Journal of AOAC International最新文献

{"title":"Determination of Aloin A, Aloin B, and Aloe-Emodin in Raw Materials and Finished Products Using HPLC Multi-Laboratory Validation Study, AOAC 2016.09, Final Action Status","authors":"Isaac Lee, Quanyin Gao, Wei Liu, Darshan Patel, Malissa Smith, Hong You, Tushar Patel, Karine Aylozyan, Silva Babajanian, Teddy Collins, Darryl Sullivan, Peter Chang, Gary Swanson","doi":"10.1093/jaoacint/qsae070","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae070","url":null,"abstract":"Background A multi-laboratory validation study was performed on AOAC Official Method of Analysis (OMA) 2016.09, for final action. Eight different laboratories throughout the world participated in the study tested the same set of 6 different laboratory samples of raw materials (commercial) and formulated products (commercial), and all the laboratories successfully generated results within the acceptance criteria. Objective The intention of the study was to evaluate specificity, precision (variation), linearity/range, system suitability, limit of detection (LOD), and limit of quantitation (LOQ) by multiple laboratories to satisfy the requirement of moving the OMA 2016.09 to the final action status. Accuracy and ruggedness were already validated in earlier work of single laboratory validation (1), and it was not necessary to include these validation parameters in the multi-laboratory validation study. Method Laboratory samples containing Aloe were sent out to participating laboratories. Each lab followed AOAC 2016.09 (First Action status) to analyze contents of aloin A, aloin B, and aloe emodin using high performance liquid chromatography (HPLC) instrument. The results generated by each laboratory were collected and evaluated. Results The specificity results show that blank and matrix chromatograms do not contain major interfering peaks on the retention time of aloin A, aloin B, and aloe-emodin. The precision (variation) results of duplicated preparations are not more than 0.05 parts per million (ppm) different. The linearity/range results from six standards (10 parts per billion (ppb), 20 ppb, 40 ppb, 80 ppb, 160 ppb, and 500 ppb) have correlation coefficient (R) value of ≥ 0.999. The system suitability results meet the acceptance criteria to show the instrument validity. The limit of detection (LOD) results show that the signal-to-noise (S/N) ratio of 10 ppb standards for all three components are about 3. The limit of quantitation (LOQ) results show that the S/N ratio of 20 ppb standards for all three components are about 10. Conclusions The validation parameters (specificity, precision (variation), linearity/range, system suitability, LOD, and LOQ) have been successfully analyzed, and it shows that the test method is suitable for its intended use. Highlights The test method has been successfully validated by the eight different laboratories around the world (US, UK, Germany, and Canada). Each of the laboratory is managed independently by the site lab management team. This multi-lab study validated the method of Determination of Aloin A, Aloin B, and Aloe-Emodin in Raw Materials and Finished Products Using high performance liquid chromatography (HPLC), and the method fits for its intended purpose.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-09-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142192522","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 Toxic Elements in Botanical Dietary Supplement Ingredient Reference Materials","authors":"Jennifer Fong Sam, Adam J Kuszak, Patrick J Gray, Stephen A Wise","doi":"10.1093/jaoacint/qsae064","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae064","url":null,"abstract":"Background The National Institute of Standards and Technology (NIST) has produced over 40 botanical dietary supplement Standard Reference Materials® (SRMs) and reference materials (RMs) with values assigned for chemical markers and/or active compounds. Although environmental accumulation or inadvertent introduction of toxic elements (arsenic, cadmium, lead, and mercury) is a potential source of exposure in botanical dietary supplement products, the majority of the dietary supplement SRMs/RMs do not have values assigned for the four major toxic elements. Objective To determine As, Cd, Pb, and Hg content in the current inventory of NIST botanical dietary supplement SRMs/RMs. Methods