Journal of AOAC International最新文献

{"title":"Electrochemical Approach on a Flavonoid: Miquelianin via Carbon Based Electrodes and Its Analysis from Calystegia Silvatica.","authors":"Nurgul K Bakirhan, Sıla Ozlem Sener, Merve Yuzbasioglu Baran, Khadija Bahend, Ufuk Ozgen","doi":"10.1093/jaoacint/qsaf032","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf032","url":null,"abstract":"<p><strong>Background: </strong>Miquelianin (MIQ) is a natural phenolic compound found in various plants, including Salvia species, with potential health benefits due to its antioxidant and anti-inflammatory properties.</p><p><strong>Objective: </strong>This study presents the investigation of electrochemical oxidation pathway and sensitive analysis of MIQ which is isolated from the aerial parts of Calystegia silvatica that grows in Trabzon, Türkiye.</p><p><strong>Methods: </strong>Electrochemical determination methods have gained significant attention for the quantitative analysis of bioactive compounds due to their simplicity, sensitivity, and cost-effectiveness. The electrochemical determination of MIQ primarily involves the utilization of electrochemical techniques such as cyclic voltammetry and differential pulse voltammetry.</p><p><strong>Results: </strong>Under optimum experimental conditions, calibration plot for MIQ with a limit of detection of 99.3 × 10-9 M and 145 × 10-9 M were obtained using differential pulse voltammetry for GCE and BDDE in the range of 2.0 × 10-6 to 3.6 × 10-5 M. The presented method was validated and successfully performed for the determination of the MIQ from plant extracts with excellent recovery values as 104.7, 101.8, and 102.1%.</p><p><strong>Conclusion: </strong>This study explores the electrochemical oxidation pathway and sensitive analysis of MIQ, isolated from Calystegia silvatica in Trabzon, Türkiye. GCE and BDDE as carbon-based electrodes have been used for the sensitive analysis of MIQ in PB solution at pH 7.0 solution. MIQ was detected by GCE and BDDE with limits of 99.3 × 10-9 M and 145 × 10-9 M, respectively, within a concentration range of 2.0 × 10-6 to 3.6 × 10-5 M. The validated method demonstrated excellent recovery values of 104.7, 101.8, and 102.1% for determining MIQ from plant extracts.</p><p><strong>Highlights: </strong>This electrochemical developed method offers promising opportunities for accurate and sensitive analysis of miquelianin. Continued research and technological advancements in this field can contribute to a deeper understanding of the electrochemical behavior of miquelianin and facilitate its practical applications in pharmaceutical, food, and nutraceutical industries, promoting its utilization as a valuable bioactive compound.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-04-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143805209","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":"Method Development for Determining β-Nicotinamide Mononucleotide (NMN) in Cosmetics Using m-PFC-HPLC.","authors":"Tao Lan, Wenyu Zhang, Hongtao Chu, Zhenyu Yun, Bin Qu","doi":"10.1093/jaoacint/qsaf017","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf017","url":null,"abstract":"<p><strong>Background: </strong>As a new cosmetic ingredient, NMN is widely used in cosmetics production, but due to the lack of detection method, quality control of related products cannot be achieved.</p><p><strong>Objective: </strong>This study will develop a detection method for NMN in three matrices (facial mask essence, emulsion and cream) for quality control of related cosmetics.</p><p><strong>Methods: </strong>Given the high ester content in facial emulsions and creams, which can hinder the detection of trace substances, a novel multiplug filtration clean-up (m-PFC) purification column packed with multi-walled carbon nanotubes (MWCNTs) was employed to purify these matrices. An HPLC method for NMN in three matrices (facial mask essence, emulsion, and cream) was established. Methodological verification was conducted.</p><p><strong>Results: </strong>Results demonstrated a good linear relationship within the range of 5.0-500 μg/mL, with a limit of quantification (LOQ) of 5.0 mg/kg. The precision experiment's relative standard deviation (RSD) was less than 3%, and the RSD for six repeated experiments ranged from 1.2% to 5.3%, indicating the method's stability, reliability, and good repeatability. Recovery rates in the three cosmetic matrices were between 93.9% and 109.4%, with an RSD below 3.7%. This method was applied to detect NMN content in seven cosmetics purchased from an e-commerce platform, some products claiming to contain NMN did not detect NMN.