Journal of AOAC International最新文献

{"title":"Understanding the Stress Testing Characteristics of Apixaban, Structural Elucidation of a Novel Degradation Impurity, and Stability-Indicating Method Development for Quantification of Related Substances.","authors":"Srikanth Reddy Surukonti, M S Surendrababu","doi":"10.1093/jaoacint/qsad106","DOIUrl":"10.1093/jaoacint/qsad106","url":null,"abstract":"<p><strong>Background: </strong>People who have non-valvular atrial fibrillation may benefit from taking a new oral anticoagulant called apixaban, which has recently been given the green light by the U.S. Food and Drug Administration. During stress testing, apixaban was found to have a high degree of degradability when subjected to both acidic and basic conditions, and one significant unknown impurity was observed in addition to the major known impurities.</p><p><strong>Objective: </strong>Our aim is the isolation and characterization of degradation product observed in stress/forced degradation studies, and also the development of a single HPLC method that is both reliable and accurate for quantifying all 10 related impurities of apixaban.</p><p><strong>Methods: </strong>Preparative HPLC was used to isolate the degradation product, and 1H NMR, 13C NMR, and MS were used to elucidate the structure of the product. Additionally, a single reverse-phase (RP) HPLC method was developed for quantification of all related impurities of apixaban.</p><p><strong>Results: </strong>Based on the spectral characterization data, the identified unknown degradation impurity was found to be a pH-independent hydrolysis degradation impurity of apixaban. The developed method is specific, linear, accurate, robust, and rugged.</p><p><strong>Conclusion: </strong>The isolated and characterized impurities were the same as those found during stress testing. The developed method has been validated for its intended purpose in accordance with the regulatory requirements that were outlined.</p><p><strong>Highlights: </strong>The unknown impurity is a new apixaban degradation impurity that helps us understand its toxicity. The scientific community will benefit from the developed analytical method information as it relates to understanding drug product impurity profiling.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10224104","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 Green-and-White Integrative Analytical Strategy Combining Univariate and Chemometric Techniques for Quantifying Recently Approved Multi-Drug Eye Solution and Potentially Cancer-Causing Impurities: Application to the Aqueous Humor.","authors":"Khalid A M Attia, Ahmed El-Olemy, Sherif M Eid, Ahmed Emad F Abbas","doi":"10.1093/jaoacint/qsad087","DOIUrl":"10.1093/jaoacint/qsad087","url":null,"abstract":"<p><strong>Background: </strong>Drug impurities are now seen as a major threat to the production of pharmaceuticals around the world and a major part of the global contamination problem, especially when it comes to carcinogenic impurities.</p><p><strong>Objective: </strong>We present the first spectrophotometric strategy based on a combination of univariate and multivariate methods as impurity profiling methods for the estimation of lignocaine (LIG) and fluorescein (FLS) with their carcinogenic impurities: 2,6-xylidine (XYL) and benzene-1,3-diol (BZD).</p><p><strong>Method: </strong>The data processing strategy depends on overcoming unresolved bands by employing five affordable, accurate, selective, and sensitive methods. The methods applied were a direct UV univariate spectrophotometric analysis (D0) and four multivariate chemometric methods, including classical least squares (CLS), principal component regression (PCR), partial least squares (PLS), and genetic algorithm (GA-PLS). FLS analysis (1-16 μg/mL) was performed using the D0 method at 478 nm; then, the application of the ratio subtraction method (RSM) allowed the removal of interference caused by the FLS spectrum. From the resulting ratio spectra, LIG, XYL, and BZD can be efficiently determined by chemometrics. The calibration set was carefully selected at five concentration levels using a partial factorial training design, resulting in 25 mixtures with central levels of 160, 40, and 3 μg/mL for LIG, XYL, and BZD, respectively. Another 13 samples were applied to validate the predictive ability.</p><p><strong>Results: </strong>The statistical parameters demonstrated exceptional recoveries and smaller prediction errors, confirming the experimental model's predictive power.</p><p><strong>Conclusions: </strong>The proposed approach was effectively tested using newly FDA-approved LIG and FLS pharmaceutical preparation and aqueous humor. Additionally, it was effectively assessed for whiteness, greenness, and sustainability using five assessment tools.