Microchemical Journal最新文献_第4页

Bottom-up measurement uncertainty evaluation for Cr(III) and Cr(VI) speciation in natural water by HPLC-ICP-MS

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-02-28 DOI: 10.1016/j.microc.2025.113190

Radka Pechancová , Ricardo J.N. Bettencourt da Silva , David Milde , Tomáš Pluháček

The monitoring of Cr(III) and Cr(VI) in natural waters is essential for the assessment of chromium-based levels that deteriorate the water quality and adversely affect aquatic biota. The evaluation of the uncertainty of this monitoring is crucial for the determination of their fitness for purpose and for the objective interpretation of the quantitative information. There is a great need for a detailed bottom-up evaluation of the uncertainty of Cr(III) and Cr(VI) measurements in natural waters by ion-exchange high-performance liquid chromatography inductively coupled plasma mass spectrometry. Detailed models of the uncertainty of sample dilution, calibrator preparation and sample signal interpolation in a weighted calibration curve are proposed. The models proved adequate from the metrological compatibility between reference and estimated concentrations of spiked river waters. Measurement of Cr(III) and Cr(VI) above 0.98 µg L^-1 and 0.5 µg L^-1 with relative expanded uncertainties as low as 4.0%, and 2.3%, respectively, can be achieved. For not diluted samples, calibrators’ values and sample signal interpolation are responsible for between 14% and 82% or 18% and 85% of the uncertainty. The analysis of a certified reference material proved that the Cr(III)/Cr(VI) interconversion during analytical work is negligible. The developed measurement models were successfully applied to the analysis of river waters and groundwater collected in the Czech Republic. Only Cr(III) at the concentration levels around 1 µg L^-1 was detected in the river samples, whereas a toxic Cr(VI) was determined in groundwater. The proposed validated methodology and user-friendly spreadsheet for the detailed evaluation of measurement uncertainty can be generally applied to other speciation approaches, where the separation techniques are hyphenated with either organic or elemental mass spectrometry.

{"title":"Bottom-up measurement uncertainty evaluation for Cr(III) and Cr(VI) speciation in natural water by HPLC-ICP-MS","authors":"Radka Pechancová , Ricardo J.N. Bettencourt da Silva , David Milde , Tomáš Pluháček","doi":"10.1016/j.microc.2025.113190","DOIUrl":"10.1016/j.microc.2025.113190","url":null,"abstract":"<div><div>The monitoring of Cr(III) and Cr(VI) in natural waters is essential for the assessment of chromium-based levels that deteriorate the water quality and adversely affect aquatic biota. The evaluation of the uncertainty of this monitoring is crucial for the determination of their fitness for purpose and for the objective interpretation of the quantitative information. There is a great need for a detailed bottom-up evaluation of the uncertainty of Cr(III) and Cr(VI) measurements in natural waters by ion-exchange high-performance liquid chromatography inductively coupled plasma mass spectrometry. Detailed models of the uncertainty of sample dilution, calibrator preparation and sample signal interpolation in a weighted calibration curve are proposed. The models proved adequate from the metrological compatibility between reference and estimated concentrations of spiked river waters. Measurement of Cr(III) and Cr(VI) above 0.98µgL<sup>-1</sup> and 0.5µgL<sup>-1</sup> with relative expanded uncertainties as low as 4.0%, and 2.3%, respectively, can be achieved. For not diluted samples, calibrators’ values and sample signal interpolation are responsible for between 14% and 82% or 18% and 85% of the uncertainty. The analysis of a certified reference material proved that the Cr(III)/Cr(VI) interconversion during analytical work is negligible. The developed measurement models were successfully applied to the analysis of river waters and groundwater collected in the Czech Republic. Only Cr(III) at the concentration levels around 1 µgL<sup>-1</sup> was detected in the river samples, whereas a toxic Cr(VI) was determined in groundwater. The proposed validated methodology and user-friendly spreadsheet for the detailed evaluation of measurement uncertainty can be generally applied to other speciation approaches, where the separation techniques are hyphenated with either organic or elemental mass spectrometry.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113190"},"PeriodicalIF":4.9,"publicationDate":"2025-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143547885","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}

