Journal of AOAC International最新文献

{"title":"Journal of AOAC INTERNATIONAL: A History of Continued Value and Relevance.","authors":"Xu-Liang Cao","doi":"10.1093/jaoacint/qsad089","DOIUrl":"10.1093/jaoacint/qsad089","url":null,"abstract":"","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":"9889305","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":"Quantification of Chlorate and Perchlorate in a Broad Range of Food Commodities, Including Baby Food, Nutritional Formulas, and Ingredients by LC-MS/MS: First Action AOAC 2022.06.","authors":"José Fernando Huertas-Pérez,&nbsp;Pascal Mottier,&nbsp;Erik Konings,&nbsp;Quentin Baslé,&nbsp;Shi Ying Tan,&nbsp;Monika Kopeć-Durska,&nbsp;Patrycja Zawada,&nbsp;Ashley Griffin,&nbsp;María Guadalupe Sánchez-Calderón,&nbsp;Juan Pablo Silva-Robledo,&nbsp;Lisette Rubio","doi":"10.1093/jaoacint/qsad086","DOIUrl":"10.1093/jaoacint/qsad086","url":null,"abstract":"<p><strong>Background: </strong>Chlorate 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.</p><p><strong>Objective: </strong>Implement 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.</p><p><strong>Method: </strong>Typically, 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).</p><p><strong>Results: </strong>The 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.</p><p><strong>Conclusion: </strong>The data generated during validation show that the method proposed is simple, accurate and robust enough to be implemented and applied in routine environments.</p><p><strong>Highlights: </strong>The AOAC Expert Review Panel approved the present method as AOAC Official First Action 2022.06.</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":"9827648","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":"Beta-Binomial Statistical Model for Validation Studies of Analytes with a Binary Response.","authors":"Robert A LaBudde,&nbsp;Paul Wehling","doi":"10.1093/jaoacint/qsad085","DOIUrl":"10.1093/jaoacint/qsad085","url":null,"abstract":"<p><strong>Background: </strong>The 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.</p><p><strong>Objective: </strong>The POD model is placed on a firm theoretical foundation, and extended to a more generalized beta-binomial model.</p><p><strong>Methods: </strong>The 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.</p><p><strong>Results: </strong>Accurate 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.</p><p><strong>Conclusions: </strong>The 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.</p><p><strong>Highlights: </strong>The 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.</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":"9833845","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":"Green and Smart Quantitative Quality Control for Veterinary Mixture of Ivermectin and Clorsulon: Ecological Evaluation of Spectral Analyses via Analytical Eco-Scale, Green Analytical Procedure Index, and Analytical GREEnness Metric Approaches.","authors":"Miranda F Kamal,&nbsp;Rasha M Youssef,&nbsp;Samir Morshedy,&nbsp;Nehal W El Sayed","doi":"10.1093/jaoacint/qsad098","DOIUrl":"10.1093/jaoacint/qsad098","url":null,"abstract":"<p><strong>Background: </strong>The 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.</p><p><strong>Objective: </strong>The 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.</p><p><strong>Methods: </strong>Mathematical-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).</p><p><strong>Results: </strong>Satisfactory recoveries, ICH compliance, and adherence of proposed methods to the ecological safety margin are achieved.</p><p><strong>Conclusions: </strong>Developed methods are eco-friendly and cost-effective and can accomplish a routine quantitative quality control for concurrent determination of both drugs.</p><p><strong>Highlights: </strong>Veterinary 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.</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":"10121588","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":"Development of a Solid-Phase Dispersive Extraction Method for Molecularly Imprinted Polymers and LC-MS/MS for Analysis of Clenbuterol Residues in Swine Livers and Kidneys.","authors":"Koichi Saito,&nbsp;Rie Ito,&nbsp;Yoshihiro Ohsawa","doi":"10.1093/jaoacint/qsad095","DOIUrl":"10.1093/jaoacint/qsad095","url":null,"abstract":"<p><strong>Background: </strong>Clenbuterol (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.</p><p><strong>Objective: </strong>We 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).</p><p><strong>Methods: </strong>Swine 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).</p><p><strong>Results: </strong>The recoveries (trueness), repeatability, and intermediate precision obtained using absolute calibration were similar to those obtained using IDMS.</p><p><strong>Conclusion: </strong>Using 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.</p><p><strong>Highlights: </strong>MIP-SPDE can be used as a pretreatment method to analyze CLB in swine organs with high accuracy.</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":"10036634","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":"Biohybrid Adsorbent for the Preconcentration of Lead and Its Determination in Fruit Juices by Electrothermal Atomic Absorption Spectrometry.","authors":"Pamela Y Quintas,&nbsp;Elizabeth Agostini,&nbsp;Ana L Wevar Oller,&nbsp;Leticia B Escudero","doi":"10.1093/jaoacint/qsad073","DOIUrl":"10.1093/jaoacint/qsad073","url":null,"abstract":"<p><strong>Background: </strong>Fruit 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.