Han Zheng, Xiaoping Song, Haifeng Wang, Yue Kou, Jia Li
{"title":"Determination of the water content of crude oil by thermometric titration.","authors":"Han Zheng, Xiaoping Song, Haifeng Wang, Yue Kou, Jia Li","doi":"10.1007/s00216-025-05833-z","DOIUrl":"https://doi.org/10.1007/s00216-025-05833-z","url":null,"abstract":"<p><p>The water content of crude oil needs to be accurately and conveniently determined. A thermometric titration method in which triethyl orthoformate and water react stoichiometrically and then absorb heat has been developed to determine the water content of crude oil. Triethyl orthoformate solution was used as the titrant; a mixture of cyclohexane, isopropanol, and xylene was used as the solvent; and dodecylbenzene sulfonic acid was used as the catalyst. The optimized method has a water mass range of 5 to 300 mg. The upper limit of water mass (300 mg) was greater than those of Karl Fischer coulometric titration (KFCT) and azeotropic distillation-KFCT (AD-KFCT). Real-time calibration by alternatively measuring the sample and a standard and modifying the result by the neighboring recovery was used to reduce the effect of the shift of the calibration curve. The effect of the types of catalysts and titrants was investigated. When the certified reference materials of light or heavy crude oil for water content were measured, the relative standard deviation and absolute value of the relative error of the results were ≤ 1.2% and ≤ 3.9%, respectively. The repeatability and accuracy were better than those of the distillation, KFCT, and AD-KFCT. The present method can determine the water content of commercial crude oil with good accuracy and convenience, and thus has the potential to be an international standard method.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-03-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143690533","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Yao Liu, Yang Li, Yuting Shan, Jiufa Zhang, Xiaohe Huang, Yueyue Yu, Cuiping Ma, Yan Xu, Chao Shi
{"title":"A rolling circle mediated exponential amplification reaction with suppressed nonspecific amplification to detect pathogen RNA with high sensitivity.","authors":"Yao Liu, Yang Li, Yuting Shan, Jiufa Zhang, Xiaohe Huang, Yueyue Yu, Cuiping Ma, Yan Xu, Chao Shi","doi":"10.1007/s00216-025-05835-x","DOIUrl":"https://doi.org/10.1007/s00216-025-05835-x","url":null,"abstract":"<p><p>Respiratory infections caused by pathogens such as influenza virus and SARS-CoV-2 seriously threaten human life and health. RNA has been widely recognized as an important biomarker for diagnosing these pathogens, creating a growing need for rapid and accurate RNA detection methods. Isothermal nucleic acid amplification has emerged as a promising molecular diagnostics approach. Exponential amplification reactions (EXPAR) is a commonly used RNA detection method, known for its simplicity and rapid signal amplification in a short time. However, traditional EXPAR is only suitable for detecting short-sequence RNA, and 3'-end template interactions in the amplification reaction can lead to nonspecific amplification, which greatly limits its practical application. Here, we established an isothermal amplification method comprising a three-way junction (3-WJ) structure and dumbbell probe (DP) for the rapid and sensitive detection of pathogen RNA in a single closed tube, termed the rolling circle mediated exponential amplification reaction (RC-EXPAR). The introduction of the DP eliminated the 3'-end of the template, suppressing nonspecific amplification caused by the 3'-end extension in the reaction. Although the trigger generation by the 3-WJ structure is a linear amplification process, the RC-EXPAR amplifies the triggers exponentially to enhance signal output further and increase sensitivity. The proposed method showed a high sensitivity with a limit of detection (LOD) of 10<sup>3</sup> copies/mL. Moreover, RC-EXPAR demonstrated strong anti-interference capability in complex biological matrices. This work opens up new ideas for suppressing nonspecific amplification and provides a promising signal amplification strategy for rapid, sensitive, and specific pathogen detection in clinical.