S K Amir Soyel, Dipak Kumar Hazra, Subhajit Ruidas, Swagata Mandal, Sudip Bhattacharyya, Rajlakshmi Poi, Rajib Karmakar, Goutam Mondal, Sujan Majumder, Prithusayak Mondal
{"title":"Simultaneous Monitoring and Decontamination of Pesticide Residues in Phytomedicine-Enriched Betel Leaf Utilizing QuEChERS-GC-MS/MS Technology to Safeguard Public Health.","authors":"S K Amir Soyel, Dipak Kumar Hazra, Subhajit Ruidas, Swagata Mandal, Sudip Bhattacharyya, Rajlakshmi Poi, Rajib Karmakar, Goutam Mondal, Sujan Majumder, Prithusayak Mondal","doi":"10.1093/jaoacint/qsad005","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad005","url":null,"abstract":"<p><strong>Background: </strong>The presence of undesirable substances, including pesticides (xenobiotics) in betel leaf (Piper betel), is a great concern for consumers because it is chewed and consumed directly. To protect the consumer's health, a modified QuEChERS method for monitoring purposes and subsequent decontamination process has been developed.</p><p><strong>Objective: </strong>The goal of this work was to establish a multi-residue analytical method for monitoring nonpermitted organophosphorus pesticide residues in betel leaf, as well as cost-effective cleaning strategies.</p><p><strong>Method: </strong>The homogenized 15 g samples (20 betel leaf samples collected in West Bengal, India) were extracted with a modified QuEChERS method using acetonitrile, reconstituted to acetone, and finally analyzed by GC-MS/MS. Possible decontamination techniques (such as tap water washing, 2% saltwater washing, and lukewarm water washing) were evaluated.</p><p><strong>Results: </strong>The limit of detection ranged from 0.003 to 0.005 mg/kg, and limit of quantification was 0.01 mg/kg. Recoveries ranged from 80 to 120% with RSDr 9%. One sample was found to contain three pesticides 4 to 7 times higher than MRLs. Suggested decontamination methods allowed reducing toxic traces below European limits.</p><p><strong>Conclusions: </strong>The suggested approach is useful for determining pesticide residues in betel leaves quickly. Traditional techniques of processing betel leaves may reduce pesticide residues below regulatory limits.</p><p><strong>Highlights: </strong>A multi-residue method and decontamination of pesticides in betel leaf using QuEChERS-GC-MS/MS technology with satisfactory method performance was achieved. Domestic decontamination techniques have a high efficacy in reducing pesticide residues from betel leaves, making them safe for human consumption.</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":"10514170","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":"Authentication of Platycladus Orientalis Leaves and Its Five Adulterants by Combination of Morphology and Microscopic Characteristics, TLC, and HPLC Analysis.","authors":"Jin-Hua Hao, Ping-Ting Xiao, Peng-Bo Duan, Dan-Yang Miao, Xiao-Yu Jiang, Yu-Jia Kuang, E-Hu Liu","doi":"10.1093/jaoacint/qsad066","DOIUrl":"10.1093/jaoacint/qsad066","url":null,"abstract":"<p><strong>Background: </strong>Platycladus orientalis leaves (POL), as the source of the traditional Chinese medicine (TCM) Platycladi Cacumen, has frequently been found to be misused with five adulterants including Chamaecyparis obtusa leaves (COL), Cupressus funebris leaves (CFL), Juniperus virginiana leaves (JVL), Sabina chinensis leaves (SCL), and Juniperus formosana leaves (JFL).</p><p><strong>Objective: </strong>The purpose of this study was to distinguish POL (fresh leaves) from its five adulterants (fresh leaves).</p><p><strong>Methods: </strong>The micromorphological features in terms of transection and microscopic characteristics of POL and adulterants were captured and compared using the an microscope. Both HPLC and TLC methods for the simultaneous determination of six bioactive flavonoids (myricitrin, isoquercitrin, quercitrin, amentoflavone, afzelin, and hinokiflavone) have been developed.</p><p><strong>Results: </strong>There were significant differences in microscopic features of transverse section and powders. The TLC results suggested that the spots of myricitrin in POL were more obvious than those in the five adulterants. The contents of myricitrin and quercitrin, or the total content of flavonoids in POL, determined by HPLC, were significantly higher than those in the adulterants.</p><p><strong>Conclusion: </strong>POL was successfully distinguished from its five adulterants by the comparison of morphology, microscopic characteristics, and chemical profiles.</p><p><strong>Highlights: </strong>This research provides a comprehensive morphology, microscopic identification, TLC, and HPLC analysis for authenticating POL and its five adulterants.</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":"10125642","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}
