Journal of AOAC International最新文献

{"title":"Relevance of Secondary Enrichment in the Detection of Salmonella Spp in Food Samples by qPCR according to DIN 10135","authors":"F Codony, G Agustí, L Barreto, D Asensio","doi":"10.1093/jaoacint/qsae002","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae002","url":null,"abstract":"Background When detecting Salmonella spp. in food samples, unlike with culture-based procedures where there are solid standards, PCR techniques are generally dominated by commercial solutions, often backed by the conformity of reference organizations, and based on rigorous validation studies. The few independent standards that exist are not subject to revision and improvement to the same extent as the manufacturer's methods. Moreover, since commercial networks do not promote them, they are less implemented in everyday practice. The German standard DIN 10135 is an example of this. In this method, before PCR detection, a primary enrichment (16–20 h) followed by a secondary selective enrichment of at least 6 hours is needed. Nevertheless, it allows the possibility of only apply the first step if evidence of their correct operation is provided. Objective To evaluate how necessary is the secondary enrichment for DIN 10135 standard. Methods Short and complete enrichment steps were compared in the context of the evaluation of the limit of detection for 11 types of food. Additionally, a blind assay was performed with 75 food samples. Results The data show that a simple primary enrichment may be sufficient and that the second selective enrichment with the tested matrices would not be strictly essential. The blind study obtained a 98.6% of trueness and precision of 100%. Conclusions At least for the end consumer products, a secondary enrichment of 6 hours is not necessary for all the products tested. Highlights In the context of the DIN 10135 standard, the primary enrichment (16–20 h, 37 ± 1 °C) can be enough for detecting Salmonella spp.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-01-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139462938","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Stability Study Through Water Activity Measurements for Dispensed Powdered Raw Materials","authors":"Harold A Prada-Ramírez, Juan Pablo Montes-Tamara, Eduardo A Rico-Jimenez, Juan Camilo Fonseca","doi":"10.1093/jaoacint/qsae005","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae005","url":null,"abstract":"Background Holding times for raw materials are relevant, since they enable us to understand the allowable time that a raw material can be kept under ideal storage conditions before the start of the manufacturing process without its quality attributes being affected. The quantification of water activity can be used as an indicator of the microbiological, physicochemical, and organoleptic stability of a specimen, since low water activity retards autohydrolysis and microbiological growth. Objective The main purpose of this investigation was to test the stability of powdered raw materials for a maximum holding time of 8 days through water activity measurements. Thus microbiological, physicochemical, and organoleptic measurements were carried out in parallel and simultaneously in order to experimentally establish a relationship between the status of the water activity of processed raw materials and the microbiological, physicochemical, and organoleptic results. Results The raw materials were stored for a maximum holding time of 8 days, in accordance with USP monographs. For all the raw materials tested, water activity measurements were performed using the dew point chilled-mirror method on days 0, 3, and 8. On days 0 and 8, microbiological, physicochemical, and organoleptic assessments were performed. It was established that under these storage conditions, the processed raw materials exhibited water activity below 0.60 during the entire holding time. However, there were statistically significant differences in water activity levels between days 0, 3, and 8 (ANOVA P < 0.05). Despite observing statistically significant differences between days, the microbiological, physicochemical, and organoleptic features were within specification at those water activity levels, below 0.60. Conclusion Water activity below 0.60 does not allow the growth of microorganisms, and the organoleptic and physicochemical features remain unperturbed. The results indicate that water activity can be used as an indicator of the microbiological load and chemical stability of the raw materials tested.