Journal of AOAC International最新文献

{"title":"A One-Step Green Microwell Spectrophotometric Assay for the Determination of Certain New Chemotherapeutic Drug Formulations.","authors":"Ibrahim A Darwish, Hany W Darwish, Mohammed S Alsalhi","doi":"10.1093/jaoacint/qsae052","DOIUrl":"10.1093/jaoacint/qsae052","url":null,"abstract":"<p><strong>Background: </strong>The formation of charge-transfer complexes (CTCs) of iodine with five chemotherapeutic drugs used for the treatment of different types of cancer has not been investigated. These drugs are olaparib, seliciclib, vandetanib, dasatinib, and tozasertib. Additionally, these drugs need an appropriate general spectrophotometric assay for their analysis in the dosage forms regardless of the differences in their chemical structures.</p><p><strong>Objective: </strong>The aim of this study was the development of a novel microwell spectrophotometric assay (MW-SPA) for one-step determination of these drugs via their interactions with iodine, which resulted in instantaneous production of bright lemon-yellow CTCs.</p><p><strong>Methods: </strong>A spectrophotometric study of the CTCs was conducted, and all CTCs were characterized. Site(s) of interaction on each drug were assigned, and the MW-SPA was developed and applied to the analysis of dosage forms.</p><p><strong>Results: </strong>The findings confirmed that the reactions proceeded via CTC formation. Beer's law was obeyed over a general concentration range of 1-6 µg/mL. The LODs and LOQs were in the ranges of 0.5-2.1 and 1.5-6.4 µg/mL, respectively. The proposed MW-SPA demonstrated excellent precisions as the relative standard deviations were < 2.24 and 2.23% for the intra- and inter-assay precision, respectively. Recovery studies demonstrated the accuracy of MW-SPA. Successful determination of all drugs in bulk and tablet forms was achieved using the MW-SPA. The environmental sustainability of the proposed methodology was determined, providing evidence of the assay's alignment with the basis of green analytical chemistry. The high throughput of the assay was documented.</p><p><strong>Conclusion: </strong>In contrast to other existing methods, the MW-SPA described herein was valid for analyzing all drugs at the same wavelength.</p><p><strong>Highlights: </strong>The assay is useful for routine analysis of drugs in their formulations in QC laboratories.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"903-911"},"PeriodicalIF":0.0,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141473955","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Penalization and Color Code Technical Approaches for Method Greenness and Whiteness Appraisal in Veterinary Medication: Assay of Toltrazuril Suspension.","authors":"Miranda F Kamal, Rasha M Youssef, Nehal W El-Sayed, Samir Morshedy, Haydi S Elbordiny","doi":"10.1093/jaoacint/qsae063","DOIUrl":"10.1093/jaoacint/qsae063","url":null,"abstract":"<p><strong>Background: </strong>Intestinal coccidiosis is a debilitating disease in poultry and livestock, leading to economic impact worldwide. Coccidiosis is prevented and treated in broilers by the inclusion of anticoccidials in feed. Toltrazuril is administered in potable water to treat coccidiosis.</p><p><strong>Objective: </strong>Three robust analytical methods for the quantitation of toltrazuril in pure and pharmaceutical formulations are developed. Furthermore, ecological metrics, either penalization- or color-code-based techniques, are applied for the appraisal of assays.</p><p><strong>Methods: </strong>First, second-derivative (Δλ; 5 nm) spectrophotometric method is used. Toltrazuril is measured from peak to peak at 244-260 nm within a linearity range of 5-25 μg/mL. The second method is an HPTLC analysis performed on an aluminum sheet of silica gel using ethyl acetate-methanol-ammonium chloride buffer-water (8:1:0.5:0.5, by volume respectively) as the elution phase. Toltrazuril, at a retardation factor of 0.66 ± 0.01, is linearly determined in the range of 1-9 μg/spot at 243 nm. The third method is reversed-phase HPLC with diode array detection, using an Agilent C18 column (5 μm, 4.6 × 150 mm) in isocratic elution mode at 1 mL/min flow rate with a mobile phase of acetonitrile and water in a ratio of 80:20 (v/v). Toltrazuril elutes at a retention time of 2.58 ± 0.1 min and is linearly determined at 243 nm in the range of 0.25-25 μg/mL.