightsThe overall study described here is useful for swiftly gaining insight into the sorption characteristics of rifaximin, and it contributes to the widespread acceptance of rifaximin tablets as a treatment option. PubDate: Thu, 07 Sep 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad103 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1471 - 1477 Abstract: AbstractBackgroundEvogliptin tartrate is a novel dipeptidyl peptidase (DPP-4) inhibitor very recently introduced into the market as an oral hypoglycemic drug.ObjectiveThe literature review has revealed no reports of stability-indicating analytical methods so far for evogliptin tartrate. Thus, the goal of this study was to develop and validate a stability-indicating high-performance thin-layer chromatography (HPTLC) method for evogliptin tartrate in bulk and tablet dosage form.MethodFor the study, precoated plates of silica gel 60F254 were used as stationary phase and acetonitrile–water–formic acid (30:8:2, v/v/v) was used as a developing system. The densitometric scanning was performed at 270 nm, and the method was validated as per International Council for Harmonisation (ICH) guidelines for accuracy, precision, limit of detection (LOD), and limit of quantitation (LOQ). Evogliptin was subjected to forced degradation studies and was exposed to various stress conditions such as acid/base hydrolysis, oxidation, thermal stress, and UV light.ResultsThe developed method furnished compact spots of evogliptin (Rf 0.62 ± 0.05) and was linear in the concentration range of 1–5 µg/spot. The lowest detection and quantitation values were found to be 0.331 and 1.003 µg/spot, respectively, and % recovery was found to be 101.09. The low RSD values (below 2%) for intra-day (% RSD 1.86) and inter-day (% RSD 1.43) precision studies demonstrated the preciseness of the developed method.ConclusionsAll the validation parameters were found to be within the acceptable range prescribed by ICH guidelines, indicating that the developed method was accurate, precise, selective, and reproducible. A total of five degradation products were resolved under various stress conditions.HighlightsThe proposed method has a promising application commercially for identification, routine quantitative determination, and monitoring of stability of the evogliptin tartrate in bulk and tablet dosage forms to guarantee its safety, efficacy, and quality. Moreover, the developed method will also help in formulation development and in determining the appropriate storage conditions. PubDate: Wed, 02 Aug 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad091 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1478 - 1504 Abstract: AbstractBackgroundThe GlutenTox® ELISA Rapid G12 test kit is a quantitative method designed for the determination of the immunotoxic fraction of gluten in food samples.ObjectiveTo obtain AOAC Performance-Tested MethodsSM certification for the method for the detection and quantification of gluten from wheat, barley, and rye flours in select foods (non-heat-processed) and incurred (heat-processed) matrixes.MethodsThe method was evaluated following the Guidelines for Validation of Quantitative Gluten Methods, with Specific Examples for ELISA Assays. The validation study was conducted at Hygiena Diagnóstica España using five food matrixes (soy flour, corn bread, seasoning mix, rolled oats, and evaporated milk) artificially contaminated with gluten from wheat, barley, or rye flour at different concentrations: 0, 5, 10, and 20 mg/kg. For each matrix and gluten contamination level, five or six individually extracted test portions were analyzed. A second bread matrix was prepared by baking a gluten-free bread mix spiked at 0, 20, and 30 mg/kg gluten from wheat, barley, or rye flour for incurred matrix testing. Ten individually extracted test portions were tested for each incurred bread and contamination level of gluten.ResultsThe method met the AOAC performance requirements for detection and quantification of wheat gluten in the selected food matrixes, incurred bread sample, and spike levels of wheat gluten, showing an acceptable recovery. When tested with barley and rye flours, most of the results showed acceptable recoveries or a slight overestimation, depending on the matrix and gluten concentration. Method developer and independent laboratory results were comparable.ConclusionsThe validation study demonstrated that the test kit is a reliable, accurate, quick, and easy-to-use method for the detection and quantification of gluten concentration in food and incurred matrixes from wheat, barley, and rye flours.HighlightsMost reagents provided in the kit are at ready-to-use concentrations. PubDate: Mon, 17 Jul 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad081 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1505 - 1524 Abstract: AbstractBackgroundChlorate is an effective herbicide, but also a byproduct of chlorinating agents used to disinfect water, which is one of the reasons why it is regularly found in food. Perchlorate is a ubiquitous contaminant, which is naturally occurring in the environment but also released from anthropogenic sources such as the industrial use of certain natural fertilizers. Chlorate affects the hematological system, and perchlorate the thyroid.ObjectiveImplement and validate a simple and robust analytical method for the accurate determination of chlorate and perchlorate in baby food, infant and adult formulas, and ingredients thereof, which is suited for its application in routine environments where a broad variety of food commodities must be analyzed simultaneously.MethodTypically, analytes are extracted with a mixture of water, acidified methanol, and