Journal of AOAC International最新文献

{"title":"Identification of Radix Bupleuri From Different Geographic Origins Using Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry and Support Vector Machine Algorithm.","authors":"Zheng-Yong Zhang,&nbsp;Ya-Ju Zhao,&nbsp;Fang-Jie Guo,&nbsp;Hai-Yan Wang","doi":"10.1093/jaoacint/qsad060","DOIUrl":"10.1093/jaoacint/qsad060","url":null,"abstract":"<p><strong>Background: </strong>The geographic origin of Radix bupleuri is an important factor affecting its efficacy, which needs to be effectively identified.</p><p><strong>Objective: </strong>The goal is to enrich and develop the intelligent recognition technology applicable to the identification of the origin of traditional Chinese medicine.</p><p><strong>Method: </strong>This 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.</p><p><strong>Results: </strong>It 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%.</p><p><strong>Conclusions: </strong>This 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.</p><p><strong>Highlights: </strong>A new intelligent recognition method of medicinal material origin based on MALDI-TOF MS and SVM has been established.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9480645","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Determination of Gemcitabine and Sorafenib in Spiked Human Plasma Using Multivariate Model Update Chemometric Methods.","authors":"Marco M Z Sharkawi,&nbsp;Norhan R Mohamed,&nbsp;Mohammed T El-Saadi,&nbsp;Noha H Amin","doi":"10.1093/jaoacint/qsad062","DOIUrl":"10.1093/jaoacint/qsad062","url":null,"abstract":"<p><strong>Background: </strong>Gemcitabine (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.</p><p><strong>Objective: </strong>The 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.</p><p><strong>Method: </strong>Two 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.</p><p><strong>Results: </strong>Validation 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.</p><p><strong>Conclusions: </strong>The 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.</p><p><strong>Highlights: </strong>Two updated chemometric methods, PCR and PLS, were developed for the estimation of GEM and SOR in spiked human plasma using their UV absorbance data.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9893314","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Principles of White Analytical Chemistry and Design of Experiments to Development of Stability-Indicating Chromatographic Method for the Simultaneous Estimation of Thiocolchicoside and Lornoxicam.","authors":"Pintu Prajapati,&nbsp;Veera Shakar Pulusu,&nbsp;Shailesh Shah","doi":"10.1093/jaoacint/qsad082","DOIUrl":"10.1093/jaoacint/qsad082","url":null,"abstract":"<p><strong>Background: </strong>A 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.</p><p><strong>Objectives: </strong>Using 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.</p><p><strong>Method: </strong>Potential 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.</p><p><strong>Results: </strong>The 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.</p><p><strong>Conclusions: </strong>Compared 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.</p><p><strong>Highlights: </strong>The 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.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9827647","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Quantitative Determination of Organophosphorus, Pyrethroid, and Dithiolane Pesticide Residues in Brown Rice Using Supercritical Fluid Extraction and Liquid Chromatography-Tandem Mass Spectrometry.","authors":"Keisuke Nakamura,&nbsp;Takamitsu Otake,&nbsp;Nobuyasu Hanari","doi":"10.1093/jaoacint/qsad080","DOIUrl":"10.1093/jaoacint/qsad080","url":null,"abstract":"<p><strong>Background: </strong>Supercritical 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.</p><p><strong>Objective: </strong>In 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.</p><p><strong>Method: </strong>A 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.</p><p><strong>Results: </strong>In 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%.</p><p><strong>Conclusions: </strong>These 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.</p><p><strong>Highlights: </strong>The 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.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9829640","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Validation of the KangarooSci® Aerobic Count Plate for the Enumeration of Meosphilic Aerobic Bacteria in Selected Foods and on Stainless Steel Environmental Surfaces: AOAC Performance Tested MethodSM 062301.","authors":"Danping Wei,&nbsp;Di Wu,&nbsp;Jisheng Wang,&nbsp;Yazhou Li,&nbsp;Xinyu Sun,&nbsp;Can Zhang,&nbsp;Shuai Zhang,&nbsp;Wesley Thompson,&nbsp;M Joseph Benzinger,&nbsp;Erin Crowley","doi":"10.1093/jaoacint/qsad088","DOIUrl":"10.1093/jaoacint/qsad088","url":null,"abstract":"<p><strong>Background: </strong>The 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.</p><p><strong>Objective: </strong>The KangarooSci ACP was evaluated for AOAC Performance Tested MethodsSM certification.</p><p><strong>Methods: </strong>The 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.</p><p><strong>Results: </strong>Results 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.</p><p><strong>Conclusion: </strong>The KangarooSci ACP is an effective method for aerobic plate count for all matrixes evaluated.</p><p><strong>Highlights: </strong>The 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.