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-01-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139462985","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 Seven Human Milk Oligosaccharides (HMO) in Infant Formula and Adult Nutritionals: First Action 2022.07","authors":"Thierry Bénet, Nathalie Frei, Véronique Spichtig, Denis Cuany, Sean Austin","doi":"10.1093/jaoacint/qsae001","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae001","url":null,"abstract":"Background Human milk oligosaccharides (HMOs) are important components of breast milk and may be responsible for some of the benefits of breastfeeding, including resistance to infections and the development of a healthy gut microbiota. Selected HMOs are now available for addition to infant formula, and suitable methods to control the dosing rate are needed. Objective To develop and validate a suitable method for the analysis of HMOs in infant formula. Method A method was developed for the determination of seven human milk oligosaccharides (2’-fucosyllactose, 3-fucosyllactose, 3’-sialyllactose, 6’-sialyllactose (6’SL), 2’,3-difucosyllactose, lacto-N-tetraose (LNT), lacto-N-neotetraose (LNnT)) in infant formula and adult nutritionals. The oligosaccharides are labelled at their reducing end with 2-aminobenzamide, separated by liquid chromatography and detected using a fluorescence detector. Maltodextrins are enzymatically hydrolyzed before analysis to prevent potential interference, likewise an optional β-galactosidase treatment can be used to remove β-galactooligosaccharides. Fructooligosaccharides or polydextrose do not generally interfere with the analysis. Results The method has been validated in a single laboratory on infant formula and adult nutritionals. The seven HMOs were spiked in to eight matrices at three or four spike levels giving a total of 176 data points. Recoveries were in the range 90.9–109% in all cases except at the lowest spike level in one matrix (elemental formula), where the LNT recovery was 113%, the LNnT recovery was 111% and the 6’SL recovery was 121%. Relative repeatabilities (RSD(r)) were in the range 0.1–4.2%. The performance is generally within the requirements outlined in the Standard Method Performance Requirements (SMPR®) published by AOAC International. Conclusions The method developed is suitable for the determination of seven HMOs in infant formula and demonstrated good performance during single laboratory validation. Highlights A method has been developed which is suitable for the determination of seven HMOs in infant formula.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-01-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139462850","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Stability and Biosimilarity Assessment of Bevacizumab Monoclonal Antibody; Orthogonal Testing Protocol Coupled With Peptide Mapping-Principal Component Analysis.","authors":"Sara H Abdelghaffar, Maha A Hegazy, Basma M Eltanany","doi":"10.1093/jaoacint/qsad094","DOIUrl":"10.1093/jaoacint/qsad094","url":null,"abstract":"<p><strong>Background: </strong>Biologics are essential in cancer treatment because they stimulate the body's natural response to fight cancer, but they are expensive. Biosimilars are more affordable compared to patent biologicals, but it must be verified that they are as effective as their innovators. Characterization of biosimilars and assessment of interchangeability requires many data points for verification.</p><p><strong>Objective: </strong>The proposed study provides a quality assessment of two new bevacizumab (BVZ) biosimilars, produced by Amgen and Biocad, Inc., through the development and greenness assessment of an orthogonal testing protocol and purity indicating assay, including size-exclusion (SE-HPLC), reversed-phase (RP-HPLC), and cation exchange chromatography (CEX-HPLC) in addition to dynamic light scattering (DLS) and sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE).</p><p><strong>Methods: </strong>SE-HPLC method was performed and validated to screen the BVZ monomer and its aggregates and/or fragments. Peak purity and system suitability parameters were calculated. Results indicate that the orthogonal protocol is a useful tool for assessing monoclonal antibody stability. It is a key criterion for biosimilarity assessment. DLS and SDS-PAGE results were compared to each other to reveal close retention times and banding patterns between BVZ innovator and its biosimilars. These results showed that Avastin® and the investigated biosimilars have the same profile in terms of peak area of related compounds within the acceptance limit and apparent molecular weight, and the SDS-PAGE technique was found to be the most eco-friendly technique among others.</p><p><strong>Conclusions: </strong>The results obtained highlighted the importance of assessing similarities and differences in ensuring the biosimilarity and interchangeability of the studied products.</p><p><strong>Highlights: </strong>BVZ is one of the essential monoclonal antibodies in the treatment of colorectal cancer (CRC). BVZ biosimilars were evaluated by developing an orthogonal testing protocol and a purity-indicating assay. The size-exclusion (SE)-HPLC method was applied and validated to monitor the BVZ monomer and its aggregates. The results demonstrated the importance of assessing the stability and biosimilarity of BVZ.