</p><p><strong>Highlights: </strong>With its remarkable analytical performance, sustainability, affordability, simplicity, and cost-efficiency, the proposed strategy is an indispensable tool for quality control and in situ analysis in little-equipped laboratories, increasing the proposed approach's surveillance ability.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10252581","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":"Fluoride Determination in Milk, Soy, and Water-Based Products Using Ion-Selective Electrode and Direct Measurement Technique: Single-Laboratory Validation, First Action 2022.05.","authors":"Renée M Erney, Charles K Black","doi":"10.1093/jaoacint/qsad104","DOIUrl":"10.1093/jaoacint/qsad104","url":null,"abstract":"<p><strong>Background: </strong>The AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals issued a call for methods for the determination of fluoride in infant formula. Standard Method Performance Requirement (SMPR®) 2014.016 was approved.</p><p><strong>Objective: </strong>A single-laboratory validation (SLV) of a fluoride ion-selective electrode (F-ISE) method was completed.</p><p><strong>Methods: </strong>Five powder samples were reconstituted, and hydrochloric acid was added to dissolve and release any bound fluoride. Samples included infant and adult nutritional products made from milk, whey, or soy, containing intact, partially hydrolyzed, or hydrolyzed proteins. Sodium citrate buffer was added to complex any interfering ions and adjust pH and ionic strength. Samples were analyzed in duplicate over 6 days using F-ISE.</p><p><strong>Results: </strong>Results were calculated based on one of two least-squares (log fit) standard curves (0.02 to 0.1 µg/100 g or 0.1 to 2.0 µg/100 g). The LOQ for the method was determined to be 3.3 µg/100 g, which was far below the minimum analytical value of 30 µg/100 g required in the SMPR. The fluoride concentrations ranged from approximately 3 to 14 µg/100 g reconstituted powder and the intermediate precision, RSDr, ranged from 0.7 to 12.4%. Although all of these results are out of scope for the SMPR due to their low fluoride, it should be noted that the RSDr for formulas with fluoride concentrations ranging from approximately 9 to 14 µg/100 g ranged from 0.7 to 4.3%, and the RSDr for the two formulas with fluoride concentrations at or below the theoretical detection limit of the method were only approximately10 and 12.4%. Recoveries ranged from 94 to 98% for samples spiked at three levels with NIST-traceable standard solutions, meeting the SMPR.</p><p><strong>Conclusion: </strong>The F-ISE method meets the SMPR and was adopted as a First Action Official MethodSM.</p><p><strong>Highlights: </strong>The fluoride ion-selective electrode method presented here is affordable and easy to run. The addition of acid to the samples dissolves any minerals which may bind the fluoride.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10277601","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":"Simultaneous Uplc Assay for Oxitropium Bromide and Formoterol Fumarate Dihydrate in Pressurised Metered Dose Inhaler Products for Chronic Obstructive Pulmonary Disease","authors":"Serdar Seckin, Serap Saglik Aslan","doi":"10.1093/jaoacint/qsad134","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad134","url":null,"abstract":"Backround Oxitropium Bromide (OB) and Formoterol Fumarate Dihydrate (FFD) are inhaler molecules that are widely used in the treatment of chronic lung diseases. Objective The goal of this work was to create a reversed phase-ultra performance liquid chromatography (RP-UPLC) technique for assay and identification of OB and FFD, as well as identification and estimate of its associated compounds in pressurised metered dose inhaler product (pMDI). Method Separation of oxitropium and formoterol peaks were enhanced on C18 (50 x 2.1 mm x 1.7 μm), UPLC column with Ethylene-Bridged-Hybrid technology, The mobile phase consists of buffer (0.07 M KH2PO4) and acetonitrile (80:20 v/v). The detector wavelength of 210 nm, flow rate of pump 0.6 mL/min and oven temperature for column were set at 25◦C. The injection volume was 10 μL. The method run time is 2 min. The mobile phase was used as the solvent. Results Retention times were 0.5 min. for OB and 1.0 min. for FFD. The assay analysis was lineear range for all analytes within the range for concentrations 0.03—14.8 µg/mL of OB, 0.01– 0.88 µg/mL of FFD. LOD values and LOQ values 0.009 µg/mL and 0.026 µg/mL for OB, 0.003 µg/mL and 0.009 µg/mL for FFD, respectively. Recoveries were obtained at 96.3% for OB and 97.2% for FFD. Precisions values were (as RSD%) ≤1.5%. Conclusions With the UPLC method developed and validated according to the current ICH guidelines, it is possible to simultaneously detect OB and FFD of assay analysis in pMDI products accurately, precisely and selectively, independent of the matrix effect. Highlights The present method is the first method in the literature based on the UPLC method for this purpose. The UPLC method is a time-saving method, it provides a faster and cheaper technique than the HPLC method.