Fifteen SRMs/RMs suites of plant part, extract, and finished products [i.e., solid oral dosage form (SODF)] were analyzed for As, Cd, Pb, and Hg using nitric acid microwave-assisted digestion followed by quantification using inductively coupled plasma—mass spectrometry. Results Results for control samples were in good agreement with certified values indicating that the analyses of 38 individual botanical SRMs/RMs were in control. Characterization of linked plant/extract SRMs/RMs derived from the same source materials demonstrated that while extraction processes can often yield extracts with lower toxic element content for Hg or As, it is also possible for mass fraction levels to remain unchanged or even increase following extraction. Conclusion The results fill significant knowledge gaps in toxic element content ranges for SRMs/RMs where no NIST assigned values existed, in particular for Hg content and for extract and SODF matrices. With comprehensive toxic element content now available, researchers can better select appropriate dietary supplement SRMs/RMs for use as controls in the analysis of dietary supplement ingredients and products. Highlights Results for As, Cd, Pb, and Hg are reported for 38 dietary supplement SRMs/RMs including 6 suites of plant, extract, and SODF and 9 pairs of plant and extract from the same batch of plant material.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-07-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141785253","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":"Evaluating the use of UV Absorbance for the Differentiation of Humified from Non-humified Materials","authors":"Mohammad Rahbari, Jarrod Psutka, Richard Lamar, Fernando Rosario-Ortiz","doi":"10.1093/jaoacint/qsae039","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae039","url":null,"abstract":"Background Products containing humic acids (HA) and fulvic acids (FA) have significant commercial potential, however, unknown to the consumer, some products may be mislabeled or contain adulterants. The prevalence of mislabelling and adulterants is primarily found in FA products. Using UV-Vis spectroscopy to differentiate between real and fake FA products is practical and desirable. Objective The objective of this study was to expand the data set generated using a UV-VIS based method proposed by Mayhew et al., 2023. Methods In total, thirty (30) test samples were used to generate ninety test portions (3 replicates per test sample) for analysis using the UV-Vis methodology outlined in Mayhew et al., 2023, which in this study is referred to as the UVAC (UV absorbance confirmation) method. Results None of the thirteen FA test samples investigated were determined as humified using the UVAC method. The FA samples studied comprised of two IHSS standards, five commercial FA products (CFAP) and six full FA fractions (SFA), which were isolated from six known solid humic material sources (SHMS). There was a leonardite, a humalite, and four peat sources used as the SHMS. Analysis of the neutralized extract of the SHMS found only 3/6 SHMS were determined as humified. Six HA (SHA) test samples were also generated by isolating the HA from the SHMS and only 3/6 SHA were determined as humified. Conclusion Given the high prevalence of false determinations more work is needed to improve the method so it can be used by industry or regulators. Highlights The proposed method failed to determine IHSS FA standards as humified. Although the method is practical, it needs improvement and further study before it can be used for reliable differentiation of real from fake FA or HA.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140831635","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 Determination of Fipronil, Permethrin and their Key Related Substances in a Topical Drug Product by a Single Stability Indicating High Performance Liquid Chromatography Method.","authors":"Renuka P Rathnasekara, Jingzhi Tian, A. M. Rustum","doi":"10.1093/jaoacint/qsae037","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae037","url":null,"abstract":"BACKGROUND\u0000The topical veterinary drug product containing fipronil and permethrin provides an effective repellent protection and high insecticidal efficacy for dogs.