dichloromethane. Optionally, for dairy products and byproducts, extraction can be performed with water, acidified methanol, and EDTA, followed by two steps of cleanup (freezing out and dispersive solid-phase extraction with C18 in acetonitrile). Quantitative determination is carried out by isotopic dilution liquid chromatography tandem mass spectrometry (LC-MS/MS).ResultsThe method was single-laboratory validated in five Nestlé Quality Assurance Centers (NQACs) in a comprehensive range of representative matrixes of different categories such as baby foods, infant/adult formulas, and ingredients, with results generally in agreement with the acceptance criteria of the Standard Method Performance Requirement (SMPR®) 2021.001 defined by AOAC INTERNATIONAL, in terms of representative matrixes validated, LOQs, trueness, and precision.The data generated during validation show that the method proposed is simple, accurate and robust enough to be implemented and applied in routine environments.ConclusionThe data generated during validation show that the method proposed is simple, accurate and robust enough to be implemented and applied in routine environments.HighlightsThe AOAC Expert Review Panel approved the present method as AOAC Official First Action 2022.06. PubDate: Tue, 18 Jul 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad086 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1525 - 1531 Abstract: AbstractBackgroundEdible insects may contain arsenic. Analysis of arsenic species is necessary in order to accurately assess arsenic exposure.ObjectiveAn analytical method was validated and used to determine and quantitate arsenic species in edible insects.MethodsArsenic species were extracted from edible insects by heating at 100°C in 0.3 mol/L nitric acid. The concentration of arsenic species was then determined by LC–inductively coupled plasma-mass spectrometry (LC–ICP-MS) using an octadecylsilane (ODS) column with a mobile phase containing an ion-pair reagent.ResultsThe LOD (0.007–0.012 mg/kg), LOQ (0.021–0.038 mg/kg), repeatability (1.2–3.2%), intermediate precision (2.8–4.5%), and trueness (recoveries 97–102% based on spiked samples) of the proposed method were satisfactory for inorganic arsenic, dimethylarsinic acid (DMA), and arsenobetaine (AB) in edible insects. Total arsenic was detected in all samples obtained in Japan (Asian forest scorpion, diving beetles, giant water bug, grasshoppers, June beetles, mole crickets, male rhino beetle, female rhino beetle, sago worms, and silkworm pupae) and consisted of mostly inorganic arsenic. Beetles in particular showed relatively high levels.ConclusionArsenic content varies among edible insect species. Feed control is important, as arsenic concentrations in edible insects may be feed dependent.HighlightsArsenic species in edible insects were analyzed by LC–ICP-MS using an ODS column with a mobile phase containing an ion-pair reagent. Inorganic arsenic was detected in most samples, with concentrations ranging from <0.04 to 29.3 mg/kg. PubDate: Fri, 14 Jul 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad083 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1532 - 1541 Abstract: AbstractBackgroundSupercritical fluid extraction (SFE) is a fast, versatile, and solvent-efficient automatic extraction method. Despite its advantages, the results of our proficiency tests imply that the applicability assessments of SFE for pesticide residues were insufficient.ObjectiveIn this study, as analytical method using SFE was optimized and validated by testing the incurred and fortified brown rice samples with organophosphorus (OP), pyrethroid (PYR), and dithiolane (DIT) pesticides.MethodA validation study using the incurred sample with etofenprox, fenitrothion, and isoprothiolane was performed by comparing the analytical results obtained using the SFE and solid-liquid extraction with homogenization (SLE), which is a well-validated official multi-residue extraction method. The tests on the fortified samples were also performed for seven pesticide residues, chlorpyrifos, diazinon, O-ethyl O-4-nitrophenyl phenylphosphonothioate (EPN), etofenprox, fenitrothion, isoxathion, and isoprothiolane, at three fortification levels, 0.001, 0.01, and 0.1 mg/kg.ResultsIn the test on the incurred samples, optimized SFE-to-SLE analytical values (CSFE/CSLE) were 99.2–100.1%, with RSD lower than 3%. In contrast, the analytical-to-spiked concentrations in the tests on the fortified samples were 96.4–105.0%, with RSD lower than 8.8%.ConclusionsThese results indicate that the proposed SFE method, which is well validated with the incurred brown rice sample, is useful for determining OP, PYR, and DIT pesticide residues in brown rice.HighlightsThe proposed SFE method satisfies EU and Japanese maximum residue limits (MRLs). The consumption of solvent can be reduced to one-fourth of that of SLE using the proposed SFE method. PubDate: Thu, 13 Jul 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad080 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1542 - 1549 Abstract: AbstractBackgroundFruit juices are one of the most non-alcoholic beverages consumed in the world. Essential elements and other nutrients present in fruit juices play an important role in human well-being. However, fruit juices may also contain potentially toxic elements at trace levels, causing health risks.ObjectiveThe objective of this work was to develop an analytical methodology based on the preconcentration of lead using a new biodegradable hybrid material (BHM) composed of Rhodococcus erythropolis AW3 bacteria and Brassica napus hairy roots.MethodsThe BHM was implemented in an online solid-phase extraction (SPE) system for the determination of lead in fruit juices