引用次数: 0

Investigation of Ruthenium–based pyridine substituted 1,2,4–Triazole–5– ylidenes complexes as molecular electrocatalysts in the effective detection of date rape drugs

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-02-28 DOI: 10.1016/j.microc.2025.113213

Nupoor Gopal Neole , Zhoveta Yhobu , K.S. Manjunatha Kumara , Doddahalli H. Nagaraju , Srinivasa Budagumpi

Numerous new psychoactive substances have been introduced into the drug market over the past decade mainly with an intention to implement their use for clinical purposes. However, the necessity of updated screening approaches for their quantification within the clinically required concentrations is crucial to avoid drug abusive incidents. Present work describes a study on the application of suitably designed N–heterocyclic carbene (NHC) coordinated ruthenium(II) p–cymene complexes for the detection of date rape drugs (DRDs) such as ketamine and scopolamine. The study highlights the synthesis of two structurally–tuned ruthenium(II) NHC complexes bearing pyridine and benzyl/benzonitrile substituted 1,2,4–triazol–5–ylidene ligand and their spectral and analytical characterization. Further, the preparation of the working electrodes using ruthenium(II) NHC complexes for electrochemical measurements evidenced the ultra–trace level detection of predatory drugs like ketamine and scopolamine, with limit of detection as low as 0.275 and 4.379 nM, respectively. Developed ruthenium NHC complexes are cost–effective, easy–to–use and successfully employed for the detection of DRDs at pertinent concentrations using an aqueous electrolyte. Furthermore, the title ruthenium derivatives are stable, hence upon real time analyses, could be employed in the assembly of point–of–care devices. Alongside, these electrochemical sensors can potentially simplify the conventional protocols that are time–consuming and demand tedious sample preparation methods; therefore, the usage of these organometallics by forensic scientists in the investigation of drug abuse cases opens up new avenues.

{"title":"Investigation of Ruthenium–based pyridine substituted 1,2,4–Triazole–5– ylidenes complexes as molecular electrocatalysts in the effective detection of date rape drugs","authors":"Nupoor Gopal Neole , Zhoveta Yhobu , K.S. Manjunatha Kumara , Doddahalli H. Nagaraju , Srinivasa Budagumpi","doi":"10.1016/j.microc.2025.113213","DOIUrl":"10.1016/j.microc.2025.113213","url":null,"abstract":"<div><div>Numerous new psychoactive substances have been introduced into the drug market over the past decade mainly with an intention to implement their use for clinical purposes. However, the necessity of updated screening approaches for their quantification within the clinically required concentrations is crucial to avoid drug abusive incidents. Present work describes a study on the application of suitably designed N–heterocyclic carbene (NHC) coordinated ruthenium(II) <em>p</em>–cymene complexes for the detection of date rape drugs (DRDs) such as ketamine and scopolamine. The study highlights the synthesis of two structurally–tuned ruthenium(II) NHC complexes bearing pyridine and benzyl/benzonitrile substituted 1,2,4–triazol–5–ylidene ligand and their spectral and analytical characterization. Further, the preparation of the working electrodes using ruthenium(II) NHC complexes for electrochemical measurements evidenced the ultra–trace level detection of predatory drugs like ketamine and scopolamine, with limit of detection as low as 0.275 and 4.379 nM, respectively. Developed ruthenium NHC complexes are cost–effective, easy–to–use and successfully employed for the detection of DRDs at pertinent concentrations using an aqueous electrolyte. Furthermore, the title ruthenium derivatives are stable, hence upon real time analyses, could be employed in the assembly of point–of–care devices. Alongside, these electrochemical sensors can potentially simplify the conventional protocols that are time–consuming and demand tedious sample preparation methods; therefore, the usage of these organometallics by forensic scientists in the investigation of drug abuse cases opens up new avenues.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113213"},"PeriodicalIF":4.9,"publicationDate":"2025-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143547964","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}