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-03-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143690529","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"SERS substrate based on large-scale self-assembled Au nanobipyramid@Ag nanorod multifunctional paper-based materials for practical and reliable quantitative SERS detection.","authors":"Longlong Luan, Xiang Zhang, Pan Li, Weiping Xu","doi":"10.1007/s00216-025-05830-2","DOIUrl":"https://doi.org/10.1007/s00216-025-05830-2","url":null,"abstract":"<p><p>Pesticides and fungicides in foods pose a significant threat to human health. The design and development of a new and efficient sensing platform for the quantitative detection of contaminants in the food industry have become an urgent problem for food security and environmental protection. Here, we report a simple and reliable large self-assembled Au nanobipyramid@Ag nanorod (Au NBPs@Ag NRs) SERS multifunctional paper-based substrate for rapid and sensitive quantitative detection of contaminants in real samples. Moreover, 4-mercaptobenzoic acid (4-MBA) was uniformly distributed on the surface of the Au NBPs@Ag NRs as an internal standard through liquid-liquid interface self-assembly. The effective correction of the fluctuations in the SERS signal and the large number of nanogaps contributed to the increase in the number of SERS \"hot spots,\" enabling the sensor to have excellent SERS performance. The results showed that the Au NBPs@Ag NRs/4-MBA SERS multifunctional paper-based substrate had excellent sensitivity and reproducibility for the detection of crystal violet (CV) probe molecules. In particular, the SERS sensor is used for the quantitative detection of malachite green (MG) in pond water and thiram (THR) on apple surfaces, and the detection limit was as low as 0.012 ppm and 0.0044 ppm. Therefore, the Au NBPs@Ag NRs/4-MBA SERS-active paper-based substrate is highly efficient and versatile and can be used for reliable sensor analysis of actual sample pollutants.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-03-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143690684","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Huaxin Wu, Ting Huang, Wei Zhang, Huan Yao, Xueyao Li, Ping Su, Yi Yang
{"title":"Purity determination of digitoxin by two-signal suppression-internal standard correction-high-performance liquid chromatography-quantitative nuclear magnetic resonance.","authors":"Huaxin Wu, Ting Huang, Wei Zhang, Huan Yao, Xueyao Li, Ping Su, Yi Yang","doi":"10.1007/s00216-025-05836-w","DOIUrl":"https://doi.org/10.1007/s00216-025-05836-w","url":null,"abstract":"<p><p>In the biomedical and chemical fields, purity assessment of compounds is a critical step in ensuring product quality and safety. In this study, a method for purity quantification was proposed as two-signal suppression-internal standard correction-high-performance liquid chromatography-quantitative nuclear magnetic resonance (TSS-ISC-HPLC-qNMR). The two-signal suppression effectively suppresses the interference of solvent signals in the NMR spectra, and the internal standard correction eliminates the influence of many variables during sample preparation and analysis. The purity result (99.89%) of the quantification of certified reference material of acesulfame (AF) by this method matched with the certified value (99.88%), which verified the accuracy of the method. The purity result (with standard deviation) of 94.42% ± 0.10% for the quantification of the low-purity drug digitoxin by the method matched with the purity result of 94.42% ± 0.11% by qNMR with deconvolution (as a validated method), which proved that the method could be used for the quantification of low-purity compounds. The methodology achieved a substantial reduction in total analysis time, from 28 to 4 h (considering only the routine analysis time after optimization), in contrast to the ISC-HPLC-qNMR approach. Additionally, it effectively decreased bias to undetectable with a standard deviation of 0.10%, while the bias of the TSS-HPLC-qNMR method was 0.93%. The present method ensures the accuracy of the quantitative results while demonstrating a low economic burden and significant time efficiency, which shows great potential for application in the accurate quantitative analysis of low-purity organic compounds.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-03-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143690671","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Yumeng Li, Ran Chen, Juanjuan Lv, Jiali Su, Mengxu Gao, Kaifu Ma, Xiupei Cheng, Wei Shu
{"title":"A dual-functional fluorescent probe for biosystem imaging and food safety monitoring of HSO<sub>3</sub><sup>-</sup> with high selectivity and sensitivity.","authors":"Yumeng Li, Ran Chen, Juanjuan Lv, Jiali Su, Mengxu Gao, Kaifu Ma, Xiupei Cheng, Wei Shu","doi":"10.1007/s00216-025-05837-9","DOIUrl":"https://doi.org/10.1007/s00216-025-05837-9","url":null,"abstract":"<p><p>In the food field, HSO<sub>3</sub><sup>-</sup> is commonly used as a beverage additive, antioxidant, enzyme inhibitor, and preservative to extend shelf life and freshness. However, excessive intake of exogenous HSO<sub>3</sub><sup>-</sup> can lead to abnormal HSO<sub>3</sub><sup>-</sup> concentration levels in the body, causing cardiovascular and