Anil Kumar Saini, Sultan Zahiruddin, Kakumani Godwin Newton, Laxman Sawant, Ranjan Mitra, Rajiva Kumar Rai, Sayeed Ahmad
{"title":"Validation and Standardization of Gallic Acid and Ellagic Acid in Quercus Infectoria, Terminalia Chebula, and Pistacia Integerrima.","authors":"Anil Kumar Saini, Sultan Zahiruddin, Kakumani Godwin Newton, Laxman Sawant, Ranjan Mitra, Rajiva Kumar Rai, Sayeed Ahmad","doi":"10.1093/jaoacint/qsad070","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad070","url":null,"abstract":"<p><strong>Background: </strong>Due to its medicinal properties, Pistacia integerrima is in high demand and is extensively used as a key ingredient in various formulations. However, its popularity has led to its inclusion on the International Union for Conservation of Nature threatened category list. In Ayurvedic texts, such as Bhaishajaya Ratnavali, Quercus infectoria is recommended as a substitute for P. integerrima in different formulations. Additionally, Yogratnakar highlights that Terminalia chebula shares similar therapeutic properties with P. integerrima.</p><p><strong>Objective: </strong>The objective of the current study was to gather scientific data on metabolite profiling and marker-based comparative analysis of Q. infectoria, T. chebula, and P. integerrima.</p><p><strong>Methods: </strong>In present study, hydroalcoholic and aqueous extracts of all three plants were prepared and standardized for the comparative evaluation of secondary metabolites. TLC was carried out for the comparative fingerprinting of the extracts using chloroform-methanol-glacial acetic acid-water (60 + 8 + 32 + 10, by volume) as a solvent system. A fast, sensitive, selective, and robust HPLC method was developed to determine gallic acid and ellagic acid from both extracts of all three plants. The method was validated for precision, robustness, accuracy, LOD and LOQ as per the International Conference on Harmonization guidelines.</p><p><strong>Results: </strong>The TLC analysis revealed the presence of several metabolites, and the pattern of metabolites in the plants exhibited a certain degree of similarity. A highly precise and reliable quantification technique was created for gallic acid and ellagic acid, operating within a linear concentration range of 81.18-288.22 µg/mL and 3.83-13.66 µg/mL, respectively. The correlation coefficients for gallic acid and ellagic acid were 0.997 and 0.996, indicating good linear relationships. The gallic acid content in all three plants ranged from 3.74 to 10.16% w/w, while the ellagic acid content ranged from 0.10 to 1.24% w/w.</p><p><strong>Conclusion: </strong>The study contributes to the scientific understanding of the metabolite profiles and comparative analysis of Q. infectoria, T. chebula, and P. integerrima. The findings provide valuable insights into the chemical composition of these plants and can be used for various applications in herbal medicine.</p><p><strong>Highlights: </strong>This pioneering scientific approach highlights the phytochemical similarities between Q. infectoria, T. chebula and P. integerrima.</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":"10133023","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Development of Recombinase Aided Amplification (RAA)-Exo-Probe Assay for the Rapid Detection of Shiga Toxin-Producing Escherichia coli.","authors":"Yuhao Cao, Taisong Fang, Jinling Shen, Guodong Zhang, Dehua Guo, Lina Zhao, Yuan Jiang, Shuai Zhi, Lin Zheng, Xiaofei Lv, Zhiyuan Yao, Daniel Yu","doi":"10.1093/jaoacint/qsad063","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad063","url":null,"abstract":"BACKGROUND\u0000Shiga toxin-producing Escherichia coli (STEC) is a significant cause of foodborne illness causing various gastrointestinal diseases including hemolytic uremic syndrome (HUS), the most severe form, which can lead to kidney failure or even death.\u0000\u0000\u0000OBJECTIVE\u0000Here, we report the development of RAA (Recombinase Aided Amplification)-exo-probe assays targeting the stx1 and stx2 genes for the rapid detection of STEC in food samples.