</p><p><strong>Results: </strong>Calculated 2D-values and peak areas are highly correlated to their corresponding drug concentrations at coefficients: r > 0.999. All methods were International Council of Harmonization (ICH) validated and applied to the dosage form with satisfactory % recoveries (97-103%). Statistical comparisons versus reported one using t-test and F-test disclose insignificant variation. In examining greenness and whiteness norms, the proposed methods were evaluated and ranked alongside four different reported methods.</p><p><strong>Conclusions: </strong>The proposed methods are green, accurate, and can be applied in routine QC for the determination of toltrazuril in pharmaceutical formulations.</p><p><strong>Highlights: </strong>Intestinal coccidiosis substantially affects the chicken intestinal tract leading to reduced growth. Toltrazuril is used for the treatment and prevention of intestinal coccidiosis. Three robust, accurate, and precise analytical methods are developed for toltrazuril determination in pure and pharmaceutical formulations. All proposed methods were ecologically assessed and compared with published ones.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"891-902"},"PeriodicalIF":0.0,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141725412","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Development of Two Green and High-Throughput Microwell Spectrometric Platforms for Determination of Reboxetine, the First FDA-Approved Selective Noradrenaline Reuptake Inhibitor Antidepressant Drug.","authors":"Ibrahim A Darwish, Mohammed S Alsalhi","doi":"10.1093/jaoacint/qsae051","DOIUrl":"10.1093/jaoacint/qsae051","url":null,"abstract":"<p><strong>Background: </strong>Reboxetine (RBX) is the first FDA-approved antidepressant drug of the selective noradrenaline reuptake inhibitors class. There is a serious need for a convenient analytical tool for the quantitation of RBX in its dosage form.</p><p><strong>Objective: </strong>This study aims toward the development and validation of two green and high-throughput microwell spectrometric platforms for the pharmaceutical analysis of RBX.</p><p><strong>Methods: </strong>The two platforms, abbreviated as MW-AB and MW-FL, involved microwell-based analysis assisted with a multifunction microplate plate reader for measuring absorbance and fluorescence signals, respectively. The MW-AB and MW-FL platforms involved the formation of colored and fluorescent derivatives upon the reaction of RBX with oxidized pyrocatechol reagent (OPC) and tetracyanoquinodimethane (TCNQ), respectively. The absorbance of colored RBX-OPC derivative at 520 nm, and the fluorescence of RBX-TCNQ charge transfer complex at 283 and 484 nm for excitation and emission, respectively. The optimum conditions of both reactions were established, their molar ratios were determined, and reaction mechanisms were postulated.</p><p><strong>Results: </strong>Both platforms were optimized and validated according to the guidelines of the International Council on Harmonization. The limits of quantitation were 19.6 µg/mL and 27 ng/mL for MW-AB and MW-FL, respectively. Both platforms were applied with excellent reliability to the quantitation of RBX content in Edranox® tablets and their drug uniformity. The greenness levels of both platforms were assessed by two comprehensive tools, and the results confirmed the high level of greenness for both platforms.</p><p><strong>Conclusions: </strong>Both platforms involved one-step reactions, adapted microwell analysis, and simultaneous handling of large number of samples. Therefore, they have the advantages of greenness and high-throughput analysis.</p><p><strong>Highlights: </strong>The proposed two platforms are valuable tools for the rapid quantitation of RBX.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"912-920"},"PeriodicalIF":0.0,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141473957","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Determination of Taurine in Infant Formula and Adult/Pediatric Nutritionals by Ultra High-Performance Liquid Chromatography with Multiple Reaction Monitoring-Mass Spectrometry: Single-Laboratory Validation, First Action 2022.08.","authors":"Geert A Ten Kate, Bertus Popma, Gerrit van der Pruik, Martin Roeleveld, Martine P van Gool","doi":"10.1093/jaoacint/qsae068","DOIUrl":"10.1093/jaoacint/qsae068","url":null,"abstract":"<p><strong>Background: </strong>Taurine (2-aminoethanesulfonic acid) is an essential β-amino acid, which is one of the most abundant intracellular amino acid component in humans. The level of free taurine in human milk is higher than in bovine milk. Since taurine is considered important for the development of a newborn, fortification of infant nutrition with taurine is common. This publication describes a rapid method for the determination of taurine in infant formula and adult/pediatric nutritionals.