\u0000\u0000\u0000OBJECTIVE\u0000The objective of this study was to develop a stability indicating high performance liquid chromatography (HPLC) method for simultaneous detection and quantification of fipronil, permethrin, their key degradation products and butylated hydroxytoluene (BHT) in a topical drug product.\u0000\u0000\u0000METHOD\u0000The two active ingredients, their degradation products, and the antioxidant (BHT) were separated by a gradient elution on a Phenomenex Kinetex C18 column (150 × 3 mm, 2.6 µm particle size) maintained at 37 °C with H2O/acetonitrile/isopropyl alcohol/85% H3PO4 (65.5 + 32.5 + 4/0.0053, v/v/v/v) as mobile phase-A and acetonitrile (100%) as mobile phase-B. The flow rate was 0.9 mL/min and analytes were detected and quantified at 235 nm.\u0000\u0000\u0000RESULTS\u0000Specificity of the method was demonstrated by adequate separation of fipronil, permethrin, their degradation products, and BHT in the forced degraded finished product. Linearity of the method was demonstrated in the range of 0.2% to 150% of target analytical concentration of both active ingredients and 50% to 150% for BHT. Excellent recoveries of fipronil, permethrin and BHT in placebo spiked active ingredient solutions in the linearity range showed sufficient accuracy of the method. LOQ and LOD of the method were determined to be 0.2% and 0.07% of the analytical concentration. A robustness study did not identify any critical parameter that adversely effected the separation and quantification.\u0000\u0000\u0000CONCLUSIONS\u0000Here, we report the development and validation of a robust, stability indicating HPLC method for identification and assay of fipronil, permethrin, and BHT, including estimation of fipronil's and permethrin's degradation products in a topical drug product for dogs.\u0000\u0000\u0000HIGHLIGHTS\u0000The new HPLC method permits the acquisition of data for all analytes of interest for a topical finished drug product containing fipronil, permethrin, and BHT.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-04-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140657021","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 Two Eco-Friendly and High-Throughput Microwell Spectrophotometric Methods for Analysis of an Antibacterial Drug Tulathromycin in Pharmaceutical Bulk Form.","authors":"Ibrahim A Darwish, Nourah Z. Alzoman, M. S. Alsalhi","doi":"10.1093/jaoacint/qsae035","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae035","url":null,"abstract":"BACKGROUND\u0000Tulathromycin (TUL) is a triamilide antibacterial drug which has been approved for use in the European Union and the United States for the treatment and prevention of bovine respiratory diseases. The existing methods for determination of TUL in its pharmaceutical bulk form are very limited and suffer from major drawbacks.\u0000\u0000\u0000OBJECTIVES\u0000The aim of this study was the development of two innovative microwell spectrophotometric methods (MW-SPMs) for determination of TUL in its pharmaceutical bulk form.\u0000\u0000\u0000METHODS\u0000The formation of charge transfer complexes (CTCs) of TUL, as an electron donor, was investigated with 2,5-dihydroxy-3,6-dichlorocyclohexa-2,5-diene-1,4-dione (HCD) and 2,3-dichloro-5,6-dicyano-p-benzoquinone (CBQ), as π-electron acceptors. The CTCs were characterized by using UV-visible spectrophotometry and computational calculations. The reactions were employed for the development of two MW-SPMs with a one-step for the quantitative analysis of TUL.\u0000\u0000\u0000RESULTS\u0000The formation of CTCs was confirmed via the formation of characteristic absorption bands with maximum absorption at 520 and 460 nm for CTCs with HCD and CBQ, respectively. The stoichiometry of both CTCs was found to be 1:1, and the values of different spectroscopic and electronic constants confirmed the stability of the CTCs. The mechanisms of the reactions were postulated. The linear range of both MW-SPMs was 10-500 µg/mL. The limits of quantitation were 13.5 and 26.4 µg/mL for methods involving reactions with HCD and CBQ, respectively. Both methods were successfully applied to the quantitation of TUL in pharmaceutical bulk form with acceptable accuracy and precision. The results of eco-friendliness/greenness assessment proved that both MW-SPMs fulfill the requirements of green analytical approaches. In addition, the one-step reactions and simultaneous handling of a large number of samples with micro-volumes in the proposed methods gave them the advantage of high throughput analysis.