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10414985","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Green HPLC Method for Simultaneous Analysis of Three Natural Antioxidants by Analytical Quality by Design.","authors":"Ramya Jonnalagadda, Seetharaman Rathinam, Krishnaveni Nagappan, Vinodhini Chandrasekar","doi":"10.1093/jaoacint/qsad105","DOIUrl":"10.1093/jaoacint/qsad105","url":null,"abstract":"<p><strong>Background: </strong>Glutathione, silybin, and curcumin are well-known potential antioxidants that are recommended as adjuvant therapy in cancer treatment.</p><p><strong>Objective: </strong>Based on the principles of Analytical Quality by Design (AQbD) and green analytical chemistry, a simple, robust, and environmentally benign HPLC method for the simultaneous estimation of glutathione, silybin, and curcumin in bulk and formulation was performed.</p><p><strong>Method: </strong>Elution was achieved by an Agilent Eclipse XDB C18 (150 mm × 4.6 mm id, 3.5 μm) column using a gradient mobile phase composed of ethanol-water pH 6.7 (with 0.1%, v/v orthophosphoric acid) and 1.07 mL/min flow rate with PDA detection at 215 nm. Critical method variables were identified by risk assessment using an Ishikawa diagram, and multivariate optimization of the experimental conditions for the HPLC technique was accomplished by central composite design using design of experiments (DoE) software.</p><p><strong>Results: </strong>The separation was achieved within 15 min, where the retention time of glutathione, silybin, and curcumin were 3.3, 4.9, and 7.3 min, respectively. The standard curve was linear in the range of 3.75-26.25 µg/mL for glutathione, 62.50-437.50 µg/mL for silybin, and 12.5-87.50 µg/mL for curcumin. The developed method was validated as per ICH guidelines Q2 (R1), and all the parameters are within specified limits.</p><p><strong>Conclusions: </strong>The proposed method is simple, precise, and robust, which can be employed for routine analysis and also concluded to be a greener approach according to AGREE, Green Analytical Procedure Index, and analytical eco-scale tools.</p><p><strong>Highlights: </strong>The chosen antioxidants were evaluated for the very first time simultaneously using the chromatographic technique in bulk and dosage forms employing green solvents. The peak purity of all three compounds was studied using a PDA detector. Wastage was reduced in terms of time, cost, and solvents by employing AQbD elements and tools. Complete application of environmentally sustainable safe solvents were employed.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10214818","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":"Smart Multivariate Spectrophotometric Determination of Two Co-Administered Autoimmune Drugs; Sulfasalazine and Pentoxifylline; in Bulk and Spiked Human Plasma.","authors":"Maimana A Magdy, Nehal F Farid, Basma H Anwar, Nessreen S Abdelhamid","doi":"10.1093/jaoacint/qsad097","DOIUrl":"10.1093/jaoacint/qsad097","url":null,"abstract":"<p><strong>Background: </strong>Sulfasalazine and pentoxifylline are co-prescribed together to treat psoriasis and pemphigus vulgaris. Sulfasalazine is an anti-inflammatory, immunosuppressant, and antibiotic drug, while pentoxifylline is a vasodilator and immunosuppressant. The spectra of the two drugs and plasma suffer from severe overlap.</p><p><strong>Objective: </strong>This work aims to simultaneously determine sulfasalazine and pentoxifylline in their binary mixture and spiked human plasma by the assessment of their UV spectral data.</p><p><strong>Methods: </strong>Two model updated chemometric methods were established using principal component regression and partial least-squares regression models. The two models were validated in accordance with the U.S. Food and Drug Administration guidelines for bioanalysis and were applied for the determination of both drugs in synthetic mixtures or spiked human plasma.</p><p><strong>Results: </strong>Accuracy and precision were within the accepted limits. In addition, three different assessment methods were used to evaluate the environmental greenness of the proposed models.</p><p><strong>Conclusion: </strong>The two updated models are simple, rapid, sensitive, and precise, and could be easily applied in QC laboratories for determination of sulfasalazine and pentoxifylline, without any preliminary separation steps or interference from plasma matrix.</p><p><strong>Highlights: </strong>Two updated chemometric models called principlal component regression and partial least-squares regression were established for determination of sulfasalazine and pentoxifylline in spiked human plasma using UV spectrophotometric data.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10052760","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 Chromatographic Estimation of Vildagliptin and Dapagliflozin Using Hybrid Principles of White Analytical Chemistry and Analytical Quality by Design.","authors":"Pintu Prajapati, Bageshree Rana, Veera Shakar Pulusu, Shailesh Shah","doi":"10.1093/jaoacint/qsad108","DOIUrl":"10.1093/jaoacint/qsad108","url":null,"abstract":"<p><strong>Background: </strong>The fixed-dose combination of vildagliptin (VDG) and dapagliflozin (DGZ) is used in the treatment of type 2 diabetes mellitus. According to the literature survey, RP-HPLC and HPTLC methods have been reported for routine analysis of VDG and DGZ. These chromatographic methods have been developed using potentially neurotoxic and teratogenic solvents, which are unsafe for human and aquatic animal life and hazardous to the environment. These types of organic solvents shall be replaced or reduced during chromatographic analysis of drugs for the safety of human and aquatic animal life and the protection of the environment. The novel white analytical chemistry (WAC) approach has been introduced, which emphasizes robust, green, user-friendly, economical, and rapid analysis of drug samples.