Accreditation and Quality Assurance最新文献

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Development of pure manganese flake reference material for X-ray energy/wave dispersive spectrometer calibration x射线能量/波色散光谱仪标定用纯锰片标准物质的研制
IF 1 4区 工程技术
Accreditation and Quality Assurance Pub Date : 2025-08-18 DOI: 10.1007/s00769-025-01667-5
Donghui Tian, Tao Song, Zhigang Wang, Yaling Chen, Gang Hu, Xu Li, Fang Cheng, Cheng Pu
{"title":"Development of pure manganese flake reference material for X-ray energy/wave dispersive spectrometer calibration","authors":"Donghui Tian,&nbsp;Tao Song,&nbsp;Zhigang Wang,&nbsp;Yaling Chen,&nbsp;Gang Hu,&nbsp;Xu Li,&nbsp;Fang Cheng,&nbsp;Cheng Pu","doi":"10.1007/s00769-025-01667-5","DOIUrl":"10.1007/s00769-025-01667-5","url":null,"abstract":"<div><p>Reference material is of great significance to the measurement accuracy of X-ray energy/wave dispersive spectrometer (EDS/WDS). In this work a reference material of manganese (Mn) content (mass fraction, %) of pure Mn flake for EDS/WDS calibration was developed. The surfaces of Mn flakes were finely treated by mechanical grinding and argon ion polishing, and the Mn flakes with high cleanliness and low roughness were obtained. The homogeneity and stability of Mn content of the Mn flakes were analyzed carefully using electron probe micro-analyzer (EPMA). The Mn content of the reference material was determined using inductively coupled plasma optical emission spectrometer (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS). The sources of uncertainty components of Mn reference material were fully analyzed and evaluated. The results show that the homogeneity of the pure Mn flake reference material meet the requirements. The Mn content of the vacuum-packed pure Mn flake is stable for up to one year at ambient temperature. The Mn content reference material of the pure Mn flake reference material is 99.5 %, and its expanded uncertainty is 0.9 % (<i>k</i> = 2). The pure Mn flake reference material can meet the calibration requirements of X-ray EDS/WDS, and guarantee the accuracy and consistency of measurement results. The content of this study complies with the definition of reference materials in ISO 17034 and can be used to calibrate measurement systems. The Mn content reference material can be widely used for element measurement in the fields of scientific research, manufacturing and trade activities.</p><h3>Graphical abstract</h3>\u0000<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":454,"journal":{"name":"Accreditation and Quality Assurance","volume":"30 5","pages":"531 - 542"},"PeriodicalIF":1.0,"publicationDate":"2025-08-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145073626","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Robustness comparison of three statistical methods commonly used in Proficiency Tests 能力测试常用三种统计方法的稳健性比较
IF 1 4区 工程技术
Accreditation and Quality Assurance Pub Date : 2025-07-24 DOI: 10.1007/s00769-025-01669-3
Willem P. Cofino, Steven Crum, Winnie van Vark, Jaap Molenaar
{"title":"Robustness comparison of three statistical methods commonly used in Proficiency Tests","authors":"Willem P. Cofino,&nbsp;Steven Crum,&nbsp;Winnie van Vark,&nbsp;Jaap Molenaar","doi":"10.1007/s00769-025-01669-3","DOIUrl":"10.1007/s00769-025-01669-3","url":null,"abstract":"&lt;div&gt;&lt;p&gt;This study compares the Algorithm A and Q/Hampel methods outlined in ISO 13528, and the NDA method utilized within the WEPAL/Quasimeme PT schemes, as far as robustness to outliers is concerned. The comparison starts with an analysis of Empirical Influence Functions. This analysis shows that NDA applies the strongest down-weighting to outliers, followed by Q/Hampel and Algorithm A, respectively. Second, we evaluated the methods using simulated datasets.. Stylized datasets using a normal distribution N(1,1) with 30 and 200 data were contaminated with 5%-45% data drawn from 32 different distributions. NDA consistently produced mean estimates closest to the true values, while Algorithm A showed the largest deviations. The percentage differences between the mean estimates of Q/Hampel and Algorithm A relative to NDA turned out to be linearly proportional to the L-skewness of the