\u0000\u0000\u0000CONCLUSIONS\u0000This study described two new MW-SPMs as valuable analytical tools for the determination of TUL.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-04-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140668138","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":"Integrated Multiplatform Analysis and Separation of Thirteen Flavonoids and Anthraquinones in Seven Medicinal Cassia Species.","authors":"A. Girme, G. Saste, Azazahemad A. Kureshi, Shubham Jagtap, Siddhi Kamble, Saurabh D Wadye, L. Hingorani","doi":"10.1093/jaoacint/qsae028","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae028","url":null,"abstract":"BACKGROUND\u0000Cassia (Family: Fabaceae) species are a large group of flowering plants rich in bioactive anthraquinone and flavonoids used in botanical supplements and nutraceuticals.\u0000\u0000\u0000OBJECTIVE\u0000A simple and reliable high-performance liquid chromatography-photodiode array (HPLC-PDA) method was developed and validated for separating and quantifying thirteen anthraquinone and flavonoids. These compounds were further confirmed using an LC-based electrospray ionization mass spectrometry (ESI-MS/MS) method in the leaves and flowers of selected Cassia species. A simple and rapid HPTLC method was developed for chemical fingerprint analysis of all Cassia species.\u0000\u0000\u0000METHOD\u0000All thirteen compounds were chromatographically separated on a Zorbax TC18 (4.6 x 250, 5 μm particle size) analytical column, and 0.1% formic acid and acetonitrile as elution solvents at a flow rate of 0.8 mL/min with detection at 259 nm. For HPTLC fingerprinting, the mobile phase compositions of toluene, ethyl acetate, and formic acid (5.5:4.2:0.6, v/v/v) were optimized to separate and identify all compounds using silica gel 60F254 aluminum plates.\u0000\u0000\u0000RESULTS\u0000The validation data for the developed HPLC-PDA method for thirteen compounds showed good linearity (r2 > 0.99) with a sensitive LOD (0.082-1.969 mg/mL), LOQ (0.250-5.967 mg/mL), and excellent recoveries (85.22-100.32%). The quantification results were found to be precise and accurate (<5.0% and relative error), -0.77-0.44 with ESI-MS/MS confirmation in the Cassia samples. The novel HPTLC method was excellent separation for thirteen compounds, with Rf values ranging between 0.12- 0.61.\u0000\u0000\u0000CONCLUSIONS\u0000The developed HPLC-PDA method was simple, and precise and could separate and quantify anthraquinones and flavonoids along with confirmation, using a novel LC-based ESI-MS/MS. The HPTLC method was found to be simple and precise, with excellent separation capabilities for these compounds.\u0000\u0000\u0000HIGHLIGHTS\u0000This novel multiplatform approach successfully identified and quantified thirteen compounds simultaneously using an integration of data strategy in seven medicinally important Cassia species' leaves and flowers.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140677725","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 Analytical Quality by Design RP-HPLC Method and Its Validation for Estimation of Gefitinib from Bulk, Tablet Dosage Form and Complex Nanoformulation.","authors":"Mahesh P. More, Sagar R. Pardeshi, Rahul Tade, P. D. Meshram, Jitendra B Naik, Prashant K. Deshmukh","doi":"10.1093/jaoacint/qsae033","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae033","url":null,"abstract":"BACKGROUND\u0000Estimation of the drug and development of the method is a critical aspect of formulation development and a critical factor for analytical scientists. Gefitinib is a poorly soluble anticancer drug.\u0000\u0000\u0000OBJECTIVE\u0000The present research enlightens the topic of the development of innovative quality by design methods for the estimation of Gefitinib (GF) from bulk, pharmaceutical tablet formulation and complex nanoformulations.\u0000\u0000\u0000METHODS\u0000To simplify the estimation of poorly soluble drugs like GF, Response Surface Methodology (RSM) was adopted with effective leverages to obtain precise computation design space using the Box-Behnken Design (BBD) model. The major 3 mixed effect independent factors (Percentage of Buffer, pH of buffer and flow rate) were screened with 3 prominent dependent responses (viz., Theoretical Plate, Retention Time, and Tailing Factor) selected for optimal analysis. Furthermore, co-processed steps were employed for the estimation of the analyte from the complex formulation.