引用次数: 0

RDA-direct targeted flavonoids profiling strategy combined with fingerprinting and chemometrics for quality evaluation of Changshan Huyou flower

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-02-28 DOI: 10.1016/j.microc.2025.113204

Bingjing Xu , Mengyao Shi , Qiang Lyu , Yunjie Sheng , Jinting Li , Jian Chen , Chaoying Tong , Dan Shou

The Changshan Huyou flower (HYF) derived from the bud of Citrus changshanhuyou Y. B. Chang is rich in flavonoids and holds significant potential for food development. However, inadequate clarification of the chemical basis and lacked quality control standards hindered its further in-depth utilisation. Herein, a novel Retro Diels-Alder (RDA)-direct strategy was proposed for flavonoid subclass profiling. Through extracting characteristic ^1,3A⁺, ^1,3B⁺ and ^0,2B⁺ ions from MS/MS spectrum, the signal-to-noise ratio can be improved up to 500 times, resulting in higher capacity of identification. Combined with relative retention time, characteristic diagnostic fragment ions, literature data and standard substance comparison, flavonoid subclass skeleton was unambiguously ascertained, with a total of 23 flavonoids (15 first reported) identified from HYF. Furthermore, quality of HYF was evaluated by high-performance liquid chromatography fingerprinting and integrated chemometrics. The similarity (> 0.944) indicated the stable quality of 20 HYF batches. Four potential quality markers including neoeriocitrin, naringin, hesperidin and neohesperidin were screened and quantified with high sensitivity (LOD, 0.039–0.442 μg/mL), satisfying precision and repeatability (RSD < 2.88 %), and pinpoint accuracy (recovery, 97.72 %–100.44 %). These markers exhibited high content levels ranging from 0.133 %–1.479 %, 3.637 %–5.146 %, 0.021 %–1.422 % and 4.978 %–9.756 %, which were closely linked to the quality of HYF that fluctuated at different growth stages. This research may offer a novel strategy and comprehensive guideline for quality evaluating of HYF and other herbal materials containing flavonoids.

{"title":"RDA-direct targeted flavonoids profiling strategy combined with fingerprinting and chemometrics for quality evaluation of Changshan Huyou flower","authors":"Bingjing Xu , Mengyao Shi , Qiang Lyu , Yunjie Sheng , Jinting Li , Jian Chen , Chaoying Tong , Dan Shou","doi":"10.1016/j.microc.2025.113204","DOIUrl":"10.1016/j.microc.2025.113204","url":null,"abstract":"<div><div>The Changshan Huyou flower (HYF) derived from the bud of <em>Citrus changshanhuyou</em> Y. B. Chang is rich in flavonoids and holds significant potential for food development. However, inadequate clarification of the chemical basis and lacked quality control standards hindered its further in-depth utilisation. Herein, a novel Retro Diels-Alder (RDA)-direct strategy was proposed for flavonoid subclass profiling. Through extracting characteristic <sup>1,3</sup>A<sup>+</sup>, <sup>1,3</sup>B<sup>+</sup> and <sup>0,2</sup>B<sup>+</sup> ions from MS/MS spectrum, the signal-to-noise ratio can be improved up to 500 times, resulting in higher capacity of identification. Combined with relative retention time, characteristic diagnostic fragment ions, literature data and standard substance comparison, flavonoid subclass skeleton was unambiguously ascertained, with a total of 23 flavonoids (15 first reported) identified from HYF. Furthermore, quality of HYF was evaluated by high-performance liquid chromatography fingerprinting and integrated chemometrics. The similarity (> 0.944) indicated the stable quality of 20 HYF batches. Four potential quality markers including neoeriocitrin, naringin, hesperidin and neohesperidin were screened and quantified with high sensitivity (LOD, 0.039–0.442 μg/mL), satisfying precision and repeatability (RSD < 2.88 %), and pinpoint accuracy (recovery, 97.72 %–100.44 %). These markers exhibited high content levels ranging from 0.133 %–1.479 %, 3.637 %–5.146 %, 0.021 %–1.422 % and 4.978 %–9.756 %, which were closely linked to the quality of HYF that fluctuated at different growth stages. This research may offer a novel strategy and comprehensive guideline for quality evaluating of HYF and other herbal materials containing flavonoids.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113204"},"PeriodicalIF":4.9,"publicationDate":"2025-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143562300","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}