</p><p><strong>Conclusion: </strong>This method had the advantages of simple operation, high sensitivity, and good accuracy, provides technical support for cosmetic regulation.</p><p><strong>Highlights: </strong>Through this study, we should raise awareness and supervision of NMN cosmetics by establishing relevant standards.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-04-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143805210","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":"Quality Analysis of Peanut Oils and Peanut Diacylglycerol Edible Oils after Frying Using Raman Spectroscopy Combined with Oil Microscopy.","authors":"Lingli Liu, Rui Liu, Zhenshi Chen, Yuanpeng Li, Mengjiao Xue, Meiyuan Chen, Wenchang Huang, Hanglin Lu, Jian Tang, Shan Tu, Jun Liu, Junhui Hu","doi":"10.1093/jaoacint/qsaf002","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf002","url":null,"abstract":"<p><strong>Background: </strong>The thermal stability and quality of fats change during oil-frying, directly impacting food safety and nutritional value; however, traditional analysis methods are time-consuming and complex.</p><p><strong>Objective: </strong>This study aimed to develop a rapid monitoring protocol using a portable Raman spectrometer for peanut oils and peanut diacylglycerol (DAG) edible oils after frying one to five times at 150 °C.</p><p><strong>Methods: </strong>Raman spectral data and the acid and peroxide values were determined for 48 oil test samples. Raman spectral data were analyzed using the characteristic-band-intensity-ratio method and oil microscopy.</p><p><strong>Results: </strong>The peroxide values of peanut oil correlated with I729/I1076, I1076/I1300, and I1268/I1655, whereas the acid and peroxide values of peanut DAG edible oil correlated with I863/I1655, I1076/I1300, and I1268/I1655. Oil microscopy analysis revealed that the fried peanut DAG oil had higher trans-fatty acid and acid values and lower unsaturated fatty acid values than regular peanut oil. Furthermore, oil microscopy revealed changes in the functional groups of the oils and fats, further elucidating the quality changes that occur in oils and fats after frying.</p><p><strong>Conclusions: </strong>Raman spectroscopy combined with oil microscopy can be used to rapidly monitor the quality of frying oil after frying.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-04-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143784665","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 and Validation of a Sensitive LC-MS/MS Method for Simultaneous Determination of Several Nitrosamines in Large Volume Parenteral.","authors":"Lukas Jost, Shiwei Zhou, Frank Sprau, Payden Trujillo, Annie Wan, Lucas Shaner, Bilig Sechin, Lars Gläser, David Young, Percy Kampeis, Weichun Yang","doi":"10.1093/jaoacint/qsaf031","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf031","url":null,"abstract":"<p><strong>Background: </strong>Nitrosamines have gained significant attention in pharmaceutical industry. However, due to the significant daily dosage of large volume parenteral (LVP), the detection limit for these products should be in the ng per liter range, which many published methods cannot achieve.</p><p><strong>Objective: </strong>This study aimed to develop and validate a sensitive LC-MS/MS method for the simultaneous determination of several nitrosamines in LVP drug products.</p><p><strong>Method: </strong>Nitrosamines and related internal standards were separated on a Waters ACQUITY UPLC HSS T3 (100 × 2.1 mm, 1.8 µm) column on a LC-MS/MS system with gradient elution. Prior to the LC injection, a Carbon A solid phase extraction (SPE) column was utilized to pretreat the test solutions. The mobile phase was composed of 0.1% formic acid in water as mobile phase A, and neat methanol as mobile phase B. Analytes were detected via multiple reaction monitoring (MRM) mode and quantitated against internal reference standards with a quantitation limit of 2.5 ng/L for N-nitrosodimethylamine (NDMA), 0.75 ng/L for other Nitrosamine analytes.