</p><p><strong>Objective: </strong>The 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.</p><p><strong>Methods: </strong>The 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).</p><p><strong>Results: </strong>Effects 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).</p><p><strong>Conclusion: </strong>The developed method was suitable for application to lead determination in different types of fruit juice.</p><p><strong>Highlights: </strong>A 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.</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":"9664775","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 Arsenic Species in Edible Insects by LC-ICP-MS.","authors":"Eri Matsumoto,&nbsp;Makoto Matsumoto","doi":"10.1093/jaoacint/qsad083","DOIUrl":"10.1093/jaoacint/qsad083","url":null,"abstract":"<p><strong>Background: </strong>Edible insects may contain arsenic. Analysis of arsenic species is necessary in order to accurately assess arsenic exposure.</p><p><strong>Objective: </strong>An analytical method was validated and used to determine and quantitate arsenic species in edible insects.</p><p><strong>Methods: </strong>Arsenic 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.</p><p><strong>Results: </strong>The 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.</p><p><strong>Conclusion: </strong>Arsenic content varies among edible insect species. Feed control is important, as arsenic concentrations in edible insects may be feed dependent.</p><p><strong>Highlights: </strong>Arsenic 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.</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":"9779069","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 GlutenTox® ELISA Rapid G12 Test Kit for Determination of Gluten in Select Non-Heat-Processed Matrixes and Heat-Processed Matrixes: AOAC Performance Tested MethodSM 042301.","authors":"Carlos Galera, Claudia Salagre, Ana López","doi":"10.1093/jaoacint/qsad081","DOIUrl":"10.1093/jaoacint/qsad081","url":null,"abstract":"<p><strong>Background: </strong>The GlutenTox® ELISA Rapid G12 test kit is a quantitative method designed for the determination of the immunotoxic fraction of gluten in food samples.</p><p><strong>Objective: </strong>To 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.</p><p><strong>Methods: </strong>The 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.</p><p><strong>Results: </strong>The 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.</p><p><strong>Conclusions: </strong>The 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.</p><p><strong>Highlights: </strong>Most reagents provided in the kit are at ready-to-use concentrations.</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/PMC10628967/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9817218","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":"Comparative Study of Continuous Wavelet Transform and Multivariate Calibration for the Simultaneous Spectrophotometric Determination of Tamsulosin and Solifenacin in Pharmaceutical Formulation and Biological Sample.","authors":"Nazanin Ashrafi,&nbsp;Mahmoud Reza Sohrabi,&nbsp;Mandana Saber Tehrani","doi":"10.1093/jaoacint/qsad065","DOIUrl":"10.1093/jaoacint/qsad065","url":null,"abstract":"<p><strong>Background: </strong>Spectrophotometry alone is not applicable for the simultaneous determination of drugs in a multicomponent pharmaceutical formulation owing to their overlap.</p><p><strong>Objective: </strong>In 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.</p><p><strong>Methods: </strong>The 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.</p><p><strong>Results: </strong>In 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.</p><p><strong>Conclusion: </strong>Analysis 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.</p><p><strong>Highlights: </strong>UV-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.</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":"9898496","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":"Stability-Indicating Densitometric Analysis of Evogliptin Tartrate in Bulk and Tablet Dosage Form.","authors":"Shruti Srivastava,&nbsp;Suneela Dhaneshwar,&nbsp;Neha Kawathekar","doi":"10.1093/jaoacint/qsad091","DOIUrl":"10.1093/jaoacint/qsad091","url":null,"abstract":"<p><strong>Background: </strong>Evogliptin tartrate is a novel dipeptidyl peptidase (DPP-4) inhibitor very recently introduced into the market as an oral hypoglycemic drug.</p><p><strong>Objective: </strong>The 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.</p><p><strong>Method: </strong>For 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.</p><p><strong>Results: </strong>The 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.</p><p><strong>Conclusions: </strong>All 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.</p><p><strong>Highlights: </strong>The 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.</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":"9981222","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}