\u0000\u0000\u0000RESULTS\u0000The RP-HPLC method utilizes the quality by design (QbD) approach can effectively estimate the analyte concentration of less than 4.5 min. The developed method was economically robust, and sensitive and shows a % relative standard deviation (%RSD) of less than 2% for all the selected validation parameters. The estimated design space suggests the highest desirability (R2-0.998) at 60% of buffer in the mobile phase, pH 4.25, and flow rate of 0.7 mL/min.\u0000\u0000\u0000CONCLUSION\u0000The QbD approach was used to design and develop the method by understanding the interaction between dependent and independent variables to get the optimum values. The developed method was validated successfully and can be useful for formulation scientists to estimate drug concentration and drug release profiles from complex nanoformulations.\u0000\u0000\u0000HIGHLIGHTS\u0000The analytical approach was designed and quantified using a quality-by-design approach to make the RP-HPLC method more robust and efficient for the estimation of analytes from complex nanoformulations. The method is also useful to eliminate the interfering molecule during estimation by employing co-processing steps. The developed method saves time, and cost of solvent and employs QbD as a requirement of recent regulatory concern.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140673217","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":"Screening of 152 Veterinary Drug Residues in Animal Source Foods by LC-MS/MS, Multilaboratory Validation Study: Final Action 2020.04","authors":"Aurélien Desmarchelier, Thomas Bessaire, Marie-Claude Savoy, Adrienne Tarres, Claudia Mujahid, Andrea Beck, Pascal Mottier, Xun Fu, Wai-Chinn Chan, Stéphanie Laborie, Nadine Hagenbourgerr, Gislaine Miranda, Thierry Delatour","doi":"10.1093/jaoacint/qsae032","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae032","url":null,"abstract":"Background The presence of veterinary drug residues in food-producing animals and animal products is regulated through the enforcement of maximum residue limits (MRLs). To answer the need of the food sector to monitor these substances in a wide range of food commodities, stakeholders at AOAC identified the need for a reliable confirmatory screening method. Such qualitative approach is required for compliance checking and to support product release in manufacturing. Objective Data were collected from 5 independent laboratories that applied the AOAC Official First Action Method AOAC 2020.04 to demonstrate adequate performance under reproducibility conditions. Probability of Detection (POD) was calculated in blank test samples and test samples spiked at the Screening Target Concentration (STC) level, with the objective to achieve PODs ≤ 10% and ≥ 90%, respectively. Additionally, the effectiveness of the screening method was assessed through participation to 92 proficiency test samples. Methods Four streams were optimized to screen for 152 veterinary drug residues by LC-MS/MS in a wide variety of food commodities including milk-based ingredients and related products (e.g., milk fractions, infant formula, infant cereals and baby foods), meat- and fish-based ingredients and related products (fresh, powdered, cooked, infant cereals and baby foods) and other ingredients such as eggs, animal fat and animal byproducts. The four streams covered 105 antibiotic residues, anti-inflammatory and antiparasitic agents (Stream A); 23 Beta-lactams (Stream B); 14 Aminoglycosides (Stream C) and 10 Tetracyclines (Stream D). Results The multi-laboratory validation led to PODs at the STC ≥ 94% and PODs in the blank ≤ 9%. Further application of the multi-laboratory validated method to 92 proficiency tests provided more than 99% satisfactory submitted results (n = 784). Conclusion The inter-laboratory reproducibility determined for this method met the acceptance criteria defined in AOAC SMPR 2018.010. Highlights AOAC has approved the method for Final Action Status.