</p><p><strong>Results: </strong>The LC-MS/MS method was able to separate all analytes of interest by gradient elution within 15 min. The method was validated according to the guidelines described in the International Conference on Harmonization guideline ICH Q2(R2). The LOQ for NMDA is 2.5 ng/L, while for other nitrosamines, it is 0.75 ng/L in peritoneal dialysis and saline matrices. For haemofiltration solution, the LOQ is 1.0 ng/L for NDMA and 0.3 ng/L for other nitrosamines. The RSD% (n = 9) of the recovery did not exceed 25% in the method accuracy evaluation. A comparative testing in three labs revealed that all three laboratories are capable of accurately measuring nitrosamine levels at 10 ng/L within the intricate LVP matrix.</p><p><strong>Conclusions: </strong>The LC-MS/MS method for several nitrosamines was successfully developed, validated, and demonstrated to be accurate, robust, and specific.</p><p><strong>Highlights: </strong>The performance of this method can reach single digit ng/L level in LVP matrices. Comparative testing was conducted in three laboratories located in China, Germany, and the United States to ensure reproducibility of the method.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-04-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143782367","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":"Comparison of Neutral Detergent Fiber Analysis Methods for Feed Ingredients, Diets, and Feces of Pigs.","authors":"Yoojin Koh, Jeonghyeon Son, Beob Gyun Kim","doi":"10.1093/jaoacint/qsaf030","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf030","url":null,"abstract":"<p><strong>Background: </strong>An accurate determination of fiber concentrations in feeds and feces is critical for the measurement of fiber digestibility in pigs. The method of AOAC for determining amylase-treated neutral detergent fiber (aNDF; method 2002.04) has been widely used for pig diets. To overcome the complexity of AOAC procedure, the Ankom method is also available for determining aNDF. Although these 2 methods have been compared for ruminant diets and feces, the comparison of the methods for pig diets and feces has not been documented.</p><p><strong>Objective: </strong>The objective was to compare aNDF values determined by the AOAC (aNDFAOAC) and the Ankom methods (aNDFAnkom) of ingredients, diets, and feces for pigs.</p><p><strong>Method: </strong>A total of 255 test samples consisted of 26 feed ingredients, 39 diets, and 190 feces of pigs were analyzed for aNDF. To compare aNDFAOAC and aNDFAnkom, regression analyses were performed with the aNDFAnkom minus the mean aNDFAnkom as an independent variable and the aNDFAOAC minus the aNDFAnkom as a dependent variable.</p><p><strong>Results: </strong>The aNDFAnkom were greater than the aNDFAOAC by 2.90 percentage unit (standard error = 0.63; P < 0.001) on average for ingredients and by 2.56 percentage unit (standard error = 0.34; P < 0.001) on average for diets. For feces, the aNDFAnkom were greater than the aNDFAOAC by 1.30 percentage unit (standard error = 0.32; P < 0.001) on average. The differences between the aNDFAnkom and the aNDFAOAC were not consistent across the data ranges represented by a linear bias (slope = -0.16; standard error = 0.04; P < 0.001) in feces.</p><p><strong>Conclusions: </strong>Amylase-treated neutral detergent fiber concentrations determined by the Ankom method were greater than the AOAC method in pig feeds and feces.</p><p><strong>Highlights: </strong>Despite convenience, the Ankom method yields greater aNDF values compared with the AOAC method.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143733666","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":"Maple Syrup Adulteration: Fluorescence Fingerprints as a Source of Information for Enhanced Detection.","authors":"M Singh, M Zhang, M Espinal-Ruiz, S Rathnayake, J Xue, J Shi, X Liu, R Hanner, M G Corradini","doi":"10.1093/jaoacint/qsaf029","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf029","url":null,"abstract":"<p><strong>Background: </strong>Maple syrup is often adulterated by dilution or substitution with other syrups due to its high demand and price. Fingerprinting techniques, e.g., DNA barcoding, detect adulteration in other foods. However, extensive processing during the transformation of sap into syrup degrades the genetic material, lowering the efficacy of this approach. In contrast, fluorescence fingerprints (EEMs) rely on a sample's intrinsic fluorophores to provide valuable information for detecting adulteration.