\u0000\u0000\u0000RESULTS\u0000These assays were found to be 100% specific to STEC strains and were also highly sensitive with a detection limit of 1.6 × 103 CFU/mL or 32 copies/reaction. Importantly, the assays were able to successfully detect STEC in spiked and real food samples (beef, mutton, and pork), with a detection limit as low as 0.35 CFU/25g in beef samples after an overnight enrichment step.\u0000\u0000\u0000CONCLUSION\u0000Overall, the RAA assay reactions completed within ∼20 minutes and were less dependent on expensive equipment, suggesting they can be easily adopted for in field testing requiring only a fluorescent reader.\u0000\u0000\u0000HIGHLIGHTS\u0000As such, we have developed two rapid, sensitive, and specific assays that can be used for the routine monitoring of STEC contamination in food samples, particularly in the field or in poorly equipped labs.","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":"10141700","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}
Ragaa Magdy, Nermine V Fares, Maha Farouk, Ahmed Hemdan
{"title":"A Novel, Sustainable, and Eco-Friendly Spectrophotometric and Chemometric Approach for Determination of Severely Overlapped Spectrum via Unified Regression Equation: Greenness and Whiteness Assessment.","authors":"Ragaa Magdy, Nermine V Fares, Maha Farouk, Ahmed Hemdan","doi":"10.1093/jaoacint/qsad037","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad037","url":null,"abstract":"<p><strong>Background: </strong>Nebivolol and valsartan (VAL) in combination with each other successfully control blood pressure and improve hypertension patient outcomes.</p><p><strong>Objective: </strong>To develop and validate innovative, simple, and sustainable spectrophotometric methods for the simultaneous analysis of nebivolol and valsartan.</p><p><strong>Method: </strong>The new modified difference amplitude modulation (MD-AM) method uses only unified regression equation and does not require any resolution techniques. Other different approaches were also applied for the determination of the same mixture including univariate and multivariate spectrophotometric methods. The multivariate methods were PLS and PCR, whereas the univariate methods were derivative ratio (DD1), ratio difference (RD), constant center (CC), constant center spectrum subtraction (CC-SS), constant value coupled with amplitude difference (CV-AD), advanced concentration value (ACV), and amplitude difference (AD). The proposed methods use a green solvent; thus, the environmental impact of the presented procedures was evaluated qualitatively and quantitatively using six well-known evaluation tools.</p><p><strong>Results: </strong>All methods were applied successfully for the analysis of the studied drugs in their bulk powder, pharmaceutical dosage form Byvalson®, and in vitro release at intestinal pH (7.4) using a USP dissolution tester. Results obtained were compared statistically with the reported method and with each other using a one-way ANOVA statistical test, and no significant differences were found.</p><p><strong>Conclusions: </strong>All green and white analytical chemistry evaluation tools results confirm the safety, sustainability, and cost-effectiveness of the approaches, indicating that the methods are regarded green and sustainable. Results were agreeable, encouraging their applicability in quality control laboratories for dosage form and making these methods an eco-friendly substitute for the analysis of this combined dosage form and for evaluating the dissolution profile.</p><p><strong>Highlights: </strong>For the first time, a severely overlapped spectrum was determined using a unified regression equation without the need of extended part or zero contribution regions by the novel method MD-AM. The proposed methods are the first study of in vitro dissolution profiling of nebivolol hydrochloride (NEB) and VAL and the first sustainable and green methods applied without compromising the analytical criteria.</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":"10197810","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}
Pintu Prajapati, Veera Shakar Pulusu, Shailesh Shah