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-04-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140609396","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":"Enhancing the Sustainability of Eco-friendly Potentiometric Ion Selective Electrodes for Stability-Indicating Measurement of Ethamsylate: Application in Bulk and Pharmaceutical Formulations","authors":"Hany H Monir, Heba A Mohamed, Amr M Badawy, Marianne Nebsen, Christine K Nessim","doi":"10.1093/jaoacint/qsae034","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae034","url":null,"abstract":"Background Through the use of sustainable and green chemistry concepts, scientists need to decrease waste, conserve energy, and develop safe substitutes for hazardous compounds, all for protecting and benefiting society and the environment. Objective Four novel eco-friendly ion selective electrodes (ISE) were created to determine Ethamsylate (ETM) in bulk powder and different pharmaceutical formulations. The present electrodes were fabricated and evaluated to clearly distinguish ETM from a variety of inorganic, organic ions, sugars, some common drug excipients and the degradation product, hydroquinone (HQ) of ETM, and thus could be used for stability-indicating methods. Methods The electrodes fabrication was based on 2-nitrophenyl octyl ether (NPOE) that was employed as a plasticizer in electrodes 1, 2, and 3 within a polymeric matrix of polyvinyl chloride (PVC) except for electrode 4, in which dibutyl sebacate was used as a plasticizer. Electrodes 1 &amp; 2 were fabricated using tetra dodecyl ammonium bromide as an anionic exchanger and adding 4-sulfocalix-8-arene as an ionophore only to electrode 2, but electrode 1 prepared without incorporation of an ionophore. The fabrication of electrodes 3 &amp; 4 was based on ethamsylate-tetraphenylborate (ETM-TPB) as an ion-association complex in a PVC matrix. The environmental sustainability was assessed using Green Analytical Procedure Index (GAPI), and Analytical Greenness Metric for Sample Preparation (AGREEprep). Results Electrodes 1 &amp; 2 had linear dynamic ranges of (10−1—10 −5) and (10−1—10 −4) respectively, with a Nernstian slope of 49.6 and 53.2 mV/decade, respectively. Electrodes 3 &amp; 4 had linear dynamic ranges of (10−1—10 −4), with a Nernstian slope of 43.9 and 40.2 mV/decade, respectively. Conclusion The generated electrodes' selectivity coefficients showed good selectivity for ETM. The utility 4-sulfocalix-8-arene as ionophore had a significant influence on increasing the membrane sensitivity and selectivity of electrode 2 compared to other electrodes.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-04-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140609397","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 β-Galactooligosaccharides (GOS) in Infant Formula: Collaborative Study, Final Action 2021.01","authors":"Denis Cuany, Sean Austin","doi":"10.1093/jaoacint/qsae031","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae031","url":null,"abstract":"Background We previously published a method for the determination of β-Galactooligosaccharides (GOS) in Infant Formula and Adult Nutritionals which is currently First Action AOAC Method 2021.01. In this study, reproducibility data were collected to support the promotion of the method to Final Action. Method A collaborative study was organized, to which 14 laboratories from eight different countries participated. Initially, laboratories were requested to analyze two practice samples and request guidance from the study director in case of issues. Successful laboratories proceeded to analyze seven samples (six infant formula and one adult nutritional) received as blind duplicates. Results Thirteen laboratories reported acceptable results for practice sample 1. Practice sample 2 could only be delivered to eight of the laboratories due to restrictions at customs. The 13 laboratories successfully analyzing practice sample 1 were requested to continue with the analysis of the MLT samples. Laboratory 14 was unable to solve some technical difficulties, so their data could not be used. Out of the seven samples tested, results for six infant formula met the requirements of the AOAC SMPR 2014.003, with RSDr ranging from 1.4 to 4.7% and RSDR ranging from 8.1 to 11.6%. The adult nutritional sample returned results outside the range of SPMR, having repeatability (RSDr) of 9.9%, higher than the SMPR target of ≤ 6%, and reproducibility (RSDR) of 12.1%, just above the SMPR target of ≤ 12%.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-04-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140578309","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}