dataset within a substantial interval around L-skewness = 0. Third, the relationship between percentual differences between the mean estimates and L-skewness was analysed for over 33,000 datasets from WEPAL/Quasimeme. The linear relationships observed in the simulation study were reproduced. The percentual differences between the mean estimates were projected onto L-moment diagrams, stratified by sample size. Across the four classes discerned, the results exhibit consistent and interpretable patterns. The three methods showed similar robustness to tail weight (L-kurtosis), but NDA was markedly more robust to asymmetry, particularly in smaller samples. The three methods yield estimates that differ by less than 2% when L-skewness approaches zero. The findings demonstrate that NDA has a higher robustness than Q/Hampel and Algorithm A. NDA exhibits a lower efficiency (~ 78%) compared to Q/Hampel and Algorithm A (both ~ 96%). Our analysis clearly shows the robustness versus efficiency trade-off that is typical for this kind of statistical methods. We recommend PT organizers to assess this trade-off in the light of the distributional characteristics of their datasets and, if necessary, adapt the selection or parametrization of the statistical methodology. For the WEPAL-Quasimeme scheme, the emphasis put by the NDA method on robustness is an advantage given the characteristics of the datasets usually analysed in this scheme. In addition to mean estimation, our study also evaluates the behaviour of the standard deviation of the estimates generated by Q&lt;sub&gt;n&lt;/sub&gt;, Q/Hampel, Algorithm A, and NDA. Q&lt;sub&gt;n&lt;/sub&gt; and Q/Hampel produced similar results in datasets with larger sample sizes (&lt;i&gt;N&lt;/i&gt; &gt; 16). Q/Hampel produced higher estimates in smaller datasets. Algorithm A provided estimates consistent with the other methods for near-Gaussian datasets, but higher estimates for higher contamination levels. NDA’s standard deviation estimates were generally in agreement with those of Q/Hampel and Q&lt;sub&gt;n&lt;/sub&gt;, but consistently lower for leptokurtic distributions. This behaviour is a","PeriodicalId":454,"journal":{"name":"Accreditation and Quality Assurance","volume":"30 5","pages":"507 - 519"},"PeriodicalIF":1.0,"publicationDate":"2025-07-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s00769-025-01669-3.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145073635","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
The updated mise en pratique for the definition of the mole 更新后的摩尔定义公式
IF 1 4区 工程技术
Accreditation and Quality Assurance Pub Date : 2025-07-24 DOI: 10.1007/s00769-025-01668-4
Richard J. C. Brown
{"title":"The updated mise en pratique for the definition of the mole","authors":"Richard J. C. Brown","doi":"10.1007/s00769-025-01668-4","DOIUrl":"10.1007/s00769-025-01668-4","url":null,"abstract":"<div><p>The important role of the <i>mises en pratique</i>, or practical realisations for the definition of units, in the International System of Units (SI) is often overlooked. This short letter explains their significance together with the historical evolution and recent update of the <i>mise en pratique</i> for the definition of the mole. The features and changes in the most recent version that are significant and of interest for the chemical metrology community are discussed in more detail.</p></div>","PeriodicalId":454,"journal":{"name":"Accreditation and Quality Assurance","volume":"30 5","pages":"489 - 492"},"PeriodicalIF":1.0,"publicationDate":"2025-07-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145073791","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Quality control charts for short or long runs without a training phase. Final part. Performances in the presence of a gradual increase in the mean and slightly autocorrelated data 没有训练阶段的短跑或长跑的质量控制图。最后一部分。表现在平均值逐渐增加和数据略有自相关的情况下
IF 1 4区 工程技术
Accreditation and Quality Assurance Pub Date : 2025-07-15 DOI: 10.1007/s00769-025-01666-6
Manuel Alvarez-Prieto, Ricardo Páez-Montero