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-12-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138742620","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":"Greenness assessment and validation of HPLC method for simultaneous determination of Resveratrol and Vitamin E in dietary supplements","authors":"Marina Topkoska, Martina Miloshevska, Marjan Piponski, Irena Slaveska Spirevska, Natalija Nakov, Katerina Brezovska, Jelena Acevska","doi":"10.1093/jaoacint/qsad131","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad131","url":null,"abstract":"Background There is an increasing interest in the use of a combination of trans-resveratrol and vitamin E in dietary supplements. Determination of the content of both components is essential for confirmation of the quality of the product. Objective To establish the applicability and ensure the greenness of the previously developed high-throughput HPLC/UV method for the simultaneous determination of trans-resveratrol and alpha-tocopherol acetate (vitamin E) in dietary supplements. Methods Separation was performed on RP C8 Select B chromatographic column, using acetonitrile and water in the mobile phase, with gradient elution. Full method validation was performed in accordance with ICH Q2(R1). The greenness of the method was assessed using the analytical eco-scale (AES) methodology and the analytical greenness metric (AGREE). Results The method is selective, linear, precise and accurate over defined concentration ranges (185—369 µg/mL of trans-resveratrol and 37—75 µg/mL of alpha-tocopherol acetate), and has a suitable sensitivity (limits of detection and quantification are 7.7 µg/mL and 23.3 µg/mL for resveratrol and 2.6 µg/mL and 7.8 µg/mL for tocopherol acetate, respectively). The obtained analytical eco-scale score of 77 and the pale green AGREE pictogram with an overall score of 0.61 confirm the method’s greenness. Conclusion The sensitivity and selectivity of the method, its short analysis time (7 minutes), the low negative environmental impact, and simple sample preparation make the method readily applicable to in-line quality control procedures. Highlights A method for simultaneously analysing vitamin E and resveratrol in dietary supplements is presented. The method is rapid, includes a simple sample preparation procedure, and has a low environmental impact.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-12-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138692628","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 FSTestTM Aerobic Count Plates Method for Enumeration of Aerobic Bacteria in a Variety of Matrixes and Stainless Steel Environmental Surface: AOAC Performance Tested MethodSM 112301","authors":"Yun Liu, Jun Fan, Xia Sun, Zican Zhou","doi":"10.1093/jaoacint/qsad132","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad132","url":null,"abstract":"Background The FSTestTM Aerobic Count (AC) Plates are ready-to-use culture mediums containing nutrients, a cold-water-soluble gelling agent and a chromogenic indicator. Objective The objective of this study was to validate the FSTest AC plate method for the AOAC Performance Tested MethodsSM (PTM) certification for a variety of foods and stainless steel. Methods The performance of the FSTest AC plates were compared to the appropriate reference method, for the detection of total aerobic bacterial in a variety of foods matrixes (raw ground beef, raw ground pork, cooked ham, raw chicken breast, raw shrimp, frozen tuna, shredded bagged lettuce, cherry tomato, pasteurized liquid milk, nonfat milk powder) and stainless steel surface. The robustness, consistency, and stability studies of the FSTest AC plate were also conducted. Results The results of the matrix study showed the standard deviation of repeatability (sr) was similar in both the FSTest AC plate method and the reference method. The 90% confidence interval of the difference between means between the two methods was found to fall within -0.5 to 0.5 log10 for all matrixes at all levels in the method developer and independent laboratory studies. The data in the report also supports that the FSTest AC plate method is robust, manufactured in a consistent manner and can be stable for 18 months at 4–10 °C. Conclusion The FSTest AC method is validated to be equivalent to the appropriate reference methods for the enumeration of aerobic bacteria in a variety of food matrixes and stainless steel surface at 36 ± 1 °C, and 32 ± 1 °C (for dairy matrixes) in 24 ± 1 h. Highlights The FSTest AC plate method offers the advantage of saving labor, space and time, as results are available within 24 h for all tested matrixes.