by electrothermal atomic absorption spectrometry (ETAAS).ResultsEffects of critical parameters on lead retention were studied. Under optimal experimental conditions, extraction efficiency higher than 99.9% and an enrichment factor of 62.5 were achieved. The dynamic capacity of the BHM was 36 mg/g, which favored the reuse of the column for at least eight biosorption−desorption cycles. The LOD and LOQ for preconcentration of 5 mL of sample were 5.0 and 16.5 ng/L lead, respectively. The RSD was 4.8% (at 1 µg/L lead and n = 10).ConclusionThe developed method was suitable for application to lead determination in different types of fruit juice.HighlightsA novel microextraction procedure based on the use of a biohybrid adsorbent. Highly sensitive determination of Pb at trace levels. Analysis of Pb in fruit juices samples. An eco-friendly microextraction technique for Pb determination. PubDate: Tue, 20 Jun 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad073 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1550 - 1563 Abstract: AbstractBackgroundIn response to the growing global need for pesticide residue testing, laboratories must develop versatile analytical methods and workflows to produce scientifically sound results. One of the many challenges faced by food chemists is acquiring suitable pesticide certified reference materials (CRMs) to calibrate analytical equipment, monitor method performance, and confirm the identity and concentration of hundreds of pesticide residues in food samples. CRM producers invest considerable resources to ensure the stability of their products.ObjectiveTo present proper CRM handling and storage practices as guidance to ensure stability based on the results of several multiresidue pesticide stability studies.MethodsThe open ampoule and combined multiresidue mix studies were conducted under controlled conditions. New ampoules containing multiresidue pesticide CRM mixtures were opened and compared to previously opened ampoules at multiple intervals while stored under freezing and refrigerated temperatures. Both LC- and GC-amenable pesticides (>200 residues) were combined and stored under typical laboratory conditions. Studies were performed with and without celery matrix.ResultsThe open ampoule study showed high levels of stability for all mixtures. All GC residues remained stable over the duration of the experiment. A week after opening LC multiresidue pesticide mixtures showed minor degradation. After combination of the multiresidue pesticide mixtures, degradation occurred rapidly for both the GC and LC mixtures.ConclusionMultiresidue pesticide mixtures are stable as ampullated until they are opened. Once the contents of a kit were opened and combined, decreasing stability was observed over time. This was true for both the LC and GC kits. Working mixtures of CRMs for instrument calibration should be made daily.HighlightsThis article shows a novel approach for measuring stability of CRM mixes. In-depth analysis of multiresidue pesticide mixtures and the stability that can be expected before and after mixing under typical storage conditions is described. PubDate: Wed, 13 Sep 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad096 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1564 - 1573 Abstract: AbstractObjectiveThe present investigation studies the efficacy of an automated growth-based system for a quantitative determination of Candida albicans and Aspergillus brasiliensis in several personal care products. The main purpose of this validation study was to prove that the alternative method’s entire performance is not inferior to the conventional pour-plate method for a quantitative determination of yeasts and molds. Thus, a performance equivalence was established in accordance with the United Stated Pharmacopeia (USP-NF) Validation of Alternative Microbiological Methods ˂1223˃.MethodsC. albicans and A. brasiliensis were pooled to use as inoculum (equivalent to 1.0 × 108 CFU/mL) in the suitability of the method test. PCP's preservatives were chemically neutralized leading to the yeast and mold recovery by means of the alternative microbiological method (AMM) and the pour-plate method. A correlation curve was generated for each PCP by plotting DTs relative to the corresponding log CFU values.ResultsThirty PCPs have been tested for quantification of yeasts and molds using an AMM. An equivalence of results was made through the construction of correlation curves that allowed the establishment of numerically equivalent results between the enumeration data from the reference method (CFU) and the alternative method (Detection times, DTs). Thus, following the guidelines of USP Ch.1223, essential validation parameters were tested, such as equivalence of results (Correlation coeficient, CC >0.95), linearity (R2 >0.9025), accuracy (% recovery >70%), operating range, precision (CV <35%), ruggedness (one-way ANOVA, P > 0.05), specificity, LOD, and LOQ.ConclusionIt was shown that all the test results obtained from the alternative method were in statistical agreement with the standard plate-count method (PCM). Thus, this new technology was found to meet all the validation criteria needed to be considered for an alternative method for yeast and mold quantification in the PCPs tested.HighlightsIn accordance with the United Stated Pharmacopeia (USP-NF) Validation of Alternative Microbiological Methods ˂1223˃, the implementation of alternative methods can offer benefits in execution and automation while improving accuracy, sensitivity, and precision and reduce the microbiological process time compared to the traditional ones. PubDate: Wed, 21 Jun 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad075 