{"title":"Quality control charts for short or long runs without a training phase. Final part. Performances in the presence of a gradual increase in the mean and slightly autocorrelated data","authors":"Manuel Alvarez-Prieto,&nbsp;Ricardo Páez-Montero","doi":"10.1007/s00769-025-01666-6","DOIUrl":"10.1007/s00769-025-01666-6","url":null,"abstract":"<div><p>Sometimes analytical laboratories receive requests with a small number of determinations and/or samples, or outside the typical scope of analytical services offered. As a result, they may not have previous data on performance of analytical processes and/or appropriate reference materials. Under these conditions, it is difficult or uneconomical to use classic quality control charts. This is the so-called start-up problem of these control charts. The Quesenberry’s Q charts are appropriated in these situations because they do not require a prior training. This experimental study of Q charts for individual measurements was performed on quality control data for the evaluation of mass fraction of Cr<sub>2</sub>O<sub>3</sub> and Fe in a serpentinite CRM by ICP-OES. The performance of Q charts is discussed when the analytical process presented a gradual increase in the process mean and in the presence of a slight autocorrelation in the raw data. In the first situation, the performances of Q charts for the mean were consistent with the performance of the classical chart for individual measurements, and their sensitivities were comparable. In the second situation, Q charts for the mean also showed a similar response when compared with the chart for individual measurements. They were able to detect the unusual pattern due to autocorrelation in both the short and the long runs. Recommendations on the application of classic and Q charts in the presence of autocorrelation are given. Some other general conclusions about the advantages and disadvantages of Q charts are offered.</p></div>","PeriodicalId":454,"journal":{"name":"Accreditation and Quality Assurance","volume":"30 5","pages":"521 - 529"},"PeriodicalIF":1.0,"publicationDate":"2025-07-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145073804","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Evaluating the measurement uncertainty in determination of eugenol content in cloves by gas chromatography 气相色谱法测定丁香酚含量的测量不确定度评定
IF 1 4区 工程技术
Accreditation and Quality Assurance Pub Date : 2025-07-11 DOI: 10.1007/s00769-025-01659-5
Dalin Chann, Sophany Ret, Chun Li, Xinxin Ding, Meng Liang
{"title":"Evaluating the measurement uncertainty in determination of eugenol content in cloves by gas chromatography","authors":"Dalin Chann,&nbsp;Sophany Ret,&nbsp;Chun Li,&nbsp;Xinxin Ding,&nbsp;Meng Liang","doi":"10.1007/s00769-025-01659-5","DOIUrl":"10.1007/s00769-025-01659-5","url":null,"abstract":"<div><p>Cloves (Syzygium aromaticum) are valued for their high eugenol content, necessitating accurate quantification for quality control. This study determined eugenol in a commercial clove sample using Gas Chromatography with Flame Ionization Detection, employing methyl salicylate as an internal standard following the Chinese Pharmacopoeia 2015 methodology. A comprehensive evaluation of the measurement uncertainty associated with this determination was performed according to the Guide to the Expression of Uncertainty in Measurement and EURACHEM/CITAC guidelines. Major potential uncertainty sources, including the relative correction factor, peak areas (analyte and internal standard), sample volume, internal standard concentration, sample mass, and repeatability, were identified and quantified. The average eugenol content was found to be 17.91% m/m. The eugenol content met the threshold required by the Chinese Pharmacopoeia (which mandates not less than 11.0% m/m) and confirmed the suitability of the commercial product for medicinal use. The combined relative standard uncertainty was calculated as 0.199, leading to an expanded uncertainty of 7.12% (coverage factor <i>k</i> = 2), corresponding to an absolute uncertainty of ± 1.28% m/m eugenol content (or ± 12.8 mg/g). The primary contributors to the overall uncertainty were identified as the peak area of the internal standard and method repeatability, validating the method's reliability for quality control purposes within the established uncertainty limits.</p></div>","PeriodicalId":454,"journal":{"name":"Accreditation and Quality Assurance","volume":"30 5","pages":"543 - 552"},"PeriodicalIF":1.0,"publicationDate":"2025-07-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145073552","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Evaluating the measurement uncertainty in content determination of paracetamol granules by ultraviolet spectrophotometry 紫外分光光度法测定对乙酰氨基酚颗粒含量的不确定度评定