{"title":"Red, Green, and Blue Model-Based Assessment and Principles of White Analytical Chemistry to Robust Stability-Indicating Chromatographic Estimation of Thiocolchicoside and Diclofenac Sodium.","authors":"Pintu Prajapati, Veera Shakar Pulusu, Shailesh Shah","doi":"10.1093/jaoacint/qsad052","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad052","url":null,"abstract":"<p><strong>Background: </strong>White analytical chemistry (WAC) is a recent approach for evaluating analytical procedures based on their effectiveness in validating results, capacity to be environmentally friendly, and economic effectiveness.</p><p><strong>Objective: </strong>The detection of diclofenac sodium (DCF) and thiocolchicoside (THC) simultaneously has been established using a WAC-driven stability-indicating chromatographic method (SICM).</p><p><strong>Methods: </strong>For the concurrent stability study of THC and DCF, the suggested chromatographic technique was developed employing safe and environmentally acceptable organic solvents. To identify critical analytical method parameters (AMPs) and analytical quality attributes (AQAs), a design of experiments (DoE)-based screening design was applied. For the DoE-based response surface modelling (RSM) of critical AMPs and AQAs, the Box-Behnken design (BBD) was employed.</p><p><strong>Results: </strong>A robust SICM was developed by navigating the analytical design space for simultaneous estimation of THC and DCF. IR, NMR, and mass spectral data were used to characterize the degradation products. Red, green, and blue (RGB) models were used to evaluate the suggested method's validation effectiveness, greenness power, and economic efficiency and compared to published chromatographic techniques. The effectiveness of the chromatographic method's validation concerning the International Council for Harmonization (ICH) Q2 (R1) guideline was evaluated using the red model. The analytical greenness (AGREE) evaluation tool and eco-scale assessment (ESA) approach were used to evaluate the green model's methodology. The blue model-based assessment was carried out for comparison of simplicity of instruments handling, cost, and time during sample analysis. The red, blue, and green scores of the techniques were averaged to arrive at the white score of the suggested and reported methods.</p><p><strong>Conclusion: </strong>For the concurrent stability study of THC and DCF, the suggested technique was shown to be validated, environmentally friendly, and cost effective. The suggested approach could be a cost-effective and environmentally friendly analytical technique for determining the stability and monitoring the quality of fixed-dose combinations (FDC) of THC and DCF.</p><p><strong>Highlights: </strong>Stability-indicating HPTLC method was developed for concomitant analysis of THC and DCF using concepts of DoE and WAC.</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":"10197854","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":"Improved Stability-Indicating RP-UPLC Method for the Levamisole Hydrochloride Assay and Estimation of Its Related Compounds.","authors":"Sarju Adhikari, Abu M Rustum","doi":"10.1093/jaoacint/qsad035","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad035","url":null,"abstract":"<p><strong>Background: </strong>Levamisole hydrochloride (LVM) is an anthelmintic drug substance with immunomodulatory and anticancer activities. LVM has also found usage as a cutting agent in street cocaine.</p><p><strong>Objective: </strong>This study was aimed to develop and validate an alternative and improved stability-indicating reversed-phase ultraperformance liquid chromatography (RP-UPLC) method for the determination of LVM and the estimation of its related compounds.</p><p><strong>Method: </strong>The UPLC method for the assay was optimized in terms of organic solvents consumed, pH, column temperature, and flow rate. Determination of LVM and its related compounds was performed using a gradient elution on a Waters ACQUITY UPLC® BEH C18 (50 mm × 2.1 mm i.d., 130 Å). The column temperature was maintained at 35°C. Mobile phase A was composed of aqueous 5 mM ammonium hydroxide, and mobile phase B was composed of acetonitrile. All the analytes were monitored by UV detection at 215 nm with a flow rate of 0.7 mL/min. The total runtime of the method with column equilibration is 4.0 min.</p><p><strong>Results: </strong>The developed method met all the acceptance criteria of the current International Council for Harmonization [ICH Q2 (R1)] guidelines. The method was tested in terms of specificity, linearity (R2 > 0.999), limit of detection (LOD; 0.06 μg/mL), limit of quantitation (LOQ; 0.2 μg/mL), accuracy, precision, and robustness. With a short analysis time (<2.5 min) and reduced consumption of organic solvents, the proposed method is considered a greener alternative to conventional chromatographic methods.