Journal of AOAC International最新文献

{"title":"Predictive Analysis of Quality Markers of Atractylodis Rhizoma Based on Fingerprint and Network Pharmacology.","authors":"Yanyun Zhao,&nbsp;Xinxin Chang,&nbsp;Xian Gu,&nbsp;Yang Li,&nbsp;Yuguang Zheng,&nbsp;Huiyong Fang","doi":"10.1093/jaoacint/qsad059","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad059","url":null,"abstract":"<p><strong>Background: </strong>Atractylodes chinensis (DC.) Koidz. (A. chinensis) is a perennial herbaceous plant that is widely used as a Chinese medicine herb for gastric diseases. However, the bioactive compounds of this herbal medicine have not been defined, and quality control is imperfect.</p><p><strong>Objective: </strong>Although the method of quality evaluation method for A. chinensis by high-performance liquid chromatography (HPLC) fingerprinting has been reported in related papers, it remains unknown whether the chemical markers selected are representative of their clinical efficacy. To develop methods for qualitative analysis and improved quality evaluation of A. chinensis.</p><p><strong>Method: </strong>In this study, HPLC was used to establish fingerprints and conduct similarity evaluation. Principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA) were used to reveal the differences of these fingerprints. Network pharmacology was used to analyze the corresponding targets of the active ingredients. Meantime, an active ingredient-target-pathway network was constructed to investigate the characteristics of the medical efficacy of A. chinensis and to predict potential Q-markers.</p><p><strong>Results: </strong>Combining network pharmacological effectiveness and composition specificity with the Q-marker concept, atractylodin (ATD), β-eudesmol, atractylenolide Ι (AT-I) and atractylenolide III (AT-III) were predicted to be potential Q-markers of A. chinensis that showed anti-inflammatory, antidepressant, anti-gastric, and antiviral effects by acting on 10 core targets and 20 key pathways.</p><p><strong>Conclusions: </strong>The HPLC fingerprinting method established in this study is straightforward, and the identified four active constituents can be used as Q-markers of A. chinensis. These findings facilitate effective quality evaluation of A. chinensis and suggest this approach could be applied to evaluate the quality of other herbal medicines.</p><p><strong>Highlights: </strong>The fingerprints of Atractylodis rhizoma were organically combined with network pharmacology to further clarify its criteria for quality control.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10496154","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":"Computer-Aided Design of Eco-Friendly Imprinted Polymer Decorated Sensors Augmented by Self-Validated Ensemble Modeling Designs for the Quantitation of Drotaverine Hydrochloride in Dosage Form and Human Plasma.","authors":"Aziza E Mostafa,&nbsp;Maya S Eissa,&nbsp;Ahmed Elsonbaty,&nbsp;Khaled Attala,&nbsp;Randa A Abdel Salam,&nbsp;Ghada M Hadad,&nbsp;Mohamed A Abdelshakour","doi":"10.1093/jaoacint/qsad049","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad049","url":null,"abstract":"<p><strong>Background: </strong>Computationally designed molecular imprinted polymer (MIP) incorporation into electrochemical sensors has many advantages to the performance of the designed sensors. The innovative self-validated ensemble modeling (SVEM) approach is a smart machine learning-based (ML) technique that enables the design of more accurate predictive models using smaller data sets.</p><p><strong>Objective: </strong>The novel SVEM experimental design methodology is exploited here exclusively to optimize the composition of four eco-friendly PVC membranes augmented by a computationally designed magnetic molecularly imprinted polymer to quantitatively determine drotaverine hydrochloride (DVN) in its combined dosage form and human plasma. Furthermore, the application of hybrid computational simulations such as molecular dynamics and quantum mechanical calculations (MD/QM) is a time-saving and eco-friendly provider for the tailored design of the MIP particles.</p><p><strong>Method: </strong>Here, for the first time, the predictive power of ML is assembled with computational simulations to develop four PVC-based sensors decorated by computationally designed MIP particles using four different experimental designs known as central composite, SVEM-LASSO, SVEM-FWD, and SVEM-PFWD. The pioneering AGREE approach further assessed the greenness of the analytical methods, proving their eco-friendliness.</p><p><strong>Results: </strong>The proposed sensors showed decent Nernstian responses toward DVN in the range of 58.60-59.09 mV/decade with a linear quantitative range of 1 × 10-7 - 1 × 10-2 M and limits of detection in the range of 9.55 × 10-8 to 7.08 × 10-8 M. Moreover, the proposed sensors showed ultimate eco-friendliness and selectivity for their target in its combined dosage form and spiked human plasma.