</p><p><strong>Objective: </strong>This publication demonstrates the suitability and applicability of the method to determine taurine content in infant formula and adult/pediatric nutritionals.</p><p><strong>Methods: </strong>Test portions are deproteinized by acid in an aqueous environment prior to analysis. The level of taurine is analyzed by hydrophilic interaction chromatography (HILIC) coupled with multiple reaction monitoring MS (MRM-MS). Quantitation is accomplished using a stable isotope-labeled internal standard (SILS) for taurine.</p><p><strong>Results: </strong>The accuracy of the method was validated using standard reference materials and spike recovery studies. The average recoveries ranged between 92% and 105%. The relative standard deviation repeatability (RSDr) and relative standard deviation intermediate precision (RSDiR) were in the range of 0.7-4.6% (RSDr) and 1.3-6.7% (RSDiR). The limit of quantitation (LOQ) was below the requirement of 0.5 mg/100 g.</p><p><strong>Conclusion: </strong>The single-laboratory validation (SLV) of the method for determination of taurine content in infant formula and adult/pediatric nutritionals demonstrates that it meets the requirements per AOAC INTERNATIONAL Standard Method Performance Requirements (SMPR) 2014.013.</p><p><strong>Highlights: </strong>A fast method to selectively determine the content of taurine in infant formula and adult/pediatric nutritionals was evaluated and found to be fit for purpose for routine product compliance testing. Based on the results of this SLV, the method was approved by the AOAC Stakeholder Program on Infant Formula and Adult Nutritionals (SPIFAN) Expert Review Panel for SPIFAN Nutrient Methods for First Action Official MethodsSM status.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"971-978"},"PeriodicalIF":0.0,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142047709","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Determination of Total Aflatoxins in Polished Rice by Liquid Chromatography-Fluorescence Detection with Multifunctional Column Cleanup and Precolumn Derivatization: Single-Laboratory and Inter-Laboratory Validation Studies.","authors":"Tomoya Yoshinari, Takahiro Watanabe, Toshihiko Takeuchi, Takahiro Ohnishi","doi":"10.1093/jaoacint/qsae066","DOIUrl":"10.1093/jaoacint/qsae066","url":null,"abstract":"<p><strong>Background: </strong>Aflatoxins (AFs) are toxic metabolites produced by Aspergillus spp. Because AFs are potent carcinogens in humans and animals, many countries have set regulatory limits for AFs in foods to prevent dietary exposure. From a global food safety perspective, in 2023, the Codex Alimentarius Commission established the maximum level (ML) of total AFs in certain cereals and cereal-based products, including polished rice. Therefore, validated analytical methods for AFs detection are necessary.</p><p><strong>Objective: </strong>In this study, an HPLC-fluorescence method coupled with multifunctional column cleanup and trifluoroacetic acid derivatization was developed for the determination of AF levels in polished rice.</p><p><strong>Methods: </strong>Our method was validated in a single-laboratory study using AF-spiked materials, followed by an inter-laboratory validation study. Twelve laboratories participated in the inter-laboratory validation study, and five polished rice test samples artificially contaminated with AFs were analyzed.</p><p><strong>Results: </strong>In a single-laboratory study, the ranges of mean recoveries of AF B1, B2, G1, G2, and total AFs were 101, 100-103, 93-96, 95-98, and 97-99%, respectively. The RSDs for within-day and between-day variations were all ≤4.4%. In the inter-laboratory validation study, the RSDs for repeatability and reproducibility were from 0.7 to 2.7% and 3.3 to 8.9% for all analytes, respectively.</p><p><strong>Conclusion: </strong>In response to the Codex ML and method performance criteria for AFs in polished rice, an analytical method based on HPLC-fluorescence detection was developed. All method performance parameters estimated from the test results of the single-laboratory and inter-laboratory validation studies met the criteria required by the Codex.</p><p><strong>Highlights: </strong>Single- and inter-laboratory studies for the validation of an analytical method for AF level determination in polished rice were successfully performed. This analytical method will be suitable to determine AF levels around the Codex ML set for polished rice.