引用次数: 0

Preparation of low fluorescence loss Multishell-QDs@SiO2-COOH and its application to quantitative immunoassay

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-02-28 DOI: 10.1016/j.microc.2025.113217

Qingzhen Liu , Jinjie Li , Xinlin Yu , Yujie Lu , Ziyi Wu , Leqian Hu

The demand for precise and sensitive detection has promoted the rapid development of QDs with good biocompatibility. QDs modified with silicon dioxide can effectively isolate the external environment without affecting the fluorescence performance of QDs while endowing them with biocompatibility. However, the existing silica modification methods suffers from significant fluorescence loss and relatively poor stability of QDs. In this paper, multishell-QDs@SiO₂-COOH (MS-QDs@SiO₂-COOH) with low fluorescence loss (quantum yield reduction value is about 11 %) is successfully prepared by using high self-fluorescence stability core/multishell QDs in the reverse microemulsion system. By adjusting the content of silicon source and the ratio of carboxylation reagent, the thickness of silica shell within the range of 6–12 nm and the carboxyl groups on the surface can be controlled, and MS-QDs@SiO₂-COOH has good stability, which can meet the detection applications requirements with different particle sizes and carboxyl content. Using the prepared MS-QDs@SiO₂-COOH as a fluorescent labeling material, the construction of a quantum dot-based fluorescence-linked immunosorbent assay (QLISA) has successfully achieved quantitative detection of C-reactive protein, showing a good linear relationship (R² = 0.992) in a wide range of 1–2000 ng/mL, with a detection limit of 0.9 ng/mL, and good recovery rates of 92.8–102.4 %. This study provides a new method for the application of QDs in quantitative detection.

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引用次数: 0

Advanced 2D material sensors for diabetes management: A comparative analysis in blood serum and urine of diabetic and non-diabetic individuals 用于糖尿病管理的先进二维材料传感器：糖尿病患者和非糖尿病患者血清和尿液中的对比分析

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-02-28 DOI: 10.1016/j.microc.2025.113195

Gowhar A. Naikoo , Mustri Bano , Fatima Ba Omar , Jahangir Ahmad Rather , Israr U. Hassan

Glucose sensing is essential in managing diabetes mellitus, as it permits real-time monitoring of blood sugar level, which is imperative for effective disease control and the prevention of complications. Herein,the MoS₂ and NiS@MoS₂ 2D materials were evaluated for the glucose detection in real biological samples such as blood serum and urine samples of diabetic and non-diabetic individuals. The NiS@MoS₂ fabricated electrode has demonstrated outstanding electrocatalytic performance for oxidation of glucose molecules in 1.0 molL^-1 in alkaline medium, owing to the existence of well-exposed electroactive sites, quick transit of catalysis-relevant species, and a high synergistic catalytic impact between NiS and MoS₂ materials. The NiS@MoS₂-GCE modified electrode was electrochemically characterized using cyclic voltametriy (CV) and electrochemical impedance spectroscopy (EIS) studies, which revealed the ecellent conductivity of NiS@MoS₂ material than MoS₂ material. The fabricated glucose sensor performed well in amperometric and differential pulse voltametric (DPV) studies, with low detection limits (6.4 nM and 5.8 nM) and a wider linear range (from 0.01 µM to 0.20 µM[Glucose]). The suggested sensor demonstrated long-term stability, reproducibility, selectivity, and a promising potential application for detecting a glucose concentration in real biological samples such as blood serum and urine of diabetic and non-diabetic individuals.