IF 1 4区 工程技术
Accreditation and Quality Assurance Pub Date : 2025-07-11 DOI: 10.1007/s00769-025-01664-8
Dalin Chann, Sophany Ret, Weicun Li, Chun Li, Jingru Qin
{"title":"Evaluating the measurement uncertainty in content determination of paracetamol granules by ultraviolet spectrophotometry","authors":"Dalin Chann,&nbsp;Sophany Ret,&nbsp;Weicun Li,&nbsp;Chun Li,&nbsp;Jingru Qin","doi":"10.1007/s00769-025-01664-8","DOIUrl":"10.1007/s00769-025-01664-8","url":null,"abstract":"<div><p>An evaluation was conducted to assess the measurement uncertainty in determining paracetamol content in granules using UV spectrophotometry, a common pharmaceutical quality control method. While the principles of uncertainty calculation are established, this study provides a detailed, practical application for this specific widely used pharmacopoeial assay. The process involved identifying uncertainty sources from the analytical procedure, including sample weighing (W<sub>s</sub>), average pack weight (W), volumetric dilutions using 100 mL flasks (V<sub>1</sub>, V<sub>3</sub>) and a 5 mL pipette (V<sub>2</sub>), absorbance measurement (A) at 257 nm, and the specific absorbance value <span>({text{E}}_{text{1 cm}}^{text{1%}})</span>. Individual uncertainty components were quantified based on instrument tolerances (balance, spectrophotometer, glassware) and temperature effects, following a cause-and-effect analysis and Eurachem guidelines. Measurement repeatability (RSD) was also incorporated. The combined standard uncertainty and expanded uncertainty (k = 2) were calculated using established formulas and spreadsheet methods. Results showed the average paracetamol content was determined to be 100.14%. For a single determination, the expanded uncertainty was 6.13%. Major contributors were identified as measurement repeatability, the uncertainty of the specific absorbance value, and volumetric steps. Performing the determination in triplicate significantly reduced the repeatability contribution, lowering the overall expanded uncertainty to 4.01%, yielding a final reported result of (100.14 ± 4.01)%. This research establishes a robust procedure for uncertainty evaluation, enhancing the reliability of UV spectrophotometric assays for paracetamol granules and providing a useful framework for quality control laboratories.</p></div>","PeriodicalId":454,"journal":{"name":"Accreditation and Quality Assurance","volume":"30 5","pages":"553 - 561"},"PeriodicalIF":1.0,"publicationDate":"2025-07-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145073553","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Residual behaviour and dietary risk assessment of combination product of trifloxystrobin and propineb in/on tomato, chilli and apple 三氯虫酯与丙泊尼复合制剂在番茄、辣椒和苹果上的残留行为及膳食风险评价
IF 1 4区 工程技术
Accreditation and Quality Assurance Pub Date : 2025-07-11 DOI: 10.1007/s00769-025-01657-7
Sapna Katna, Tanuja Banshtu, Ajay Sharma, Jatiender Kumar Dubey, Sakshi Sharma, Nisha Devi, Arvind Kumar, Shubhra Singh
{"title":"Residual behaviour and dietary risk assessment of combination product of trifloxystrobin and propineb in/on tomato, chilli and apple","authors":"Sapna Katna,&nbsp;Tanuja Banshtu,&nbsp;Ajay Sharma,&nbsp;Jatiender Kumar Dubey,&nbsp;Sakshi Sharma,&nbsp;Nisha Devi,&nbsp;Arvind Kumar,&nbsp;Shubhra Singh","doi":"10.1007/s00769-025-01657-7","DOIUrl":"10.1007/s00769-025-01657-7","url":null,"abstract":"<div><p>A comprehensive study was undertaken to assess residual behaviour and dietary risk associated with a combination product containing trifloxystrobin and propineb in tomato, chilli and apple. Sample analysis was performed using validated QuEChERS method for trifloxystrobin and CGA 321113, while for propineb, method validated by Dubey and Stan (J Food Sci Technol 35:482–485, 1998) was used across all three crops, with residue detection using GC-ECD and UV–Vis spectrophotometer. Trifloxystrobin exhibited half-lives of 2.72–2.77 days in tomatoes, 2.49–2.89 days in chillies and 4.14–4.49 days in apples. Meanwhile, the half-life of propineb in tomatoes, chillies and apples were 1.27–1.51, 1.60–2.27 and 1.73–2.27 days, respectively. Upon comparing estimated daily intake (EDI) in India for both components of combination product with acceptable daily intake (ADI), the cumulative index of risk assessment and hazard index was consistently below 1 in all three crops, indicating no potential risk to consumers.