</p><p><strong>Conclusions: </strong>The proposed sensors were validated in accordance with International Union of Pure and Applied Chemistry (IUPAC) recommendations, proving their sensitivity and selectivity for drotaverine determination in dosage form and human plasma.</p><p><strong>Highlights: </strong>This work presents the first ever application of both the innovative SVEM designs and MD/QM simulations in the optimization and fabrication of drotaverine-sensitive and selective MIP-decorated PVC sensors.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10141671","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Validation of the AnticFast® Beta-Lactams Rapid Test Kit for Detection of Beta-Lactams (Penicillins and Cephalosporins) in Raw Cow's Milk: AOAC Performance Tested MethodSM 032303.","authors":"Katrien Broekaert,&nbsp;Sigrid Ooghe,&nbsp;Meng Yang,&nbsp;Xiumei Tian,&nbsp;Wim Reybroeck","doi":"10.1093/jaoacint/qsad054","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad054","url":null,"abstract":"<p><strong>Background: </strong>AnticFast® Beta-Lactams Rapid Test Kit is a qualitative two-step (2 min + 5 min) rapid lateral flow assay to detect β-lactam (penicillins and cephalosporins) antibiotic residues in raw commingled cow's milk.</p><p><strong>Objective: </strong>The method performance was evaluated according to Commission Decision 2002/657/EC, Commission Implementing Regulation 2021/808, and Community Reference Laboratories Residues Guidelines for the Validation of Screening Methods for Residues of Veterinary Medicines.</p><p><strong>Methods: </strong>The AnticFast Beta-Lactams Rapid Test Kit was evaluated for detection capability, selectivity, false-positive results, repeatability, robustness, suitability for various milk types and milk compositions, milks from various species, and test kit consistency and stability. Samples included milks spiked at concentrations bracketing the EU maximum residue limits (MRLs) for β-lactams as well as bulk farm and tanker milks.</p><p><strong>Results: </strong>The AnticFast Beta-Lactams Rapid Test Kit is specific for the detection of β-lactams in milk and does not detect compounds from other antibiotic families. Interference was seen with clavulanic acid, a β-lactamase inhibitor, which was expected. The test can detect all residues of β-lactams (penicillins and cephalosporins) present on the EU-MRL list for milk at their respective MRL except for desfuroylceftiofur and cephalexin, which were above the MRL. No false positives were detected in the 602 (300 blank farm and 302 tanker load) samples tested. Robustness testing indicated that the detection in heat-treated milk types may be slightly hampered. For substances with a detection capability well below the MRL, this interference does not cause problems since detection at MRL remains guaranteed, but care should be taken for substances with a CCβ at or near their MRL. Diminished sample flow was seen with reconstituted milk powder and blank ewes' milk, so sample flow should always be verified for these milk types.</p><p><strong>Conclusions: </strong>Results of this validation show that the AnticFast Beta-Lactams Rapid Test Kit is a reliable test for rapid screening of raw cows' milk for residues of β-lactam antibiotics.</p><p><strong>Highlights: </strong>AnticFast Beta-Lactams Rapid Test Kit is an easy, realiable, robust and highly specific test for screening of raw cows' milk for residues of penicillins and cephalosporins.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10496150","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 Comprehensive Quality Evaluation of Cimicifugae Rhizoma Using UPLC-Q-Orbitrap-MS/MS Coupled with Multivariate Chemometric Methods.","authors":"Zi Cheng Ma,&nbsp;Mei Qi Liu,&nbsp;Guo Qiang Liu,&nbsp;Zhen Yu Zhou,&nbsp;Xiao Liang Ren,&nbsp;Lili Sun,&nbsp;Meng Wang","doi":"10.1093/jaoacint/qsad064","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad064","url":null,"abstract":"<p><strong>Background: </strong>Cimicifugae Rhizoma, known in Chinese as Shengma, is a common medicinal material in traditional Chinese medicine (TCM), mainly used for treating wind-heat headaches, sore throat, uterine prolapse, and other diseases.</p><p><strong>Objectives: </strong>An approach using a combination of ultra-performance liquid chromatography (UPLC), MS, and multivariate chemometric methods was designed to assess the quality of Cimicifugae Rhizoma.</p><p><strong>Methods: </strong>All materials were crushed into powder and the powdered sample was dissolved in 70% aqueous methanol for sonication. Chemometric methods, including hierarchical cluster analysis (HCA), principal component analysis (PCA), and orthogonal partial least-squares discriminant analysis (OPLS-DA), were adopted to classify and perform a comprehensive visualization study of Cimicifugae Rhizoma. The unsupervised recognition models of HCA and PCA obtained a preliminary classification and provided a basis for classification. In addition, we constructed a supervised OPLS-DA model and established a prediction set to further validate the explanatory power of the model for the variables and unknown samples.