{"title":"Advanced 2D material sensors for diabetes management: A comparative analysis in blood serum and urine of diabetic and non-diabetic individuals","authors":"Gowhar A. Naikoo , Mustri Bano , Fatima Ba Omar , Jahangir Ahmad Rather , Israr U. Hassan","doi":"10.1016/j.microc.2025.113195","DOIUrl":"10.1016/j.microc.2025.113195","url":null,"abstract":"<div><div>Glucose sensing is essential in managing diabetes mellitus, as it permits real-time monitoring of blood sugar level, which is imperative for effective disease control and the prevention of complications. Herein,the MoS<sub>2</sub> and NiS@MoS<sub>2</sub> 2D materials were evaluated for the glucose detection in real biological samples such as blood serum and urine samples of diabetic and non-diabetic individuals. The NiS@MoS<sub>2</sub> fabricated electrode has demonstrated outstanding electrocatalytic performance for oxidation of glucose molecules in 1.0 molL<sup>-1</sup> in alkaline medium, owing to the existence of well-exposed electroactive sites, quick transit of catalysis-relevant species, and a high synergistic catalytic impact between NiS and MoS<sub>2</sub> materials. The NiS@MoS<sub>2</sub>-GCE modified electrode was electrochemically characterized using cyclic voltametriy (CV) and electrochemical impedance spectroscopy (EIS) studies, which revealed the ecellent conductivity of NiS@MoS<sub>2</sub> material than MoS<sub>2</sub> material. The fabricated glucose sensor performed well in amperometric and differential pulse voltametric (DPV) studies, with low detection limits (6.4 nM and 5.8 nM) and a wider linear range (from 0.01 µM to 0.20 µM[Glucose]). The suggested sensor demonstrated long-term stability, reproducibility, selectivity, and a promising potential application for detecting a glucose concentration in real biological samples such as blood serum and urine of diabetic and non-diabetic individuals.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113195"},"PeriodicalIF":4.9,"publicationDate":"2025-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143561913","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}

引用次数: 0

Deep eutectic solvent-functionalized metal-organic frameworks in sorptive extraction techniques and their applications – A review 吸附萃取技术中的深共晶溶剂功能化金属有机框架及其应用--综述

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-02-28 DOI: 10.1016/j.microc.2025.113201

Wajid Ali Khan , Muhammad Balal Arain , Sana Balal , Afsaneh Mollahosseini , Mustafa Soylak

Metal-organic frameworks (MOFs) are porous adsorbents that get much attention in sorptive extraction techniques due to the availability of various structures and properties. MOFs are functionalized with a variety of materials to enhance their extraction ability. Green deep eutectic solvents (DESs) are an emerging solvent for MOF functionalization. Functionalization of MOFs with green deep eutectic solvents (DESs) improves the porosity, structural properties, active sites, hydrogen bonding capability, reusability, and extraction efficiency of deep eutectic solvent-functionalized metal–organic frameworks (DES@MOFs). This review briefly examines the benefits and drawbacks of MOF materials. In addition, the promising properties, classification, and preparation approaches for DESs are discussed in detail. This review also emphasizes the various sorptive extraction techniques, including solid-phase extraction (SPE), solid-phase microextraction (SPME), and magnetic solid-phase extraction (MSPE) reported DES@MOFs as a sorbent for a variety of analytes. A comparative analysis is presented to determine which technique is most appropriate among the reported techniques. Furthermore, the applications of DES@MOFs in pharmaceutical, dye, heavy metal, and pesticide analysis are discussed in various aspects and summarized in a table.

{"title":"Deep eutectic solvent-functionalized metal-organic frameworks in sorptive extraction techniques and their applications – A review","authors":"Wajid Ali Khan , Muhammad Balal Arain , Sana Balal , Afsaneh Mollahosseini , Mustafa Soylak","doi":"10.1016/j.microc.2025.113201","DOIUrl":"10.1016/j.microc.2025.113201","url":null,"abstract":"<div><div>Metal-organic frameworks (MOFs) are porous adsorbents that get much attention in sorptive extraction techniques due to the availability of various structures and properties. MOFs are functionalized with a variety of materials to enhance their extraction ability. Green deep eutectic solvents (DESs) are an emerging solvent for MOF functionalization. Functionalization of MOFs with green deep eutectic solvents (DESs) improves the porosity, structural properties, active sites, hydrogen bonding capability, reusability, and extraction efficiency of deep eutectic solvent-functionalized metal–organic frameworks (DES@MOFs). This review briefly examines the benefits and drawbacks of MOF materials. In addition, the promising properties, classification, and preparation approaches for DESs are discussed in detail. This review also emphasizes the various sorptive extraction techniques, including solid-phase extraction (SPE), solid-phase microextraction (SPME), and magnetic solid-phase extraction (MSPE) reported DES@MOFs as a sorbent for a variety of analytes. A comparative analysis is presented to determine which technique is most appropriate among the reported techniques. Furthermore, the applications of DES@MOFs in pharmaceutical, dye, heavy metal, and pesticide analysis are discussed in various aspects and summarized in a table.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113201"},"PeriodicalIF":4.9,"publicationDate":"2025-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143534676","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}