</p><p><strong>Objective: </strong>This study evaluates the capabilities and limitations of EEMs to scout for adulteration markers and discriminate between pure and adulterated maple syrup samples.</p><p><strong>Methods: </strong>EEMs of pure amber and dark maple syrups and admixtures with common adulterants (beet, corn, and rice syrups at 1-50%) were obtained using a spectrophotometer (λex=250-500 nm, and λem=280-650 nm). The major components of the EEMs were identified using PARAFAC and confirmed by LC-MS/MS. The ratio of intensities of the two most prevalent EEM features was calculated. An artificial neural network (ANN) and a convolutional neural network (CNN) were developed to analyze the EEMs based on emissions at two selected excitation wavelengths and the full EEM image, respectively, to discriminate presence and level of adulteration.</p><p><strong>Results: </strong>EEMs of the samples allowed identifying valuable discriminatory information. The efficacy of the ratio of the emission intensities at λem=350 and 425 (I425/I350) when λex= 290 nm to identify potential fraud (70-86% correct identifications) depended on the adulterant. This ratio was particularly effective for beet syrup adulteration, even at concentrations <2%. Applying machine learning algorithms improved detection for all adulterants. ANN correctly identified adulteration type and level (90 & 82%). The CNN approach accurately classified 75-99% of adulterated syrups but required additional computational power and denser data sets.</p><p><strong>Conclusion: </strong>This study aids in providing a quick, non-destructive and green monitoring tool for maple syrup adulteration based on its intrinsic fluorophores.</p><p><strong>Highlights: </strong>Maple syrup is often adulterated with other syrups due to high demand and price. DNA barcoding is ineffective in detecting maple syrup adulteration due to DNA degradation. Fluorescence fingerprints or EEMs allow scouting for discriminatory markers in maple syrup. Machine learning algorithms (ANN and CNN) applied to EEM data can aid detection.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-03-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143733693","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":"Chemical Fingerprints combined with chemometric analysis to evaluate and distinguish between Plantago asiatica L. and Plantago depressa Willd.","authors":"Guoqiang Liu, Zicheng Ma, Jinli Wen, Xiaoran Zhao, Yanru Deng, Lili Sun, Xiaoliang Ren","doi":"10.1093/jaoacint/qsaf023","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf023","url":null,"abstract":"<p><strong>Background: </strong>Plantago, also known as plantain, has been used as a traditional herb in Asia for centuries to treat urinary tract inflammation and kidney disease. Recently, there has been increasing interest in its potential applications in the food industry. In China, there are two common species of, namely Plantago asiatica L.(PAL) and P. depressa Willd.(PDW), which are not distinguished in folk and clinical practices, leading to safety and efficacy risks in plantago applications.</p><p><strong>Objectives: </strong>The objective of this study is to establish a reliable method for differentiating and evaluating the quality of PAL and PDW by integrating fingerprint analysis with multivariate chemometrics.</p><p><strong>Methods: </strong>Firstly, HPLC was used to collect chemical characteristic information from the whole plant samples of 13 PAL and 18 PDW, establishing fingerprints for the different species. Multiple chemometric methods, including hierarchical cluster analysis (HCA), principal component analysis (PCA), and partial least squares discriminant analysis (PLS-DA), were employed to analyze the chemical differences between the two species and to identify chemical markers. Finally, the differences in the content of the three chemical markers in the two plantago samples were determined and analyzed.