</p><p><strong>Conclusions: </strong>An alternative and improved UPLC method was successfully developed and validated in accordance with the ICH guidelines for the determination of LVM and the estimation of its related compounds.</p><p><strong>Highlights: </strong>Due to its high degree of selectivity, speed, and accuracy, the developed method can significantly benefit the end-users with laboratory efficiency and throughput during routine analysis of production batches and stability monitoring of LVM-related drug products.</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":"10514686","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":"Analysis of Taurine in Infant Formulas and Adult Nutritionals by Hydrophilic Interaction Liquid Chromatography-Mass Spectrometry: First Action 2022.03.","authors":"Brendon D Gill, Jackie E Wood","doi":"10.1093/jaoacint/qsad079","DOIUrl":"10.1093/jaoacint/qsad079","url":null,"abstract":"<p><strong>Background: </strong>Taurine is recognized as an essential growth factor and as being critical in the maintenance of functional tissue regulation.</p><p><strong>Objective: </strong>To evaluate the analytical performance of a hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS) method for compliance with AOAC Standard Method Performance Requirements (SMPR®) for taurine analysis described in SMPR 2014.013.</p><p><strong>Method: </strong>Following protein precipitation with Carrez solutions, taurine is extracted and separated by HILIC with detection by triple quadrupole MS using multiple reaction monitoring (MRM). Stable isotope labeled (SIL) taurine internal standard is used for quantification to correct for losses in extraction and variations in ionization in the ion source.</p><p><strong>Results: </strong>The method was shown to meet the requirements specified in the SMPR with a linear range of 0.27-2700 mg/hg RTF (ready-to-feed), a limit of detection of 0.14 mg/hg RTF, acceptable recovery of 97.2-100.1%, and acceptable repeatability of 1.6-6.4% relative standard deviation. Additionally, the method was found to have no statistically significant bias compared with reference values for National Institute of Standards and Technology (NIST) 1849a certified reference material (CRM) (P-value = 0.95) and 1869 CRM (P-value = 0.31), and with results from AOAC 997.05 (P-value = 0.10).</p><p><strong>Conclusions: </strong>A recent review of the method and validation data by the Stakeholder Program on Infant Formula and Adult Nutritionals (SPIFAN) Expert Review Panel (ERP) found that this method met all the criteria for analysis of taurine specified in SMPR 2014.013 and voted to adopt this method as First Action AOAC Official MethodSM2022.03.</p><p><strong>Highlights: </strong>A method for the analysis of taurine in infant formulas and adult nutritionals by HILIC-MS/MS is described. A single-laboratory validation (SLV) study demonstrated the applicability of the method to meet requirements of SMPR 2014.013. In December 2022, the SPIFAN ERP voted to adopt this method as First Action AOAC Official Method 2022.03.</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":"10480300","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}
Jia-Jia Zou, Xiao-Li Xu, Lin Yang, Yi-Wu Wang, Yan Li, Lei Dai, Dan He
{"title":"Comprehensive Quality Evaluation of Qizhi Xiangfu Pills Based on Quantitative Analysis of Multi-Components by a Single Marker Combined with GC Fingerprints and Chemometrics.","authors":"Jia-Jia Zou, Xiao-Li Xu, Lin Yang, Yi-Wu Wang, Yan Li, Lei Dai, Dan He","doi":"10.1093/jaoacint/qsad043","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad043","url":null,"abstract":"<p><strong>Background: </strong>Qizhi Xiangfu Pills (QXPs) are a traditional Chinese medicine (TCM) used clinically for qi stagnation and blood stasis. The current quality control of QXPs in the ministry standards and the reported literature is minimal, and requires improvement.</p><p><strong>Objective: </strong>This study aimed to analyze and determine the active ingredients in QXPs for its overall evaluation.