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-12-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138560721","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":"Quality evaluation of gentamicin sulfate reference standards in Japanese Pharmacopoeia using hydrophilic interaction chromatography combined with tandem mass spectrometry","authors":"Keiko Maekawa, Ryuichi Sawa, Mari Matsui, Toshifumi Konda, Yumiko Kubota, Ayaka Matsuo, Akiho Maeda, Chisato Takahashi, Tsuyoshi Tanimoto, Yukari Nakagawa, Sachiyo Yoneda, Yuri Mori, Satowa Suzuki","doi":"10.1093/jaoacint/qsad135","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad135","url":null,"abstract":"Background Through the recent development of analytical technology, antibiotics quantification in the Japanese Pharmacopoeia (JP) has changed from traditional microbiological assays to physicochemical methods with high specificity and precision. However, for several multicomponent antibiotics without typical UV absorption, potency cannot be directly determined using instrumental methods such as high-performance liquid chromatography; therefore, traditional microbiological assays are still used. Gentamicin sulfate (GmS), which consists of three major components, C1, C1a, and C2, is such a typical antibiotic, and its antimicrobial potency continues to be assayed using microbiological methods in JP monographs. Introduction of physicochemical assay for GmS is needed to help ensure its quality and quantity. Objective This study aimed to develop quality control measures for GmS that could be complimentary to quantitative assays and purity tests specified in the JP. Methods For each gentamicin C component (C1, C2, and C1a), theoretical potencies were determined based on the quantitative relationship between purity and potency, as measured by quantitative 1H NMR and microbiological assays, respectively. Two lots of the JP reference standard (RS) were used as test samples, with the contents of each component and impurity (sisomicin and garamine) being determined using hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS). Results The ratios of theoretical potency for C1, C2, and C1a were 1.00, 1.21, and 1.80, respectively. The potencies of the GmS JP RSs, which were estimated based on the contents and theoretical potency of each C component, corresponded well with those determined through microbiological assays. Marked differences in impurities (%) between the two RS lots were highlighted by quantifying sisomicin and garamine. Conclusion The developed analytical procedure enabled the characterization of two different JP RSs in terms of content ratio, potencies, and impurities. Highlights Novel analytical procedures useful for routine quality control of GmS were developed using HILIC-MS/MS.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-12-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138560983","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":"Exciting Advances in Sustainable Spectrophotometric Micro-Quantitation of an Innovative Painkiller “Tramadol and Celecoxib” Mixture in the Presence of Toxic Impurity, Promoting Greenness and Whiteness Studies","authors":"Eman A Bahgat, Hisham Hashem, Hanaa Saleh, Ebraam B Kamel, Maya S Eissa","doi":"10.1093/jaoacint/qsad133","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad133","url":null,"abstract":"Background Tramadol (TRM) and celecoxib (CLX) are a novel mixture that helps relieve impetuous, acute pain when other painkillers have no action. It is also reported that the currently studied drugs, tramadol and celecoxib, are used to control COVID-19 symptoms. Objective The current work highlights three important pillars of modern pharmaceutical analysis, which are as follows; impurity profiling, greenness/whiteness studies and simplicity accompanied by sensitivity. Since 4-methyl acetophenone inhibits the human carbonyl reductase enzyme (type I), and since this compound may pose a health risk, it is crucial to regulate its concentration in all dosage forms of CLX. Methods Two simple and green spectrophotometric methods were developed, namely; Third Derivative (D3) and Fourier Self Deconvulation (FSD) for resolving severely overlapped spectra of tramadol and celecoxib in the presence of 4-methyl acetophenone (4-MAP) as a process-related impurity in their novel tablet combination. Results The two approaches showed acceptable linearity with an excellent correlation coefficient. Simply, for both methods tramadol was measured when celecoxib and 4-methyl acetophenone were zero-crossing. The same procedure was applied for measuring celecoxib and its process-related impurity; 4-methyl acetophenone. Conclusion The methodologies developed were thoroughly validated in compliance with ICH guidelines. Student t and F-tests revealed no statistically substantial variation among the current methods and the reported method. Highlights No spectrophotometric methods have been published for the simultaneous analysis of TRM and CLX along with 4-MAP. As a result, the newly developed spectrophotometric approaches hold great relevance and originality in the field of pharmaceutical analysis.