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1574 - 1588 Abstract: AbstractBackgroundStaphylococcus is a genus of Gram-positive bacteria, known to cause food poisoning and gastrointestinal illness in humans. Additionally, the emergence of methicillin-resistant S. aureus (MRSA) strains has caused a major health care burden worldwide. Cronobacter is a group of Gram-negative bacteria that can survive in extreme dry conditions. Cronobacter sakazakii is known to contaminate powdered infant formula and cause life-threatening infections in neonates. Vibrio is a genus of human-pathogenic Gram-negative bacteria that can cause foodborne illness by consuming undercooked or raw seafood. Vibrio parahaemolyticus can cause serious gastrointestinal disease in humans. Thus, rapid identification of Staphylococcus spp., Cronobacter spp., and Vibrio spp. is crucial for the source tracking of contaminated food, as well as to measure the transmission dynamics of these bacterial pathogens causing foodborne diseases and outbreaks.ObjectiveThis single-laboratory performance evaluation study used the VITEK MS system to evaluate the potential of MALDI-TOF MS technology for rapid identification of S. aureus-like, C. sakazakii-like, and V. parahaemolyticus-like isolates of public health importance.MethodA total of 226 isolates recovered from various food, environmental surveillance samples, and other sources were identified by bioMérieux VITEK 2 and VITEK MS systems as Staphylococcus spp., Cronobacter spp., and Vibrio spp. Five American Type Culture Collection (ATCC) reference Gram-positive and Gram-negative bacterial isolates were also tested to complete the study. In addition, for some Staphylococcus spp. isolates, whole genome sequencing (WGS) and DNA sequencing of 16S rRNA partial region were also performed for species identification.ResultsThe VITEK MS system was able to provide species identification to all 96 isolates of Staphylococcus spp. and to all 29 isolates of Vibrio spp. examined with a high confidence value (99.9%). Similarly, species identification was observed for the majority of spots (245 of 303) for the 101 Cronobacter spp. isolates (∼82.0%) with a high confidence value (99.9%), and genus level identification was noticed for the rest of the Cronobacter spp. isolates (18.0%; 58 of the 303 spots) analyzed. Species identification data generated by VITEK 2 system were comparable to data obtained by the VITEK MS system.ConclusionsThe VITEK MS system is a reliable high-throughput platform that can rapidly identify Staphylococcus, Vibrio, and Cronobacter to the genus level, as well as S. aureus, C. sakazakii, V. parahaemolyticus, and other closely related foodborne isolates and bacterial isolates from additional sources, in most cases.HighlightsThe VITEK MS system can be used in the rapid genus and species identification of human-pathogenic Staphylococcus spp., Cronobacter spp., and Vibrio spp. isolates. PubDate: Tue, 19 Sep 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad109 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1589 - 1597 Abstract: AbstractBackgroundThe KangarooSci® Aerobic Count Plate (ACP) is a sample-ready culture medium system for direct counting of aerobic bacteria colonies after 48–72 h of incubation.ObjectiveThe KangarooSci ACP was evaluated for AOAC Performance Tested MethodsSM certification.MethodsThe KangarooSci ACP was evaluated through matrix studies and product consistency/stability study and robustness testing. For the matrix study, nine food products (nonfat dry milk powder, fresh raw bovine milk, pasteurized liquid bovine milk, fresh raw ground beef, frozen uncooked chicken breast, cooked shredded pork, apple juice, ice cream, and fresh strawberries), and one environmental surface (stainless steel) were evaluated following the KangarooSci ACP product instructions and compared to the ISO 4833–1:2013, Microbiology of food and animal feeding stuffs—Horizontal methods for the enumeration of microorganisms—Part 1: Colony count at 30 °C by the pour plate technique reference standard. The product consistency and stability testing evaluated three separate production lots of the KangarooSci ACP. The robustness testing examined three test parameters, volume of sample plated, incubation time, and incubation temperature, using a factorial study design.ResultsResults from the matrix study demonstrated equivalent performance between the KangarooSci ACP and the ISO 4833–1:2013 reference standard. The product consistency and stability testing showed that the performance of the assay was equivalent over time up to 12 months and between production lots. Minor changes to the operational test conditions showed no significant impact on performance during the robustness testing.ConclusionThe KangarooSci ACP is an effective method for aerobic plate count for all matrixes evaluated.HighlightsThe KangarooSci ACP allows for fast, reliable enumeration of aerobic bacteria. Utilizing the alternative method takes up less space in incubators, requires no sample spreader, and requires fewer consumables compared to the reference method. PubDate: Mon, 31 Jul 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad088 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1598 - 1607 Abstract: AbstractBackgroundRubia cordifolia L., Rubiaceae, is globally reported to treat skin-related problems. The study aimed to assess the antityrosinase potential of Rubia cordifolia (ARC) and the development of gel formulation.MethodsThe AutoDock Vina (version V.1.2.0) program package was used for molecular docking to check for the binding affinity of ligands with protein. Response surface methodology (RSM) software was used to optimize extraction parameters for an