</p><p><strong>Methods: </strong>In this study, a quantitative analysis of multi-components by a single marker (QAMS) method was established to simultaneously determine caryophyllene oxide, cyperotundone, ligustilide, and α-cyperone in QXPs by GC. Moreover, the GC fingerprints of 22 batches of samples were also established, and the common peaks were initially identified by GC-MS, then classified in various dimensions using chemometric methods, and the main markers causing the discrepancies between groups were analyzed by orthogonal partial least-squares discrimination analysis (OPLS-DA).</p><p><strong>Results: </strong>Compared with an internal standard method (ISM), the determination results obtained by QAMS had no significant difference. Twenty-two common peaks were distinguished in the fingerprint of 22 batches of QXPs, 17 of which were identified, and the similarity of the fingerprints was greater than 0.898. The 22 batches of QXPs were roughly divided into 3 categories, and 12 main markers causing the discrepancies were discovered.</p><p><strong>Conclusion: </strong>The established QAMS method combined with the GC fingerprint and chemometrics is convenient and feasible, which helps to improve the quality evaluation of QXPs and provides a demonstration for the related study of compound preparations and single herbs.</p><p><strong>Highlights: </strong>QAMS combined with a GC fingerprint and chemometrics method was established to evaluate the quality of QXPs for the first time.</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":"10495653","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 Thermo Scientific™ SureTect™ Vibrio cholerae, Vibrio parahaemolyticus, and Vibrio vulnificus PCR Assay for the Detection of Vibrio cholerae, Vibrio parahaemolyticus, and Vibrio vulnificus in Seafood Matrixes: AOAC Performance Tested MethodsSM 022301.","authors":"Nikki Faulds, Jessica Williams, Katharine Evans, Annette Hughes, Dean Leak, David Crabtree, Nicole Prentice, Daniele Sohier, Pauliina Heikkinen, Emmi Hurskainen, Wendy McMahon, Nicole Cuthbert, Bailey Matthews, Lydia Ruben, Luvie Sturghill, Frank Godawski","doi":"10.1093/jaoacint/qsad061","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad061","url":null,"abstract":"<p><strong>Background: </strong>The Thermo Scientific™ SureTect™ Vibrio cholerae, Vibrio parahaemolyticus, and Vibrio vulnificus PCR Assay method is a real-time PCR method for the multiplex detection of Vibrio cholerae, Vibrio parahaemolyticus, and Vibrio vulnificus in seafood.</p><p><strong>Objective: </strong>The Thermo Scientific SureTect Vibrio cholerae, Vibrio parahaemolyticus, and Vibrio vulnificus Assay was evaluated for AOAC Performance Tested MethodsSM certification.</p><p><strong>Method: </strong>Inclusivity/exclusivity, matrix, product consistency/stability, and robustness studies were conducted to assess the method's performance. For the matrix study, the method was validated using the Applied Biosystems™ QuantStudio™ 5 Real-Time PCR Food Safety Instrument and the Applied Biosystems™ 7500 Fast Real-Time PCR Food Safety Instrument against the U.S. Food and Drug Administration Bacteriological Analytical Manual, Chapter 9 (2004), Vibrio and ISO 21872-1:2017 Microbiology of the food chain-Horizontal method for the determination of Vibrio spp.-Part 1: Detection of potentially enteropathogenic Vibrio parahaemolyticus, Vibrio cholerae, and Vibrio vulnificus reference methods.</p><p><strong>Results: </strong>Matrix studies showed equivalent or superior performance of the candidate method compared to the reference method and, overall, no difference between presumptive and confirmed results, except for one matrix due to high background flora. The inclusivity/exclusivity study correctly identified/excluded all strains analyzed. Robustness testing showed no statistically significant differences in assay performance under varied test conditions. Product consistency and stability studies demonstrated no statistically significant differences between assay lots with different expiration dates.</p><p><strong>Conclusions: </strong>The data presented show that the assay constitutes a rapid and reliable workflow for the detection of V. cholerae, V. parahaemolyticus, and V. vulnificus in seafood matrixes.</p><p><strong>Highlights: </strong>The SureTect PCR Assay method allows for fast, reliable detection of stipulated strains in seafood matrixes with results obtained in as little as 80 min post-enrichment.</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://ftp.ncbi.nlm.nih.gov/pub/pmc/oa_pdf/00/f8/qsad061.PMC10472736.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10149482","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}