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9889294","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A Review on Analytical Methods for Tigecycline Estimation From Its Bulk and Dosage Form.","authors":"Bansi Rakholiya,&nbsp;Priyangi Shah,&nbsp;Yash Patel,&nbsp;Gayatri Patel,&nbsp;Samir Patel,&nbsp;Archita Patel","doi":"10.1093/jaoacint/qsad099","DOIUrl":"10.1093/jaoacint/qsad099","url":null,"abstract":"<p><strong>Background: </strong>Tigecycline (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.</p><p><strong>Objective: </strong>The present review discusses various analytical methodologies for determining TIG from its bulk, lyophilized powder, pharmacopoeial methods and factors responsible for its instability.</p><p><strong>Methods: </strong>The present review represents the analysis of data reported in the literature from 1999-2022 for the analysis of TIG.</p><p><strong>Results: </strong>Numerous 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.</p><p><strong>Conclusions: </strong>Several 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.</p><p><strong>Highlights: </strong>Various analytical methods such as spectrometric, fluorimetric and chromatographic methods have been discussed for estimation of TIG from its bulk and different dosage form.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10180474","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Eco-Friendly UV-Spectrophotometric Methods Employing Magnetic Nano-Composite Polymer for the Extraction and Analysis of Sexual Boosters in Adulterated Food Products: Application of Computer-Aided Design.","authors":"Mohamed A Abdelshakour,&nbsp;Khaled Attala,&nbsp;Ahmed Elsonbaty,&nbsp;Randa A Abdel Salam,&nbsp;Ghada M Hadad,&nbsp;Aziza E Mostafa,&nbsp;Maya S Eissa","doi":"10.1093/jaoacint/qsad084","DOIUrl":"10.1093/jaoacint/qsad084","url":null,"abstract":"<p><strong>Background: </strong>Solid 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.</p><p><strong>Objective: </strong>The 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.</p><p><strong>Methods: </strong>We 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.</p><p><strong>Results: </strong>The 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.</p><p><strong>Conclusion: </strong>The 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.</p><p><strong>Highlights: </strong>An 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.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9779063","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Utilization of Chemometric-Aided UV Spectrophotometric Methods for Concurrent Assessment of Emtricitabine, Tenofovir Disoproxil Fumarate, Elvitegravir, and Cobicistat in Tablet Formulation.","authors":"Veena D Singh,&nbsp;Vijay K Singh,&nbsp;Sanjay J Daharwal","doi":"10.1093/jaoacint/qsad067","DOIUrl":"10.1093/jaoacint/qsad067","url":null,"abstract":"<p><strong>Background: </strong>Emtricitabine (ETC), tenofovir disoproxil fumarate (TNF), elvitegravir (EVG), and cobicistat (CBS) are antiviral drugs used to treat human immunodeficiency virus (HIV) infections.</p><p><strong>Objective: </strong>To 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.</p><p><strong>Methods: </strong>Two 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.</p><p><strong>Results: </strong>The 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.</p><p><strong>Conclusion: </strong>The 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.</p><p><strong>Highlights: </strong>Novel 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.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9586789","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Consumer-Led Investigation into Potential Issues That Arise When Testing Dairy Matrixes for Gluten With the NIMA Sensor.","authors":"Tricia Thompson, Adrian Rogers, Johnna Perry","doi":"10.1093/jaoacint/qsad092","DOIUrl":"10.1093/jaoacint/qsad092","url":null,"abstract":"<p><strong>Background: </strong>Some 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.</p><p><strong>Objective: </strong>The 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.</p><p><strong>Methods: </strong>Cream 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).</p><p><strong>Results: </strong>Using 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.</p><p><strong>Conclusion: </strong>The 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.</p><p><strong>Highlights: </strong>Slight variations in weight and volume of test materials can result in false positive results when testing dairy matrixes for gluten using the Nima sensor.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10628963/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9951103","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Validation of an HPLC Method for the Determination of Diclofenac Diethylamine and Three of Its Impurities in a Gel Pharmaceutical Form.","authors":"Mounir El Kacemi,&nbsp;Aimen El Orche,&nbsp;Omar Elhamdaoui,&nbsp;Amine Laouni,&nbsp;Mohamed Azougagh,&nbsp;Khalid Karrouchi,&nbsp;Mustapha Bouatia,&nbsp;Miloud El Karbane","doi":"10.1093/jaoacint/qsad078","DOIUrl":"10.1093/jaoacint/qsad078","url":null,"abstract":"<p><strong>Background: </strong>Monitoring 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.</p><p><strong>Objective: </strong>In this study, a simple, efficient, and direct HPLC method was developed for the determination of three impurities of diclofenac.</p><p><strong>Methods: </strong>The 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).</p><p><strong>Results: </strong>The 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.</p><p><strong>Conclusion: </strong>The 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.</p><p><strong>Highlights: </strong>The validation of a robust HPLC method for the determination of diclofenac impurities is of great importance for the pharmaceutical industry to control its products.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9756498","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}