</p><p><strong>Objective: </strong>Hence, the WAC-based RP-HPLC method has been developed for the estimation of VDG and DGZ using lower toxic and economical solvents.</p><p><strong>Method: </strong>The development of the RP-HPLC method includes the implementation of the analytical quality by design approach using principles of design of experiments to reduce organic waste generation and regulatory compliance of analytical method. The central composite design was applied for response surface modeling (RSM) and optimization of the RP-HPLC method. The method validation was carried out according to ICH Q2 (R1) guidelines.</p><p><strong>Results: </strong>The fixed-dose combinations of VDG and DGZ were assayed, and results were found in compliance with their labeled claim. The published and proposed RP-HPLC methods were assessed for chromatographic analysis of VDG and DGZ using the Red-Green-Blue (RGB) model, AGREE calculator, Eco-Scale Assessment tool, GAPI software, and NEMI standards.</p><p><strong>Conclusions: </strong>The proposed method was found to be robust, green, economical, and user-friendly for chromatographic analysis of VDG and DGZ. The proposed method can be an economical and eco-friendly analytical tool in the pharmaceutical industry for quality control and routine analysis of fixed-dose combinations of VDG and DGZ.</p><p><strong>Highlights: </strong>Hybrid principles of WAC and analytical quality by design to RP-HPLC method for simultaneous estimation of VDG and DGZ in their fixed-dose combinations.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10277600","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A Simple UV Spectrophotometric Method Based on Continuous Wavelet Transform and Multivariate Calibration Model for the Concurrent Analysis of Three Water-Soluble Vitamins in Fertility Supplements.","authors":"Mahla Lohrdy, Mahmoud Reza Sohrabi, Mehran Davallo","doi":"10.1093/jaoacint/qsad093","DOIUrl":"10.1093/jaoacint/qsad093","url":null,"abstract":"<p><strong>Background: </strong>Owing to the presence of overlapping spectra in pharmaceutical components, classical spectrophotometry is hard for concurrent determination. The advance of chemometrics along with UV-Vis spectrophotometry has contributed to solving this problem.</p><p><strong>Objective: </strong>In this study, a fast, easy, precise, accurate, low-cost, and eco-friendly spectrophotometric technique was introduced and validated for the simultaneous analysis of vitamin B6, vitamin B12, and vitamin C in fertility supplements for men and women using continuous wavelet transform (CWT) and partial least squares (PLS) techniques without using time-consuming extraction process and organic solvents.</p><p><strong>Method: </strong>In the CWT method, the zero-crossing technique was applied to obtain the optimum points for plotting calibration curves for each component. The validation of both methods was evaluated by analyzing several mixtures with different concentrations. The efficiency of the proposed methods was also surveyed on commercial capsules.</p><p><strong>Results: </strong>Wavelet families, including Symlet (sym2) at 230, Biorthogonal (bior1.3) at 378 nm, and Daubechies (db2) at 261, were considered for vitamins B6, B12, and C, respectively. The linear range was found to be 8-20, 8-20, and 10-25 μg/mL with the coefficient of determination (R2) equal to 0.9982, 0.9978, and 0.9701 for B6, B12, and C, respectively. Low limit of detection (LOD) (<0.09 μg/mL) and limit of quantification (LOQ) <0.9 μg/mL were achieved. The mean recovery values in synthetic mixtures were from 98.38 to 98.89% and from 99.83 to 99.99%, where root-mean-square error (RMSE) of not more than 0.4 and 0.05 using the CWT and PLS methods, respectively.</p><p><strong>Conclusions: </strong>The obtained results from the commercial capsules, applying the suggested techniques, were compared to those yielded by the high-performance liquid chromatography (HPLC) method using the analysis of variance (ANOVA) test. According to the results, there are no significant differences, and they were in good agreement. According to all the mentioned cases, the proposed approaches can replace the time-consuming and costly HPLC method in quality control laboratories.</p><p><strong>Highlights: </strong>Green spectrophotometry coupling chemometrics methods were proposed. Simultaneous determination of three water-soluble vitamins in fertility supplements was done using these approaches. Rapidity, simplicity, low cost, and accuracy are the benefits of the proposed methods. A HPLC technique was used as a reference method to compare with the chemometrics methods.