respiratory diseases. This highlights the urgent need to develop a rapid and sensitive probe for the quantitative detection of HSO<sub>3</sub><sup>-</sup> in foods and biosystems. In this study, we design and synthesize a novel HSO<sub>3</sub><sup>-</sup> fluorescent probe named DCPD. Bioimaging experiments show that DCPD has good mitochondrial targeting and can be used to imaging the redox process of HSO<sub>3</sub><sup>-</sup>/H<sub>2</sub>O<sub>2</sub> in cells and tissue. In addition, DCPD has been used in detecting HSO<sub>3</sub><sup>-</sup> in foods with satisfactory recoveries (98.62-105.06%), further demonstrating its compatibility and utility. Thus, the DCPD probe offers substantial promise for application in food analysis and the assessment of HSO<sub>3</sub><sup>-</sup> concentrations in biological systems.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-03-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143676671","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Wenya Li, Bingling Gao, Tao Yang, Liping Tang, Dan Song, Hongmei Li, Keqi Sun, Peng Xiao
{"title":"Development and validation of an isotope dilution-liquid chromatography (ID-LC-MS/MS)-based candidate reference measurement procedure for total 3,3',5-triiodothyronine in human serum.","authors":"Wenya Li, Bingling Gao, Tao Yang, Liping Tang, Dan Song, Hongmei Li, Keqi Sun, Peng Xiao","doi":"10.1007/s00216-025-05834-y","DOIUrl":"https://doi.org/10.1007/s00216-025-05834-y","url":null,"abstract":"<p><p>3,3',5-Triiodothyronine (T3) plays a crucial role in the diagnosis and evaluation of thyroid diseases. The current reference measurement procedure (RMP) has been in place for 20 years and is widely adopted by reference laboratories around the world. To enhance the performance of the RMP, we developed and validated a simplified, SI-traceable candidate RMP specifically targeting serum total T3 (TT3) using isotope dilution-liquid chromatography with tandem mass spectrometry (ID-LC-MS/MS). Specifically, T3 reference material was employed as the standard. Compared to the RMP, our method incorporates a simplified serum cleanup process involving protein precipitation and nitrogen drying. The method validation followed ISO guidelines for measurement uncertainty assessment. Our results indicated that there was no significant conversion of T4 into metabolites during the serum pretreatment. The lower limit of the measuring interval was determined to be 0.077 nmol/L, and the regression model was linear across a range of 0.016 to 13.086 nmol/L. The imprecision of intra-assays ranged from 0.1 to 1.9%, while inter-assay imprecision ranged from 0.5 to 1.2%. The bias observed when analyzing SRM971 was between - 0.34 and - 1.65%. This candidate RMP demonstrated excellent agreement with the RMPs developed by RELA activity, showing a mean bias falling within the educational mean ratio (6%). The measurement uncertainties were 0.022 nmol/L for RELA2023A and 0.120 nmol/L for RELA2023B. In conclusion, the developed candidate RMP is traceable, reliable, and easy to operate, showing promising potential for the development of serum reference materials and the standardization of routine assays.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-03-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143690498","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Hui Ran, Yusha Huang, Qi Wang, Lianzhe Hu, Min Wang
{"title":"Mimicking phosphatase function using Ce<sup>4+</sup>-modified metal-organic frameworks as heterogeneous catalysts for the discrimination of phosphorylated peptides.","authors":"Hui Ran, Yusha Huang, Qi Wang, Lianzhe Hu, Min Wang","doi":"10.1007/s00216-025-05831-1","DOIUrl":"https://doi.org/10.1007/s00216-025-05831-1","url":null,"abstract":"<p><p>In this study, a general approach to prepare metal-organic framework (MOF)-based heterogeneous catalysts is proposed. The Ce<sup>4+</sup>-modified MOFs were obtained by the co-precipitation of catalytic active Ce<sup>4+</sup> ions and catalytic inactive MOFs (ZIF-67, MOF-5, and ZIF-8). The Ce<sup>4+</sup>-modified MOFs retained the phosphatase-like activity of Ce<sup>4+</sup> ions and were used for the fluorescent detection of phosphorylated amino acids by using o-phospho-L-tyrosine (p-Tyr) as a model target. Using Ce<sup>4+</sup>-modified ZIF-67 particles as the heterogeneous catalysts, the linear range for p-Tyr detection is 1-10 µM with a detection limit of 0.26 µM. Compared with homogeneous Ce<sup>4+</sup> ion catalysts, a significant improvement in the sensitivity was achieved by using Ce<sup>4+</sup>-modified ZIF-67 particles as heterogeneous catalysts (from 11.21 to 0.26 µM). As the proposed method holds great promise in the fluorescent detection of phosphorylated amino acids, the Ce<sup>4+</sup>-modified ZIF-67-based catalytic system was further used for the discrimination of normal peptides and phosphorylated peptides with excellent resolution.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-03-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143676716","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Subramani Natarajan, Diana Bucur, Steven Kildea, Fiona Doohan