alcoholic extract of Rubia cordifolia (ARC). The developed HPTLC method for the quantification of purpurin in ARC was validated as per the International Conference on Harmonization (ICH) guidelines. A bioautographic study for the evaluation of antityrosinase effects was performed; an anthraquinone-enriched fraction (AEF)-loaded gel formulation developed and evaluated physicochemically which could be used to reduce skin pigmentation.ResultsPurpurin showed optimum binding affinity (−7.4 kcal/mol) with the molecular target (tyrosinase) when compared to that of standard kojic acid (−5.3 kcal/mol). Quantification of purpurin in ARC, optimized by RSM software, was validated and physiologically significant results were observed for the antityrosinase potential of an AEF, along with TLC–MS-bioautographic identification for antityrosinase compounds: purpurin (m/z 256.21) and ellagic acid (m/z 302.19). Evaluation of an AEF-loaded gel formulation by in vitro and ex vivo permeation studies was performed.ConclusionARC extraction parameters optimized by RSM, and a bioautographic study helped identify antityrosinase compounds. The development of a gel formulation could be a cost-effective option for the treatment of depigmentation in the future.HighlightsA TLC–MS-Bioautography-based Identification of Antityrosinase Compounds and development of AEF-loaded Topical Gel formulation from a Bioactive Fraction of an RSM-Optimized Alcoholic Extract of Rubia Cordifolia L. stem, which could help with promising results in reducing skin pigmentation and maintaining even tone. PubDate: Thu, 20 Jul 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad076 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1608 - 1619 Abstract: AbstractBackgroundSolid phase extraction (SPE) techniques, based on computationally designed magnetic-based multi-targeting molecular imprinted polymer (MT-MIP), combined with UV spectrophotometric approaches provide advantages in the examination of counterfeit samples.ObjectiveThe current work describes an innovative and sustainable methodology for the simultaneous determination of tadalafil (TAD) and dapoxetine hydrochloride (DAP) in aphrodisiac counterfeit products (honey and instant coffee) utilizing SPE exploiting MT-MIP. Additionally, an innovative UV spectrophotometric method capable of resolving TAD in its pharmaceutical binary mixtures with DAP was developed. A novel computational approach was implemented to tailor the synthesis and design of the MT-MIP particles.MethodsWe applied a newly developed UV spectrophotometric method which was based on a Fourier self-deconvolution (FSD) method coupled with the isoabsorptive point for determination of TAD and DAP in pharmaceutical dosage form. We also applied an SPE process based on MT-MIP designed particles, assisting in the analysis of both drugs in counterfeit food samples. The SPE process and the UV spectroscopic methodology were assessed regarding their greenness using the pioneering green analytical procedure index (GAPI), analytical greeness including sample preparation (AGREEprep) and AGREE tools. The synthesized MT-MIP particles were characterized by scanning electron microscopy and energy-dispersive x-ray spectroscopy.ResultsThe suggested spectrophotometric methods revealed a wide linear concentration range of 2–50 µg/mL with lower LODs in the range of 0.604–0.994 µg/mL. Additionally, the suggested method demonstrated the utmost sensitivity and eco-friendliness for their target in its mixed dosage form and counterfeit food products.ConclusionThe SPE process and the developed analytical UV spectroscopic methodology were validated as per the ICH guidelines, and were found to be suitable for overseeing some counterfeiting activities in commercially available honey and instant coffee aphrodisiac products.HighlightsAn SPE method based on MT-MIP magnetic-based polymer and a UV spectroscopic method were successfully developed for analysis of TAD and DAP in different matrices. PubDate: Fri, 14 Jul 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad084 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1620 - 1628 Abstract: AbstractBackgroundSpectrophotometry alone is not applicable for the simultaneous determination of drugs in a multicomponent pharmaceutical formulation owing to their overlap.ObjectiveIn this study, the combination of UV-Vis spectrophotometry and chemometric methods, including continuous wavelet transform (CWT) and partial least-squares (PLS) was presented for the simultaneous estimation of tamsulosin (TAM) and solifenacin (SOL) in synthetic mixtures, commercial formulations, and a biological sample.MethodsThe simultaneous spectrophotometric determination of TAM and SOL in binary mixtures, a real sample, and a biological sample was performed by applying CWT and PLS approaches.ResultsIn the CWT method, two various wavelet families named Daubechies (db2) at wavelength 223 nm and Biorthogonal (bior1.3) at wavelength 227 nm based on the appropriate zero-crossing point were selected for TAM and SOL, respectively. The linear ranges of TAM and SOL were 0.25–4 μg/mL and 10–30 μg/mL, respectively. The LODs were 0.0459 μg/mL and 0.2085 μg/mL, while the LOQs were 0.3208 μg/mL and 0.6495 μg/mL for TAM and SOL, respectively. The average recovery values of 18 mixtures were 98.28% and 97.79% for TAM and SOL, respectively. Also, the root mean square error (RMSE) of both components was lower than 2.3. Based on the k-fold cross-validation in the PLS approach, the optimum number of components related to TAM and SOL were 9 and 5 with a mean square error prediction (MSEP) of 0.0153 and 0.0370, respectively. The mean recovery values of the test set were found to be 100.09% for TAM and 