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10414983","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 and Validation of a Method for Trace Level Zinc Quantification in Pharmaceutical Zinc Supplements Using a Carboxyl Functional Group Packed Column and Refractive Index Detector.","authors":"Nagavardhana Reddy Vanga, Venkata Ratnam Kesamsetty, Kumaraswamy Ummiti, Venkata Nadh Ratnakaram, Hanimi Reddy Bapatu","doi":"10.1093/jaoacint/qsad101","DOIUrl":"10.1093/jaoacint/qsad101","url":null,"abstract":"<p><strong>Background: </strong>Zinc helps with cell division, growth, wound healing, and carbohydrate breakdown. Humanbeings have to obtain zinc from food or supplements because our bodies do not produce it naturally. In view of the greater advantages (such as low cost, time of analysis, and stability-indicating) compared to other quantification methods (titration, ion chromatography, Atomic absorption spectroscopy) proposed in the literature, a refractive index detector coupled with HPLC has been used in quantification of zinc.</p><p><strong>Objective: </strong>The goal of this research is to develop and validate a sensitive, low-cost, high-resolution, and stability- indicating method for detecting and quantifying zinc levels in zinc supplement pharmaceutical products (injectables, tablets, and capsules).</p><p><strong>Methods: </strong>A novel isocratic reverse-phase HPLC method with a refractive index detector (with sensitivity 64, detector temperature 35°C, and positive polarity) was developed using a carboxyl functional group packed column and 0.8% (v/v) formic acid as the mobile phase to detect and quantify zinc content.</p><p><strong>Results: </strong>The reported method has a good optimal sensitivity (LOQ: 0.006 mg/mL and LOD: 0.002 mg/mL). The correlation coefficient (r) obtained from the zinc calibration plot was greater than 0.998, indicating that the method was linear and that there was a strong correlation between zinc concentration (0.006 mg/mL to 0.375 mg/mL) and peak response. The accuracy at LOQ level was found to be 95-105% and 97-103% at the remaining levels (50, 100, and 150%).</p><p><strong>Conclusion: </strong>The proposed method was successfully developed and validated as per International council for harmonisation (ICH) guidelines. Therefore, this method can be used for the quantitative testing of zinc in the QC laboratory.</p><p><strong>Highlights: </strong>A novel method was developed for zinc levels determination in pharmaceutical products using HPLC with a refractive index detector. The present approach has a quick run time of 10 min and is inexpensive.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10172141","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":"Detection of the Adulteration of Dendrobium Huoshanense with Dendrobium Henanense by UV-Vis-Shortwave Near-Infrared Diffuse Reflectance Spectroscopy Combined with Chemometrics.","authors":"Jing-Wen Hao, Nai-Dong Chen, Xiao-Quan Liu, Qiang Li, Hui-Min Xu, Wei-Han Yang, Chao-Feng Qin, Ya-Qing Bu","doi":"10.1093/jaoacint/qsad090","DOIUrl":"10.1093/jaoacint/qsad090","url":null,"abstract":"<p><strong>Background: </strong>Dendrobium huoshanense (DHS) is a classic traditional Chinese medicine (TCM) with distinctive medicinal benefits and great economic worth; nevertheless, because of similar tastes and looks, it is simple to adulterate with less expensive substitutes (such as Dendrobium henanense [DHN]).</p><p><strong>Objective: </strong>This work aimed to develop a reliable tool to detect and quantify the adulteration of DHS with DHN by using UV-Vis-shortwave near-infrared diffuse reflectance spectroscopy (UV-Vis-SWNIR DRS) combined with chemometrics.</p><p><strong>Methods: </strong>Adulterated samples prepared in varying concentrations (0-100%, w/w) were analyzed with UV-Vis-SWNIR DRS methods. Partial least-square-discriminant analysis (PLS-DA) and partial least-squares (PLS) regression techniques were used for the differentiation of adulterated DHN from pure DHS and the prediction of adulteration levels.</p><p><strong>Results: </strong>The PLS-DA classification models successfully differentiated adulterated and nonadulterated DHS with an over 100% correct classification rate. UV-Vis-SWNIR DRS data were also successfully used to predict adulteration levels with a high coefficient of determination for calibration (0.9924) and prediction (0.9906) models and low error values for calibration (3.863%) and prediction (5.067%).</p><p><strong>Conclusion: </strong>UV-Vis-SWNIR DRS, as a fast and environmentally friendly tool, has great potential for both the identification and quantification of adulteration practices involving herbal medicines and foods.</p><p><strong>Highlights: </strong>UV-Vis-SWNIR DRS combined with chemometrics can be applied to identify and quantify the adulteration of herbal medicines and foods.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9981228","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}