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"953-959"},"PeriodicalIF":0.0,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142057669","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Validation of a New Liquid Asymmetric-Electrode Plasma Optical Emission Spectroscopy (LAEP-OES) Method for Measurement of Total Mercury in Tuna.","authors":"Hidenori Takagi, Yoshiaki Shibuta, Michiaki Yamashita","doi":"10.1093/jaoacint/qsae053","DOIUrl":"10.1093/jaoacint/qsae053","url":null,"abstract":"<p><strong>Background: </strong>Mercury intake is caused by eating seafood, such as tuna and other predatory fish species. To reduce the health risks of mercury intake, it is necessary to continuously measure and monitor mercury concentrations at fish farms and markets. We have developed a compact system that can detect multiple heavy metals by liquid asymmetric-electrode plasma optical emission spectroscopy (LAEP-OES).</p><p><strong>Objective: </strong>The validity of the LAEP-OES method for total mercury levels was evaluated using standard solutions, certified substances, and specimens of bluefin tuna and other fish species.</p><p><strong>Methods: </strong>All specimens were dissolved in 4 M lithium hydroxide solution and then dispensed into a sample reservoir well of the single-use measurement reagent pack. Total mercury levels were automatically measured within 15 min of placement into the dedicated equipment. A total of 102 fish specimens, classified into 10 fish species, were evaluated using the new method and the results were compared to those obtained from validated analytical methods.</p><p><strong>Results: </strong>LOD (0.02 mg/kg), LOQ (0.07 mg/kg), repeatability (4.0%), intermediate precision (9.8%), and trueness (recoveries 107%) of the proposed method were within satisfactory limits for total mercury levels in fish. Additionally, when using various fish species, the method had a strong positive correlation with the results of cold-vapor atomic absorption spectrometry (CV-AAS, the official method) with Spearman rs = 0.984.</p><p><strong>Conclusion: </strong>The LAEP-OES method can be used for measuring total mercury levels in bluefin tuna. Total mercury measurement using this new method has the potential to be applied to other fish species.</p><p><strong>Highlights: </strong>Total mercury levels in fish were measured using our unique analysis system. Pacific bluefin tuna, southern bluefin tuna, and Atlantic bluefin tuna distributed in the Japanese market were analyzed for total mercury in their wild and farmed fish varieties.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"943-952"},"PeriodicalIF":0.0,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11532634/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141473959","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Headspace Gas Chromatography-Mass Spectrometry Method for Determination of Class-I Residual Solvents in Several Drug Substances: Method Evaluation by Quality by Design Statistical Tool.","authors":"Kousrali Sayyad, Leela Prasad Kowtharapu, Tanmoy Mondal","doi":"10.1093/jaoacint/qsae061","DOIUrl":"10.1093/jaoacint/qsae061","url":null,"abstract":"<p><strong>Background: </strong>Class-I residual solvents such as 1,1-dichloroethene, 1,1,1-trichloroethane, carbon tetrachloride, benzene, 1,2-dichloroethane are toxic, environmental hazards, and carcinogenic to humans. A headspace-gas chromatography-mass spectrometer is a sophisticated instrument for the quantification of residual solvents at lower limits.</p><p><strong>Objective: </strong>An exact, sensitive, reliable, and fast method was developed to determine 1,1-dichloroethene, 1,1,1-trichloroethane, carbon tetrachloride, benzene, and 1,2-dichloroethane present in different drug substances using a headspace-gas chromatography-mass spectrometer.</p><p><strong>Methods: </strong>Helium is used as a carrier gas. N-methyl-2-pyrrolidone is used as a diluent, and the stationary phase is a DB-624 (60 m × 0.25 mm × 1.4 μm film thickness) column with a flow rate of 1.5 mL/min.</p><p><strong>Results: </strong>The concentration LODs for 1,1-dichloroethene, 1,1,1-trichloroethane, carbon tetrachloride, benzene, and 1,2-dichloroethane were 0.24, 5, 0.12, 0.06, and 0.15 ppm. The concentrations LOQs for the aforementioned impurities were 0.8, 15, 0.4, 0.2, and 0.5 ppm. The linearity was assessed over the range from LOQ to 120% of the specification level.</p><p><strong>Conclusion: </strong>The current method's system suitability, precision, linearity, and accuracy parameters were assessed in accordance with the United states pharmacopeia (USP) < 1225> and International Conference on Harmonization of technical standards for the registration of medicines for human use (ICH) Q2(R2), and the results were within the acceptance criteria.