</p><p><strong>Results: </strong>Exploratory research found that the samples were divided into two groups, and the differences were related to appearance traits. The correct classification of the prediction set also demonstrated a strong predictive ability of the models for new samples. Subsequently, six chemical makers were characterized by UPLC-Q-Orbitrap-MS/MS, and the content of four components was determined. The results of the content determination revealed the distribution of representative chemical markers caffeic acid, ferulic acid, isoferulic acid, and cimifugin in two classes of samples.</p><p><strong>Conclusions: </strong>This strategy can provide a reference for assessing the quality of Cimicifugae Rhizoma, which is significant for the clinical practice and QC of Cimicifugae Rhizoma.</p><p><strong>Highlights: </strong>The HCA, PCA and OPLS-DA models visually classify Cimicifugae Rhizoma by appearance traits and obtain the chemical markers that influence the classification. The training and prediction sets were built to demonstrate the accuracy of the classification. Advanced UPLC-Q-Orbitrap-MS/MS technology provides powerful elucidation of critical chemical markers.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10133009","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":"Amplicon Sequencing Minimal Information (ASqMI): Quality and Reporting Guidelines for Actionable Calls in Biodefense Applications.","authors":"Ishi Keenum,&nbsp;Robert Player,&nbsp;Jason Kralj,&nbsp;Stephanie Servetas,&nbsp;Michael D Sussman,&nbsp;Joe Russell,&nbsp;Jennifer Stone,&nbsp;Sailaja Chandrapati,&nbsp;Shanmuga Sozhamannan","doi":"10.1093/jaoacint/qsad047","DOIUrl":"10.1093/jaoacint/qsad047","url":null,"abstract":"<p><strong>Background: </strong>Accurate, high-confidence data is critical for assessing potential biothreat incidents. In a biothreat event, false-negative and -positive results have serious consequences. Worst case scenarios can result in unnecessary shutdowns or fatalities at an exorbitant monetary and psychological cost, respectively. Quantitative PCR assays for agents of interest have been successfully used for routine biosurveillance. Recently, there has been increased impetus for adoption of amplicon sequencing (AS) for biosurveillance because it enables discrimination of true positives from near-neighbor false positives, as well as broad, simultaneous detection of many targets in many pathogens in a high-throughput scheme. However, the high sensitivity of AS can lead to false positives. Appropriate controls and workflow reporting can help address these challenges.</p><p><strong>Objectives: </strong>Data reporting standards are critical to data trustworthiness. The standards presented herein aim to provide a framework for method quality assessment in biodetection.</p><p><strong>Methods: </strong>We present a set of standards, Amplicon Sequencing Minimal Information (ASqMI), developed under the auspices of the AOAC INTERNATIONAL Stakeholder Program on Agent Detection Assays for making actionable calls in biosurveillance applications. In addition to the first minimum information guidelines for AS, we provide a controls checklist and scoring scheme to assure AS run quality and assess potential sample contamination.</p><p><strong>Results: </strong>Adoption of the ASqMI guidelines will improve data quality, help track workflow performance, and ultimately provide decision makers confidence to trust the results of this new and powerful technology.</p><p><strong>Conclusion: </strong>AS workflows can provide robust, confident calls for biodetection; however, due diligence in reporting and controls are needed. The ASqMI guideline is the first AS minimum reporting guidance document that also provides the means for end users to evaluate their workflows to improve confidence.</p><p><strong>Highlights: </strong>Standardized reporting guidance for actionable calls is critical to ensuring trustworthy data.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10472743/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10141655","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Updated Journal Scope.","authors":"Xu-Liang Cao","doi":"10.1093/jaoacint/qsad069","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad069","url":null,"abstract":"","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10230593","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 Easily Implemented Spectrophotometric Methods for Concurrent Determination of Ephedrine Hydrochloride and Naphazoline Nitrate in Nasal Preparations Containing Methylparaben.","authors":"Rehab M Abdelfatah,&nbsp;Maimana A Magdy","doi":"10.1093/jaoacint/qsad050","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad050","url":null,"abstract":"<p><strong>Background: </strong>Spectrophotometric resolution of a mixture of several drugs is considered a cheaper, simpler, and more versatile alternative compared to costly chromatographic instruments.</p><p><strong>Objective: </strong>The work aims to resolve the interfering spectra of ephedrine hydrochloride, naphazoline nitrate, and methylparaben in nasal preparations using smart spectrophotometric methods.