{"title":"Digital PCR assays for quantifying trichothecene-producing Fusarium species, including Fusarium langsethiae, F. poae, and F. sporotrichioides, in oats.","authors":"Subramani Natarajan, Diana Bucur, Steven Kildea, Fiona Doohan","doi":"10.1007/s00216-025-05840-0","DOIUrl":"https://doi.org/10.1007/s00216-025-05840-0","url":null,"abstract":"<p><p>Fusarium fungi cause Fusarium head blight (FHB) in oats, reducing yield and contaminating grains with harmful trichothecene mycotoxins. FHB symptoms in oats are often not visually distinct, necessitating alternative detection methods. We developed digital PCR (dPCR) assays as the most accurate DNA-based method to detect trichothecene-producing Fusarium species commonly found in oats. Building on existing quantitative PCR (qPCR) assays, we developed dPCR assays targeting all trichothecene producers (the Tri5 gene), or specific to F. langsethiae (Fl), F. poae (Fp), and F. sporotrichioides (Fs). All targeted single copy genes, except F. poae which targeted rDNA which is a variable and multi-copy target (and hence not as reliable as the other assays for quantification). Optimized dPCR assays showed excellent linearity (R<sup>2</sup> = 0.99) and greater resilience than qPCR to varying oat DNA concentrations. Overall, when comparing assay sensitivity using both fungal and field oat DNA extracts, dPCR assays were superior to qPCR for Tri5, Fl, and Fs, but the converse was true for Fp. Performance comparisons using field samples showed moderate to perfect agreement between qPCR and dPCR for Tri5 and Fl (κ = 0.5 and 0.86) and poor agreement for Fp (κ = 0.00). Strong correlations were observed between the methods for Tri5, Fl, and Fp (r = 0.88-0.97), but unlike dPCR, qPCR did not detect Fs in any of the field samples. We conclude that the dPCR assays for Tri5, Fl, and Fs offer a reliable method for quantification while that for Fp is reliable for fungal detection but less reliable for quantification of the pathogen in field samples.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-03-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143673115","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Diego A Garzón, Diego A Ahumada, Cristhian Paredes, Elianna Castillo
{"title":"Development of a reference material for mercury in fish: certified for total mercury and characterized for methylmercury.","authors":"Diego A Garzón, Diego A Ahumada, Cristhian Paredes, Elianna Castillo","doi":"10.1007/s00216-025-05817-z","DOIUrl":"https://doi.org/10.1007/s00216-025-05817-z","url":null,"abstract":"<p><p>Reference materials (RMs) and certified reference materials (CRMs) are essential for ensuring compliance of food products with international standards. In fish, mercury content is closely monitored due to associated human health risks. This study developed and certified a CRM for total mercury (Hg) and methylmercury (MeHg) in striped catfish (Pseudoplatystoma fasciatum) from the Colombian Amazon. The process involved raw material selection, sample preparation, homogeneity, and stability, resulting in the CRM INM-039-1. Total Hg was measured using inductively coupled plasma-mass spectrometry (ICP-MS) and cold vapor atomic absorption spectrometry (CV-AAS), while MeHg was analyzed by gas chromatography-mass spectrometry (GC-MS). Calibration methods varied: ICP-MS used gravimetric standard addition, CV-AAS employed bracketing calibration, and GC-MS applied matrix-matched calibration. Method validation was performed using CRMs DORM-4 and ERM-CE464. The total Hg results were combined using the Levenson approach, yielding a relative standard uncertainty of 1.8%, while MeHg was 2.9%. Other uncertainty components included long-term stability (2.5%), homogeneity (1.8%), and short-term stability under transport conditions (0.02%). The CRM was certified with a total Hg mass fraction of 3.94 mg/kg (relative expanded uncertainty 7.1%, k = 2) and an informative MeHg mass fraction of 3.79 mg/kg (relative expanded uncertainty 8.3%, k = 2). This CRM is a valuable tool for assessing mercury in similar matrices, supporting compliance with safety standards for small and mid-size fish producers in the region.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-03-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143661817","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}