</p></div>","PeriodicalId":454,"journal":{"name":"Accreditation and Quality Assurance","volume":"30 5","pages":"591 - 604"},"PeriodicalIF":1.0,"publicationDate":"2025-07-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145073550","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Computational insights into the interactions of sofosbuvir and remdesivir with RNA-directed RNA polymerase: ligand screening, docking simulations, and interaction analysis 索非布韦和瑞德西韦与RNA定向RNA聚合酶相互作用的计算见解:配体筛选,对接模拟和相互作用分析
IF 1 4区 工程技术
Accreditation and Quality Assurance Pub Date : 2025-07-11 DOI: 10.1007/s00769-025-01652-y
Sirvan Abbasbeigi
{"title":"Computational insights into the interactions of sofosbuvir and remdesivir with RNA-directed RNA polymerase: ligand screening, docking simulations, and interaction analysis","authors":"Sirvan Abbasbeigi","doi":"10.1007/s00769-025-01652-y","DOIUrl":"10.1007/s00769-025-01652-y","url":null,"abstract":"<div><p>This review explores sofosbuvir, a nucleoside analog approved for hepatitis C, as a potential inhibitor of SARS-CoV-2 RNA-dependent RNA polymerase (RdRp), compared to remdesivir, which is constrained by hepatic and renal toxicity. RdRp, essential for viral replication, is a key target for COVID-19 therapeutics. Ligand-based virtual screening through the DrugRep virtual screening server, utilizing algorithms like Morgan fingerprint, identified compounds structurally akin to remdesivir. Structure-based molecular docking with CB-Dock2 and AutoDock Vina targeted the RdRp structure (PDB ID: 7BV2), revealing sofosbuvir’s binding affinity of − 7.6 kcal/mol, slightly lower than remdesivir’s − 8.4 kcal/mol, but with strong hydrogen bonds to ARG349 (3.05, 2.99, 2.89 Å) and CYS395 (3.41 Å), alongside Pi-Sigma and Pi-Alkyl interactions with PRO461 and VAL315. Molecular dynamics simulations (30 ns, LAMMPS) suggest sofosbuvir’s stability, with lower RMSD (~ 1.4 Å vs. ~ 1.8 Å for remdesivir) and more persistent hydrogen bonds, supported by its reliable structure and connectivity. Compared to remdesivir, sofosbuvir exhibits fewer unfavorable interactions and a well-established safety profile. Interaction analyses using BIOVIA Discovery Studio and LigPlot + confirmed sofosbuvir’s stability within the RdRp active site, corroborated by in vitro and clinical evidence. These findings highlight the pivotal role of in silico methods in drug repurposing for COVID-19. However, experimental validation is crucial to confirm sofosbuvir’s efficacy, particularly against SARS-CoV-2 variants, and to explore its therapeutic potential for addressing current and future viral threats.</p></div>","PeriodicalId":454,"journal":{"name":"Accreditation and Quality Assurance","volume":"30 5","pages":"493 - 505"},"PeriodicalIF":1.0,"publicationDate":"2025-07-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145073551","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Simultaneous Quantification of Artemether and Lumefantrine in Rat Plasma Using a Validated LC-MS/MS Method 高效液相色谱-质谱联用法同时测定大鼠血浆中蒿甲醚和氨芳碱的含量
IF 1 4区 工程技术
Accreditation and Quality Assurance Pub Date : 2025-07-10 DOI: 10.1007/s00769-025-01647-9
Ripal Shah,  Tejal Soni, Dinal Patel, Jenee Christian, Mansi Dholakia, Mehul Patel, Kishor Sorathia