</p><p><strong>Results: </strong>The analysis revealed a distinct classification of PAL and PDW into two groups. Significant differences were observed in the content of key components such as plantamajoside, acteoside, and isoacteoside between the two species.</p><p><strong>Conclusion: </strong>This study provides a reliable scientific basis for the rational application and quality evaluation of plantago. The findings contribute to ensuring the safe and effective use of plantago in various applications.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-03-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143712290","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":"An Ultra-High Performance Liquid Chromatography-Mass Spectrometry Method Based on Solid Phase Extraction Was Developed for the Analysis of Polyphenols in Prunus Mume Sieb. et Zucc.","authors":"Weiting Wang, Xuanxuan Fan, Naidong Chen, Jingwen Hao, Manman Zhang, Zhengjun Xie","doi":"10.1093/jaoacint/qsaf028","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf028","url":null,"abstract":"<p><strong>Background: </strong>Prunus mume Sieb. et Zucc. (P. mume) is rich in various phenolic compounds; however, there is a lack of effective quality evaluation methods.</p><p><strong>Objective: </strong>The aim of this study was to establish and validate a quality evaluation method that combines composition and activity to evaluate P. mume.</p><p><strong>Method: </strong>Phenolic compounds were quantified using an ultra-high performance liquid chromatography-diode array detector (UPLC-DAD) and identified using quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS). Solid-phase extraction (SPE) method was used for enrichment and purification. Chromatographic column: Eclipse Plus-C18 (2.1 × 50 mm, 5 μm); column temperature: 30 °C; detection wavelength: 325 nm, flow rate: 0.25 mL/min. 2,2'-azinobis- 3-ethylbenzthiazoline-6-sulphonate (ABTS) and ferric ion-reducing antioxidant power (FRAP) assays were used to determine the antioxidant activity of P. mume. In addition, tyrosinase inhibitory activity (TIA) was verified for the first time.</p><p><strong>Results: </strong>Twelve major phenolic compounds were identified, among which taxifolin and ferulic acid were first detected in P. mume. The established UPLC-DAD method exhibited a strong linear relationship (R2 = 0.9999). The LOD and LOQ of the standard compounds were in the ranges of 0.001-0.014 ng/g and 0.009-0.048 ng/g, respectively. The method exhibited good linearity, precision, stability and repeatability. The phenolic compound content was in the range of 0.38-75.88 mg/g. In addition, P. mume extract showed excellent ABTS•+ radical scavenging capacity (IC50 = 108.93 ± 9.43 μg/mL), FRAP (10.23 ± 0.11 μM), and TIA (IC50 = 4.79 ± 0.08 mg/mL).</p><p><strong>Conclusions: </strong>The established quality control method based on composition and activity is dependable and can be used for the quality control of P. mume.</p><p><strong>Highlights: </strong>SPE chromatographic analysis method is reliable and can provide a reference for quality control methods for the combination of ingredients and activity in flower-based foods.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-03-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143694884","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":"Extraction and measurement of 1,4 dioxane in detergents using head space microextraction followed by gas chromatography.","authors":"Azizollah Nezhadali, Masoumeh Darbanian, Mohammad Reza Mohammadian","doi":"10.1093/jaoacint/qsaf027","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf027","url":null,"abstract":"<p><strong>Background: </strong>1,4-dioxane is a hazardous by-product commonly found in sanitary detergents due to certain manufacturing processes. Accurate detection and quantification of this compound are essential for consumer safety.</p><p><strong>Objective: </strong>This study aims to develop and optimize a method for detecting and quantifying 1,4-dioxane in sanitary detergents. The approach involves electropolymerization of graphene oxide nanocomposites on stainless steel mesh, followed by headspace microextraction (HS-ME) and analysis using gas chromatography with a flame ionization detector (GC-FID).