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-12-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138560474","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":"Simultaneous quantification of Two Neonicotinoids using QuERChERS-LC-MS/MS in Moroccan Spearmint (Mentha Spicata.L): Qualimetry of the method by Uncertainty estimation using Generalized Pivotal Quantities approach and Monte Carlo simulation","authors":"Hicham Aaziz, Taoufiq Saffaj, Yassine Hameda Benchekroun, Bouchaib Ihssane","doi":"10.1093/jaoacint/qsad136","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad136","url":null,"abstract":"Background Neonicotinoids are used for the phystosanitary treatment of Mentha Spicata.L crops, and this practice requires precise control of these harmful substances at very low concentrations. Objective The objective of this study is to apply an approach allowing simultaneously validation and evaluation of measurement uncertainty based on total error methodology, in order to accurately quantify the presence of two neonicotinoids in Mentha Spicata.L utilizing a QuEChERS-LC-MS/MS methodology. Methods Assay of Imidacloprid and Acetamiprid using QuEChERS extraction method coupled with LC-MS/MS to guarantee the analytical method's accuracy and control the risk of its routine use. A complete and exhaustive validation approach based on the “β-content, γ-confidence” tolerance interval was used for the uncertainty assessment, using the Generalised Pivot Quantity (GPQ) concept and Monte Carlo simulation, which avoids the need for additional data while achieving intermediate precision for each concentration level within predetermined acceptable limits. Results The validation procedure is based on the choice of a quadratic model for the two neonicotinoids, allowing the validation of Acetamiprid and Imidacloprid by LC-MS/MS assay within the range of working concentration. The flexibility of the Uncertainty Profile intervals was demonstrated with a variation in β-content values (66.7%, 80%, and 90%) and risk values (10% and 5%), which remained within the acceptability limits of 20%, and the relative expanded uncertainty did not exceed 15% and 11%. Conclusion QuEChERS- LC-MS/MS method for the analysis of two neonicotinoids has successfully been fully validated using the Uncertainty Profile strategy. Highlights Application of a full validation strategy based on the validation and uncertainty assessment for the quantification of two main Neonicotinoids in Mentha Spicata.L using QuEChERS- LC-MS/MS. This qualimetric has been conducted by computing of the measurement uncertainty of the method utilizing data from analytical validation under conditions of intermediate precision at each level of concentration without additional effort, after that we have demonstrate the flexibility of this strategy for the LC-MS/MS quantification of acetamiprid and imidacloprid, using a decision tool that enables the choice and modification of β-content and γ-confidence values.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-12-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138560567","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 Study and Handling Recommendations for Multiresidue Pesticide Mixes under Diverse Storage Conditions for LC-MS/MS and GC-MS/MS.","authors":"Landon A Wiest, Jana R Hepner, Jason E Fisher, Karen M Risha, John H Lidgett, Valerie N Ballarotto, Joseph D Konschnik","doi":"10.1093/jaoacint/qsad096","DOIUrl":"10.1093/jaoacint/qsad096","url":null,"abstract":"<p><strong>Background: </strong>In 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.</p><p><strong>Objective: </strong>To present proper CRM handling and storage practices as guidance to ensure stability based on the results of several multiresidue pesticide stability studies.</p><p><strong>Methods: </strong>The 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.</p><p><strong>Results: </strong>The 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.</p><p><strong>Conclusion: </strong>Multiresidue 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.</p><p><strong>Highlights: </strong>This 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.</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/PMC10628962/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10221643","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}