{"title":"Simultaneous Quantification of Artemether and Lumefantrine in Rat Plasma Using a Validated LC-MS/MS Method","authors":"Ripal Shah,&nbsp; Tejal Soni,&nbsp;Dinal Patel,&nbsp;Jenee Christian,&nbsp;Mansi Dholakia,&nbsp;Mehul Patel,&nbsp;Kishor Sorathia","doi":"10.1007/s00769-025-01647-9","DOIUrl":"10.1007/s00769-025-01647-9","url":null,"abstract":"<div><p>A robust and reproducible LC–MS/MS method was developed and optimized for the simultaneous quantification of artemether (ART) and lumefantrine (LUF) in rat plasma, employing carbamazepine as an internal standard (IS). The mass spectrometer operated in positive ionization mode with electrospray ionization (ESI), yielding product ions at m/z 163.05(ART), m/z 511.95 (LUF), and m/z 194.1 (IS). Chromatographic separation was achieved using a Waters™ X Select C18 column (100 mm × 4.6 mm, 2.5 µm) with a mobile phase of 0.2 % formic acid in water: methanol (10:90) at a flow rate of 0.5 mL/min. Retention times for ART, LUF, and IS were 4.30 min, 1.60 min, and 2.46 min, respectively, within a 6-min runtime. The liquid–liquid extraction (LLE) method utilized ethyl acetate with acidified methanol for optimal analyte recovery, achieving mean recoveries of 92.12 % for ART and 91.07% for LUF. Calibration curves were linear over the range of 5–1000 ng/mL with regression coefficients of ≥ 0.9992. The method demonstrated high precision (%CV: 0.16–1.89) and accuracy (98.24–106.42 %) at the lower limit of quantification (LLOQ: 5 ng/mL). The method exhibited minimal matrix effects, with stability tests confirming analyte integrity under benchtop and freeze–thaw conditions. To the best of our knowledge, this is the first validated LC-MS/MS method developed for the simultaneous quantification of ART and LUF in rat plasma for preclinical pharmacokinetic studies, providing a novel, sensitive, and cost-effective analytical tool for routine high-throughput analysis.</p></div>","PeriodicalId":454,"journal":{"name":"Accreditation and Quality Assurance","volume":"30 4","pages":"429 - 443"},"PeriodicalIF":1.0,"publicationDate":"2025-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145164273","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
HPTLC method for simultaneous determination of rivaroxaban and its aminomethyl process impurity/metabolite 高效液相色谱法同时测定利伐沙班及其氨甲基工艺杂质/代谢物
IF 1 4区 工程技术
Accreditation and Quality Assurance Pub Date : 2025-07-03 DOI: 10.1007/s00769-025-01663-9
Amit Shimpi, Bhatu Patil, Kunal Bhadane, Yogesh Agrawal, Vaishnavi Pawar, Amod Patil, Atul Shirkhedkar, Iqrar Ahmad, Harun Patel
{"title":"HPTLC method for simultaneous determination of rivaroxaban and its aminomethyl process impurity/metabolite","authors":"Amit Shimpi,&nbsp;Bhatu Patil,&nbsp;Kunal Bhadane,&nbsp;Yogesh Agrawal,&nbsp;Vaishnavi Pawar,&nbsp;Amod Patil,&nbsp;Atul Shirkhedkar,&nbsp;Iqrar Ahmad,&nbsp;Harun Patel","doi":"10.1007/s00769-025-01663-9","DOIUrl":"10.1007/s00769-025-01663-9","url":null,"abstract":"<div><p>Simultaneous high-performance thin-layer chromatography (HPTLC) method was developed and validated for the quantification of rivaroxaban and its aminomethyl process impurity/metabolite. Using a toluene–methanol–triethylamine (6:3.5:0.5%v/v/v) mobile phase, the method achieved optimized R<i>f</i> values of 0.75 for rivaroxaban and 0.38 for the impurity. The method exhibited a linear response for both analytes in the range of 800–1300 ng/band, with correlation coefficients of 0.998 and 0.997, respectively. Sensitivity assessments revealed detection limits of 0.0086 ng/band for rivaroxaban and 0.0165 ng/band for the impurity, with quantification limits of 0.026 ng/band and 0.050 ng/band, respectively. Robustness and precision tests confirmed the method’s reliability, with %RSD values below 2.0 for all parameters. This validated HPTLC method offers an efficient solution for simultaneous determination of rivaroxaban and aminomethyl impurity/metabolite of rivaroxaban in pharmaceutical formulations. This simple HPTLC method provides a comprehensive approach for impurity profiling and quality control in pharmaceutical formulations. Its high sensitivity, reproducibility, and robustness make it a valuable tool in ensuring drug safety and compliance with regulatory standards.</p></div>","PeriodicalId":454,"journal":{"name":"Accreditation and Quality Assurance","volume":"30 4","pages":"419 - 427"},"PeriodicalIF":1.0,"publicationDate":"2025-07-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145161214","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
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