</p><p><strong>Methods: </strong>Graphene oxide nanocomposites were electropolymerized on stainless steel mesh to create the absorbent material. This absorbent was utilized in HS-ME for extracting 1,4-dioxane from sanitary detergent samples. A Plackett-Burman design (PBD) screened Seven factors, including extraction time, extraction temperature, salt addition effect, stirring speed, desorption time, type of extraction solvent, and volume of extraction solvent. Based on the screening results a central composite design (CCD) optimized the four critical factors: extraction time, extraction temperature, stirring speed, and type of extraction solvent. Quantification of 1,4-dioxane was performed using GC-FID.</p><p><strong>Results: </strong>The optimized method demonstrated a linear range of 0.5 to 200 μg/mL with a correlation coefficient (R2) of 0.9989. The limits of detection and quantification were determined as 0.15 and 0.5 μg/mL, respectively. Method accuracy, assessed through the relative recovery percentage of 1,4-dioxane, yielded values between 91.6 and 104%. Intra-laboratory reproducibility percentages ranged from 3.2 to 6.8%.</p><p><strong>Conclusion: </strong>The developed method, utilizing electropolymerized graphene oxide nanocomposites on stainless steel mesh for HS-ME coupled with GC-FID, provides a sensitive and accurate approach for detecting and quantifying 1,4-dioxane in sanitary detergents.</p><p><strong>Highlights: </strong>Electropolymerization of graphene oxide nanocomposites on stainless steel mesh was successfully implemented to create an effective absorbent for HS-ME of dioxane. A systematic optimization approach, combining PBD and CCD, identified and fine-tuned critical factors influencing extraction efficiency.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-03-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143672118","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":"Highly Sensitive Determination of Tetracycline in Milk Based on Gold Nanoparticles/Graphene Oxide/Molecularly Imprinted Polymer as Recognition Element and Signal Amplifier.","authors":"Bingyuan Su, Xiaotian Tian, Kexin Zou, Wanwan Wang, Xiaomei Chen","doi":"10.1093/jaoacint/qsaf024","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf024","url":null,"abstract":"<p><strong>Background: </strong>Tetracycline (TC) is widely utilized in aquaculture as a broad-spectrum antibiotic with notable bactericidal properties. Nevertheless, the inappropriate or excessive application of TC may result in the presence of antibiotic residues in edible tissues, presenting significant risks to human health. In this study, a tetracycline-sensitive electrochemical sensor was developed by modifying glassy carbon electrodes with gold nanoparticles (AuNPs)/graphene oxide (GO)/tetracycline-templated molecularly imprinted polymer (MIP) composites.</p><p><strong>Objective: </strong>A highly sensitive sensor for the detection of tetracycline in milk.</p><p><strong>Methods: </strong>The MIP, synthesized by thermal polymerization, acted as a selective recognition element and pre-concentrating agent for tetracycline. To improve the conductivity of the MIP film and enhance the transfer of electrons across the electrode surface, AuNPs/GO composites were embedded in the MIP film. The morphology, structure, thermal stability, and electrochemical properties of the AuNPs/GO-MIP film were characterized through the utilization of scanning electron microscopy, Fourier-transform infrared spectroscopy, thermogravimetric analysis, and electrochemical impedance spectroscopy.</p><p><strong>Results: </strong>The modified electrode, featuring a composite film, exhibited a broad linear detection range (1-30 μg/L, 0.03-0.5 mg/L, and 0.5-20 mg/L), low detection limit (0.7 μg/L; S/N = 3), and high selectivity toward tetracycline.</p><p><strong>Conclusion: </strong>The proposed sensor effectively quantified tetracycline in milk.</p><p><strong>Highlights: </strong>In this study, AuNPs/GO composites were embedded to improve the conductivity of the composites; conductive MIP films were prepared and used as recognition elements and signal amplifiers. We present an electrochemical sensor for sensitive and selective detection of tetracycline; the sensor can effectively quantify tetracycline in milk.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-03-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143672119","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}