99.95% for SOL where RMSE values were 0.0064 and 0.0169 for TAM and SOL, respectively.ConclusionAnalysis of variance (ANOVA) was applied to the results of the real sample and there was no significant difference between the proposed methods and HPLC as a reference technique. The result obtained revealed that the proposed methods were found to be fast, facile, economical, and precise, and provide a suitable alternative to the HPLC technique for the concurrent determination of TAM and SOL in QC laboratories.HighlightsUV-Vis spectrophotometry combined with CWT and PLS was developed. Simultaneous analysis of TAM and SOL was performed using the proposed approaches. These methods were implemented on synthetic mixtures, commercial formulations, and a biological sample. ANOVA test was used to compare the suggested methods and the HPLC technique. PubDate: Sat, 27 May 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad065 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1629 - 1653 Abstract: AbstractBackgroundThe probability of detection (POD) model has had widespread application for statistically analyzing single and multiple collaborator validations studies with binary outcome data for a wide range of analytes over the last decade.ObjectiveThe POD model is placed on a firm theoretical foundation, and extended to a more generalized beta-binomial model.MethodsThe POD model is revisited and embedded in the beta-binomial model. This generalization includes collaborator reproducibility as a specific parameter. The new model includes only two distributional parameters: the overall across-collaborator probability of detection (LPOD) and the intraclass correlation of collaborators (ICC), measuring irreproducibility. Differences between methods are measured by the difference in LPOD values, denoted dLPOD.ResultsAccurate statistical estimators and confidence intervals are provided with validation by simulation. This new beta-binomial model will be applicable to a full range of candidate methods giving binary qualitative results, including microbiological, toxin, allergen, biothreat, and botanical analytes.ConclusionsThe new beta-binomial model provides easy equivalence tests to show the study clearly demonstrates (with 95% confidence) that the method differences and collaborator reproducibility are acceptable.HighlightsThe validation system for qualitative binary methods using probability of detection (POD) of an analyte as the parameter of interest has been modified and further validated. PubDate: Fri, 14 Jul 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad085 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1654 - 1665 Abstract: AbstractBackgroundA variety of chromatographic methods have been published for the stability evaluation of thiocolchicoside (THC) and lornoxicam (LNX). Nevertheless, the development of chromatographic methods requires the use of neurotoxic and teratogenic organic solvents that are detrimental to the environment and harmful to human life.ObjectivesUsing the principles of design of experiments (DoE), a novel white analytical chemistry-driven stability-indicating high-performance thin-layer chromatographic (SI-HPTLC) method has been developed for the concurrent stability study of THC and LNX. To protect the environment and human life, the stability-indicating HPTLC method was developed using safe organic solvents.MethodPotential analytical method risk parameters (AMRPs) and analytical method performance attributes (AMPAs) were screened using the fractional factorial design. The response surface analysis and optimization of critical AMRPs and AMPAs was carried out using full factorial design. Navigation of the method operable design region (MODR) was used to develop the SI-HPTLC technique. The developed method was validated in accordance with the International Council for Harmonization (ICH) Q2 (R1) guideline.ResultsThe developed method’s greenness was evaluated using the AGREE (Analytical Procedure Greenness) tool and ESA (Eco-Scale Assessment). The Blue (B) model was used to assess the proposed method’s cost and time efficiency and user-friendliness. For the stability studies of THC and LNX, the 12 principles of WAC (white analytical chemistry) were used to evaluate the published and proposed chromatographic techniques.ConclusionsCompared to previously published chromatographic techniques for studying the stability of THC and LNX, the suggested approach was found to be more affordable, environmentally friendly, and user-friendly.HighlightsThe development of a stability-indicating HPTLC method using a novel white analytical chemistry approach and organic solvents with low toxicity potential. Application of the developed method for analysis of the forced degraded sample and fixed-dose combinations of THC and LNX. PubDate: Tue, 18 Jul 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad082 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1666 - 1672 Abstract: AbstractBackgroundGemcitabine (GEM), a pyrimidine nucleoside, has been used as a first-line treatment in non-small-cell lung cancer (NSCLC). Sorafenib (SOR), a nonselective multi-kinase inhibitor, is used as a chemotherapeutic agent in different types of cancers including NSCLC in preclinical studies. Co-administration of GEM and SOR was found to be effective and well-tolerated in the treatment of NSCLC.ObjectiveThe aim of the present work is to determine the studied drugs in spiked human plasma simultaneously through resolving the overlapping spectra and removing the interference of the plasma matrix.MethodTwo updated chemometric models were developed using UV absorbance of the drugs, which named principal component regression (PCR) and partial least-squares (PLS) for determination of GEM and SOR in the ranges of 5–25 and 2–22 µg/mL, respectively.ResultsValidation of the two updated models has been achieved in accordance with US Food and Drug Administration (FDA) guidelines, and the results were satisfactory. The two methods had the advantages of high predictive ability of the studied drugs with high precision and accuracy. Moreover, there was no significant difference obtained when statistical comparison was done between the developed and reported methods, showing good validity of the suggested methods.ConclusionsThe two updated models have the advantages of being rapid, accurate, sensitive, and cost-effective for the determination of GEM and SOR in quality control laboratories without any need for initial separation procedures.HighlightsTwo updated chemometric methods, PCR and PLS, were developed for the estimation of GEM and SOR in spiked human plasma using their UV absorbance data. PubDate: Fri, 26 May 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad062 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1673 - 1681 Abstract: AbstractBackgroundEmtricitabine (ETC), tenofovir disoproxil fumarate (TNF), elvitegravir (EVG), and cobicistat (CBS) are antiviral drugs used to treat human immunodeficiency virus (HIV) infections.ObjectiveTo develop chemometric-aided UV spectrophotometric methods for concurrent estimation of the aforementioned drugs used to treat HIV. This method can be used to reduce modification of the calibration model by assessing the absorbance at various points in the zero-order spectra within the selected wavelength range. Additionally, it eliminates interfering signals and provides sufficient resolution in multi-component systems.MethodsTwo chemometric-assisted UV spectrophotometric methods, namely, partial least-squares (PLS) and principal component regression (PCR) models, were established for the concurrent assessment of EVG, CBS, TNF, and ETC in tablet formulations. The proposed methods were applied to decrease complexity of overlapped spectra and to achieve maximum sensitivity and the lowest error. These approaches were performed in accordance with International Council on Harmonization (ICH) criteria and compared to the reported HPLC method.ResultsThe proposed methods were used to assess EVG, CBS, TNF, and ETC in the ranges of 5–30, 5–30 , 5–50, and 5–50 µg/mL, respectively, with an excellent correlation coefficient (r2 ≥ 0.998). The accuracy and precision results were found to be within the acceptable limits. No statistical difference was observed between the proposed and reported studies.ConclusionThe chemometric-aided UV spectrophotometric approaches could be considered as alternatives to chromatographic procedures in the pharmaceutical industry for routine analysis and testing of readily accessible commercial formulations.HighlightsNovel chemometric-assisted UV spectrophotometric techniques were developed for assessment of multicomponent antiviral combinations in single-tablet formulations. The proposed methods were performed without using harmful solvents, tedious preparation, or expensive instruments. The proposed methods were compared statistically with a reported HPLC method. Assessment of EVG, CBS, TNF, and ETC was performed without interference from excipients in their multicomponent formulations. PubDate: Thu, 08 Jun 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad067 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1682 - 1688 Abstract: AbstractBackgroundThe geographic origin of Radix bupleuri is an important factor affecting its efficacy, which needs to be effectively identified.ObjectiveThe goal is to enrich and develop the intelligent recognition technology applicable to the identification of the origin of traditional Chinese medicine.MethodThis article establishes an identification method of Radix bupleuri geographic origin based on matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) and support vector machine (SVM) algorithm. The Euclidean distance method is used to measure the similarity between Radix bupleuri samples, and the quality control chart method is applied to quantitatively describe their quality fluctuation.ResultsIt is found that the samples from the same origin are relatively similar and mainly fluctuate within the control limit, but the fluctuation range is large, and it is impossible to distinguish the samples from different origins. The SVM algorithm can effectively eliminate the impact of intensity fluctuations and huge data dimensions by combining the normalization of MALDI-TOF MS data and the dimensionality reduction of principal components, and finally achieve efficient identification of the origin of Radix bupleuri, with an average recognition rate of 98.5%.ConclusionsThis newly established approach for identification of the geographic origin of Radix bupleuri has been realized, and it has the advantages of objectivity and intelligence, which can be used as a reference for other medical and food-related research.HighlightsA new intelligent recognition method of medicinal material origin based on MALDI-TOF MS and SVM has been established. PubDate: Thu, 18 May 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad060 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1689 - 1695 Abstract: AbstractBackgroundTigecycline (TIG) is a third-generation glycylcycline derivative used as an antimicrobial and anticancer agent for the past few years. Its intricate structure makes it more vulnerable toward degradation under the influence of various environmental factors and leads to the generation of impurities. Due to its stability issues, TIG is available as a lyophilized powder for injection. The analysis of TIG