</p><p><strong>Method: </strong>In our work, derivative and dual-wavelength methods were combined to eliminate this interference, under the name of derivative dual-wavelength method. Other methods, namely successive derivative subtraction and chemometric analysis, were also able to eliminate this interference. The methods have proven their applicability as they follow the International Conference on Harmonization (ICH) requirements regarding repeatability, precision, accuracy, selectivity, and linearity. Eco-scale, GAPI, and AGREE tools were used to estimate the possible environmental effects of the methods.</p><p><strong>Results: </strong>Acceptable results for repeatability, precision, accuracy, selectivity, and linearity were obtained. Limit of detection (LOD) values were 2.2 for ephedrine and 0.3 for naphazoline. The correlation coefficients were above 0.999. The methods were proven to be safe for application.</p><p><strong>Conclusions: </strong>The introduced methods are cheap and easily implemented compared to chromatographic techniques. They can be used in purity-checking of raw material and estimation of concentrations in market formulations. The replacement of the published chromatographic techniques with our developed methods is useful when needing to save money, effort, and time.</p><p><strong>Highlights: </strong>The three components of a decongestant nasal preparation were determined using cheap, green, and versatile spectrophotometric methods that keep the advantages of chromatographic techniques, including accuracy, reproducibility, and selectivity.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10514722","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 Antibacterial Investigation of Linezolid-Loaded SPIONs and HPLC Method Development for Quantitative Analysis of Linezolid.","authors":"Musarrat Husain Warsi,&nbsp;Sharmistha Mohapatra,&nbsp;Mohammed Asfer,&nbsp;Mohammad Yusuf,&nbsp;Abuzer Ali,&nbsp;Mohammad Akhlaquer Rahman,&nbsp;Amena Ali,&nbsp;Abdul Qadir,&nbsp;Gaurav K Jain","doi":"10.1093/jaoacint/qsad071","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad071","url":null,"abstract":"<p><strong>Background: </strong>Linezolid (LNZ) is extremely prone to resistance. The development of resistance to LNZ should be taken into consideration when selecting this drug as a therapeutic option. It is well established that reactive oxygen species (ROS) generated by iron oxide nanoparticles (MNPs) could kill the infecting bacteria. So, we hypothesized the synergistic antibacterial effect of iron oxide nanoparticles and LNZ.</p><p><strong>Objective: </strong>To study the release and antibacterial effects of LNZ-loaded superparamagnetic iron oxide nanoparticles (SPIONs) on Staphylococcus aureus and Streptococcus pneumoniae.</p><p><strong>Method: </strong>Ferrofluid containing SPIONs was synthesized via chemical co-precipitation method and stabilized by sodium lauryl sulphate (SLS). SPIONs were then loaded with LNZ and characterized for particle size, FT-IR, XRD, and entrapment efficiency. Further antibacterial activity of SPIONs and LNZ-loaded SPIONs was investigated. For the in vitro release findings, HPLC analytical method development and validation were performed.</p><p><strong>Results: </strong>Isolation of LNZ was accomplished on a C-18 column with methanol-TBHS (tetra butyl ammonium hydrogen sulphate, 50:50, v/v). The eluate was monitored at 247 nm with a retention time of 4.175 min. The MNP's DLS measurement revealed monodispersed particles with an average size of 16.81 ± 1.07 nm and PDI 0.176 ± 0.012. In optimized formulation, 25 ± 1.75% (w/w) of the drug was found to be entrapped. XRD revealed uniform coating of oleic acid covering the entire magnetic particles' surface with no change in its crystallinity. An effective antimicrobial activity was observed at the lowered dose of drug.</p><p><strong>Conclusions: </strong>A robust HPLC method was developed to quantify the LNZ in MNPs, and outcomes showed that the reduced dose of LNZ incorporated in SPIONs was able to show similar activity as the marketed product.</p><p><strong>Highlights: </strong>Successfully reduction of the dose of LNZ was established with the aid of biocompatible MNPs to attain the equivalent antibacterial activity.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10496654","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 Different Perspective on the Characterization of a New Degradation Product of Flibanserin With HPLC-DAD-ESI-IT-TOF-MSn and Its Pharmaceutical Formulation Analysis With Inter-Laboratory Comparison.","authors":"Aysun Geven,&nbsp;Saniye Özcan,&nbsp;Serkan Levent,&nbsp;Nafiz Öncü Can","doi":"10.1093/jaoacint/qsad074","DOIUrl":"10.1093/jaoacint/qsad074","url":null,"abstract":"<p><strong>Background: </strong>Flibanserin (FLB) was first synthesized as an antidepressant drug; however, due to its enhancing effects on sexual activity, it was approved for treatment of hypoactive sexual desire disorder in women in 2015.