</p><p><strong>Highlights: </strong>No research studies have been reported on determining class-I residual solvents in lincomycin hydrochloride, dapagliflozin, vonoprazan fumarate, and telmisartan drug substances. The proposed research aims to develop a common method for the quantification of class-I residual solvents for drug substances. The quality by design (QbD) concept is utilized in performance verification.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"921-933"},"PeriodicalIF":0.0,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141604671","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Analysis of Bovine Lactoferrin in Infant Formula and Adult Nutritional Products by Optical Biosensor Immunoassay: Collaborative Study, Final Action 2021.07.","authors":"Brendon D Gill, Harvey E Indyk, Tadashi Kobayashi, Jackie E Wood, Fiona Clow, Olan Dolezal, Lauren Hartley-Tassell, Martina Jones, William Kelton, Robyn Stoller, Lorna Wilkinson-White","doi":"10.1093/jaoacint/qsae042","DOIUrl":"10.1093/jaoacint/qsae042","url":null,"abstract":"<p><strong>Background: </strong>Bovine lactoferrin is increasingly being used as an ingredient in infant formula manufacture to enhance nutritional efficacy through the provision of growth, immunoprotective, and antimicrobial factors to the neonate.</p><p><strong>Objective: </strong>To evaluate method reproducibility of AOAC First Action Official Method 2021.07 for compliance with the performance requirements described in Standard Method Performance Requirement (SMPR®) 2020.005.</p><p><strong>Methods: </strong>Eight laboratories participated in the analysis of blind-duplicate samples of seven nutritional products. Samples were diluted in buffer, and an optical biosensor immunoassay was used in a direct-assay format to quantitate bovine lactoferrin by its interaction with an immobilized anti-lactoferrin antibody. Quantitation was accomplished by the external standard technique with interpolation from a four-parameter calibration regression.</p><p><strong>Results: </strong>After outliers were removed, precision as reproducibility was found to be within limits set in SMPR 2020.005 (≤ 9%) for six out of seven samples and all had acceptable Horwitz Ratio (HorRatR) values ranging from 1.0 to 2.1. Additionally, comparison with an alternative independent Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN) First Action method (heparin cleanup LC-UV), showed negligible difference between results.</p><p><strong>Conclusion: </strong>The method described is suitable for the quantification of intact, undenatured bovine lactoferrin in powdered infant formulas. The SPIFAN Expert Review Panel evaluated the method and accompanying validation data from this multi-laboratory testing (MLT) study in July 2023 and recommended Official Method 2021.07 for adoption as a Final Action Official MethodSM.</p><p><strong>Highlights: </strong>A multi-laboratory validation study of an automated optical biosensor immunoassay for the determination of intact, undenatured bovine lactoferrin is described.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"833-838"},"PeriodicalIF":0.0,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141077484","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A Novel Approach for Single-Step Analyte Fractionation of Raw Milk Prior to Antibiotic Residue Trace Analysis as an Alternative to QuEchERS-Based Extraction.","authors":"Jan-Michael Steils, Maren Lang, Melina Kraus, Klaus Schöne, John Cashman, Christian Baumgartner","doi":"10.1093/jaoacint/qsae022","DOIUrl":"10.1093/jaoacint/qsae022","url":null,"abstract":"<p><strong>Background: </strong>Antibiotic residues in milk are a well-known hazard in the dairy food chain. Detection methods for these residues, such as nonspecific microbiological inhibitor tests or group-specific receptor tests, are relatively inexpensive, easy to use, and widely applied to ensure food safety. In contrast, specific detection by liquid chromatography-tandem mass spectrometry (LC-MS/MS)-although a critical, complimentary method to confirm the results of nonspecific testing-is relatively costly, time-consuming, and laborious. Furthermore, sample processing before LC-MS/MS analysis requires unique preparation procedures for different groups of antibiotic compounds.</p><p><strong>Objective: </strong>To simplify and speed up specific antibiotic residue detection, a low-cost, passive, and single-step method to fractionate analytes in raw milk was developed.