becomes a cumbersome task for analysts due to its instability in solution form. As TIG works as a life-saving drug, it is important to review its analytical methods for its quality control.ObjectiveThe present review discusses various analytical methodologies for determining TIG from its bulk, lyophilized powder, pharmacopoeial methods and factors responsible for its instability.MethodsThe present review represents the analysis of data reported in the literature from 1999-2022 for the analysis of TIG.ResultsNumerous alternative analytical techniques such as UV-visible spectrophotometry, spectrofluorimetric methods, RP-HPLC (reversed-phase high-performance liquid chromatography) and FT-IR (Fourier transform infrared), and electrophoresis has been reported for quantification, identification, and characterization of TIG.ConclusionsSeveral analytical techniques are available to be used as a quality control tool for tigecycline, including HPLC without derivatization, whereas the fluorescence technique requires derivatization using acidic dye. A few methods require tedious pre-sample preparation techniques, become time-consuming, and involve using one or more organic solvents; there is a need to develop eco-friendlier methods for analyzing tigecycline.HighlightsVarious analytical methods such as spectrometric, fluorimetric and chromatographic methods have been discussed for estimation of TIG from its bulk and different dosage form. PubDate: Thu, 07 Sep 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad099 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1696 - 1700 Abstract: AbstractBackgroundSome consumers with celiac disease use personal, point-of-use gluten detection devices to test food. False-positive results may occur due to sampling, matrix effects, and sensor issues.ObjectiveThe purpose of the present study was to determine if the positive gluten results some users were obtaining when testing cream cheese and materials of similar consistency were false positives and, if so, what might be causing them to occur.MethodsCream cheese, soft cheese, and yogurt were tested for gluten using the Ridascreen Gliadin R7001 sandwich R5 ELISA and the Ridascreen Gliadin R7021 competitive R5 ELISA. Two test portions were taken, extracted, and tested from each homogenized material. Materials were also analyzed for gluten using a NIMA sensor, a personal, point-of-use gluten detection device. Multiple test portion weights were tested beginning at 0.13 to 0.17 g (the ideal weight of the test portion according to the NIMA sensor development team).ResultsUsing the sandwich R5 ELISA and the competitive R5 ELISA, all materials tested below the lower LOD for gluten. Using a NIMA sensor, as the weight of the test portion tested increased, sensor results went from no gluten found, to gluten found, to no test result.ConclusionThe gluten found results using the NIMA sensor are likely false positives that appear to correspond with the weight and volume of the material tested, as well as the viscosity. There is also an apparent disconnect between the gluten found result reported by the sensor and an interpretation of the lateral flow device (LFD) strip result when assessed by eye which should also be taken into account. Ideally, NIMA sensor users should be advised on the weight amount of material to analyze and test portions should be weighed before being used with the NIMA sensor. However, this is not a practical solution when testing in many environments, including restaurants.HighlightsSlight variations in weight and volume of test materials can result in false positive results when testing dairy matrixes for gluten using the Nima sensor. PubDate: Mon, 07 Aug 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad092 Issue No:Vol. 106, No. 6 (2023)
Please help us test our new pre-print finding feature by giving the pre-print link a rating. A 5 star rating indicates the linked pre-print has the exact same content as the published article.
Pages: 1701 - 1705 Abstract: AbstractBackgroundClenbuterol (CLB) is approved as a veterinary drug because of its tracheal smooth muscle and uterine relaxant effects. However, if improperly administered for the purpose of fattening livestock, CLB can remain in the organs, which may pose a health hazard to humans.ObjectiveWe aimed to examine the combination of molecularly imprinted polymer (MIP) and solid-phase dispersive extraction (SPDE) as a pretreatment method for swine liver and kidney, which contain more coexisting impurities than muscle tissue, and attempted to construct an analytical method using liquid chromatography–tandem mass spectrometry (LC–MS/MS).MethodsSwine livers and kidneys were homogenized and extracted using liquid–liquid partitioning with an ethyl acetate–n-hexane (1 + 1) mixture, followed by SPDE using an MIP gel, and measured using LC–MS/MS. For LC–MS/MS, either an absolute calibration method or isotope dilution mass spectrometry (IDMS) was used. For method validation, a recovery test (additive concentrations: 0.05 and 0.5 ng/g) was conducted, and the data were analyzed using one-way analysis of variance (ANOVA).ResultsThe recoveries (trueness), repeatability, and intermediate precision obtained using absolute calibration were similar to those obtained using IDMS.ConclusionUsing MIP-SPDE as a pretreatment method for CLB in swine liver and kidney samples yielded comparable results for absolute calibration and IDMS in LC–MS/MS analysis.HighlightsMIP-SPDE can be used as a pretreatment method to analyze CLB in swine organs with high accuracy. PubDate: Mon, 21 Aug 2023 00:00:00 GMT DOI: 10.1093/jaoacint/qsad095 Issue No:Vol. 106, No. 6 (2023)
Hybrid journal (It can contain Open Access articles)
[1 journal]