</p><p><strong>Objective: </strong>The aim of this study was to develop a new and fully validated HPLC method for analysis of FLB in pharmaceutical formulations besides its degradation products, and identification of possible formation mechanisms by using HPLC-DAD-ESI-IT-TOF-MSn.</p><p><strong>Method: </strong>The HPLC separation was achieved in a Supelco Ascentis® Express series phenyl hexyl column (100 × 4.6 mm, ID 2.7 µm). The mobile phase was acetonitrile-ammonium acetate solution (50:50, v/v, 10 mM, pH 5.4) mixture, which was pumped at the rate of 0.5 mL/min. Chromatography, detection, and structural identification was performed by using a LCMS-IT-TOF instrument (Shimadzu, Japan).</p><p><strong>Results: </strong>1-(2-(4-(3-hydroxy-5-(trifluoromethyl)phenyl)piperazine-1-yl)ethyl)-1,3-dihydro-2H-benzo[d]imidazol-2-one is proposed as a novel degradation product, with a mass of 407.1695 and a formula of C20H21F3N4O2 with a margin of error about 0.001 ppm. The developed method is applicable with 98% accuracy within the 2.5-50.0 µg/mL range. The LOD and LOQ were about 500 ng/mL and 1.50 µg/mL, respectively. The transferability and variation between laboratories were tested by inter-laboratory comparison and evaluated with one-way analysis of variance.</p><p><strong>Conclusions: </strong>A novel FLB degradation product, which was produced under oxidative forced degradation conditions was observed and identified for the first time; in addition, the formation kinetics of the degradation product besides decomposition of FLB was studied. Furthermore, an inter-laboratory comparison was carried out, and application of the proposed method on a pseudo Addyi® (Sprout Pharmaceuticals, Inc.) sample was tested using both instrument configurations.</p><p><strong>Highlights: </strong>A novel stability-indicating assay method was developed and fully validated according to the International Council on Harmonization (Q2) R1 for the analysis of FLB in the pharmaceutical preparations. A new degradation product was identified in the oxidative forced degradation condition and characterized using HPLC-DAD-ESI-IT-TOF-MS3. Moreover, the possible mechanism and the formation kinetic of the degradation product were revealed. In addition, the developed method was transferred to another LC-PDA instrument for inter-laboratory comparison. Finally, the current method was applied to a pseudo formulation of Addy in both instruments, and ANOVA was applied for evaluation.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10560319/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10218304","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Application of Rapid Identification and Determination of Moisture Content of Coptidis Rhizoma From Different Species Based on Data Fusion.","authors":"Mengyin Tian,&nbsp;Xiaobo Ma,&nbsp;Mengying Liang,&nbsp;Hengchang Zang","doi":"10.1093/jaoacint/qsad058","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad058","url":null,"abstract":"BACKGROUND\u0000For thousands of years, Traditional Chinese Medicine (TCM) has been clinically proven, and doctors have highly valued the differences in utility between different species.\u0000\u0000\u0000OBJECTIVE\u0000This study aims to replace the complex methods traditionally used for empirical identification by compensating for the information loss of a single sensor through data fusion. The research object of the study is Coptidis Rhizome (CR).\u0000\u0000\u0000METHODS\u0000Using spectral optimization and data fusion technology, Near Infrared (NIR) and Mid-Infrared (MIR) spectra were collected for CR. PLS-DA (n = 134) and PLSR (n = 63) models were established to identify the medicinal materials and determine the moisture content in the medicinal materials.\u0000\u0000\u0000RESULTS\u0000For the identification of the three species of CR, the mid-level fusion model performed better than the single-spectrum model. The sensitivity and specificity of the prediction set coefficients for NIR, MIR, and data fusion qualitative models were all higher than 0.95, with an AUC value of 1. The NIR data model was superior to the MIR data model. The results of low-level fusion were similar to those of the NIR optimization model. The RPD of the test set of NIR and low-level fusion model was 3.6420 and 3.4216, respectively, indicating good prediction ability of the model.\u0000\u0000\u0000CONCLUSION\u0000Data fusion technology using NIR and MIR can be applied to identify CR species and determine the moisture content of CR. It provides technical support for the rapid determination of moisture content, with fast analysis speed and without the need for complex pretreatment methods.\u0000\u0000\u0000HIGHLIGHTS\u0000This study is the first to introduce spectral data fusion technology to identify CR species. Data fusion technology is feasible for multivariable calibration model performance and reduces the cost of manual identification. The moisture content of CR can be quickly evaluated, reducing the difficulty of traditional methods.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10496148","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}