</p><p><strong>Methods: </strong>Untreated raw milk was fractionated into its water and fat/protein phases using a Fractionation of Milk for Trace Analysis of Contaminants and Residues for Antibiotics (FraMiTrACR® AB) fractionation unit. The water fraction was then analyzed by LC-MS/MS. The analyte fractionation method was evaluated against a Quick Easy Cheap Effective Rugged and Safe (QuEChERS)-based method for sample preparation.</p><p><strong>Results: </strong>Our method allows qualitative and quantitative detection of substances from the penicillin, cephalosporin, macrolide, lincosamide, sulfonamide, tetracycline, and fluoroquinolone groups of antibiotics. Detection limits are below the legally prescribed maximum residue levels, allowing reliable, specific, and rapid validation of a positive result in nonspecific microbiological inhibitor tests.</p><p><strong>Conclusion: </strong>Analyte fractionation by FraMiTrACR AB is a faster alternative to QuEChERS-based sample preparation for the detection of antibiotic substances in milk.</p><p><strong>Highlight: </strong>This method describes a low-cost, environmentally friendly, passive, and single-step milk analyte fractionation. As an alternative to QuEChERS-based preparation, this fractionation method simplifies and speeds up the process for specific antibiotic residue detection.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"649-662"},"PeriodicalIF":0.0,"publicationDate":"2024-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140103064","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Structural and Compositional Changes in Two Marine Shell Traditional Chinese Medicines: A Comparative Analysis Pre- and Post-Calcination.","authors":"Lizhu Wu, Chenlu Liu, Tao Yao, Yun Shi, Jinyang Shen, Xun Gao, Kunming Qin","doi":"10.1093/jaoacint/qsae023","DOIUrl":"10.1093/jaoacint/qsae023","url":null,"abstract":"<p><strong>Background: </strong>Arcae concha and Meretricis concha cyclinae concha are two marine shellfish herbs with similar composition and efficacy, which are usually calcined and used clinically.</p><p><strong>Objective: </strong>This study investigated variations in the inorganic and organic components of Arcae concha and Meretricis concha cyclinae concha from different production regions, both Arcae concha and Meretricis concha cyclinae concha. The aim was to enhance the understanding of these two types of marine shell traditional Chinese medicine (msTCM) and provide a foundation for their future development and application.</p><p><strong>Method: </strong>Spectroscopic techniques, including infrared spectroscopy, X-ray spectroscopy, and X-ray fluorescence spectroscopy, were used to analyze the calcium carbonate (CaCO3) crystal and trace elements. Thermogravimetric analysis was used to investigate the decomposition process during heating. The proteins were quantified using the BCA protein assay kit. Principal component analysis (PCA) was used to classify inorganic elements in the two marine shellfish traditional Chinese medicines.</p><p><strong>Results: </strong>No significant differences were found among the various production regions. The crystal structure of CaCO3 in the raw products was aragonite, but it transformed into calcite after calcination. The contents of Ca, Na, Sr, and other inorganic elements were highest. The protein content was significantly reduced after calcination. Therefore, these factors cannot accurately reflect the internal quality of TCM, rendering qualitative identification challenging. CaCO3 dissolution in the decoction of Arcae concha and Meretricis concha cyclinae concha increased after calcination, aligning with the clinical application of calcined shell TCM. PCA revealed the inorganic elements in them, indicating that the variation in trace element composition among different drugs leads to differences in their therapeutic focus, which should be considered during usage.</p><p><strong>Conclusions: </strong>This study clarifies the composition and structure changes of corrugated and clam shell before and after calcining, and it lays the foundation for the comprehensive utilization of marine traditional Chinese medicine.</p><p><strong>Highlights: </strong>These technical representations reveal the differences between raw materials and processed products, which will provide support for the quality control of other shellfish TCM.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"704-713"},"PeriodicalIF":0.0,"publicationDate":"2024-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140141322","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}