引用次数: 0

A label-free CRISPR/Cas12a-dimeric G-quadruplex/thioflavin T aptasensor for the sensitive detection of deoxynivalenol

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-02-28 DOI: 10.1016/j.microc.2025.113202

Huang Dai , Junlan Yu , Run Zhou , Guijie Hao , Zhaohui Qiao , Haiyang Gu , Xin Liu , Jie Bi , Jiahua Wang , Xiaodan Liu , Fuwei Pi , Yafang Shen

Rapid detection of deoxynivalenol (DON) is crucial for food safety. Herein, a highly sensitive method integrating recombinase polymerase amplification (RPA)-CRISPR/Cas12a with dimeric G-quadruplex (G₄) was developed for DON detection. In this method, DON was specifically recognized by an aptamer, resulting in the release of a complementary DNA (cDNA) which initially hybridized with the aptamer on the well of a microplate. The released cDNA in the supernatant was sucked out of the microplate, amplified through RPA and activated Cas12a for the trans-cleavage of G₄. The disruption of the dimeric G₄/thioflavin T (ThT) structures resulted in a significant fluorescence decrease for DON detection. The CRISPR/Cas12a system with excellent specificities, the RPA with efficient amplification capabilities and the dimeric G₄/ThT with admirable fluorescent properties induced synergistic effects and remarkably enhanced the detection performance with a low detection limit of 0.0539 ng/mL. The whole detection time of the assay was approximately 1.5 h. Moreover, the minimal content of DON that could be detected in rice flour and corn flour was 2.5 μg/kg. This method offers a promising alternative for DON detection and broadens the application of the CRISPR technique for non-nucleic acid target detection, satisfying the urgent demand in the field of grain analysis.

{"title":"A label-free CRISPR/Cas12a-dimeric G-quadruplex/thioflavin T aptasensor for the sensitive detection of deoxynivalenol","authors":"Huang Dai , Junlan Yu , Run Zhou , Guijie Hao , Zhaohui Qiao , Haiyang Gu , Xin Liu , Jie Bi , Jiahua Wang , Xiaodan Liu , Fuwei Pi , Yafang Shen","doi":"10.1016/j.microc.2025.113202","DOIUrl":"10.1016/j.microc.2025.113202","url":null,"abstract":"<div><div>Rapid detection of deoxynivalenol (DON) is crucial for food safety. Herein, a highly sensitive method integrating recombinase polymerase amplification (RPA)-CRISPR/Cas12a with dimeric G-quadruplex (G<sub>4</sub>) was developed for DON detection. In this method, DON was specifically recognized by an aptamer, resulting in the release of a complementary DNA (cDNA) which initially hybridized with the aptamer on the well of a microplate. The released cDNA in the supernatant was sucked out of the microplate, amplified through RPA and activated Cas12a for the <em>trans</em>-cleavage of G<sub>4</sub>. The disruption of the dimeric G<sub>4</sub>/thioflavin T (ThT) structures resulted in a significant fluorescence decrease for DON detection. The CRISPR/Cas12a system with excellent specificities, the RPA with efficient amplification capabilities and the dimeric G<sub>4</sub>/ThT with admirable fluorescent properties induced synergistic effects and remarkably enhanced the detection performance with a low detection limit of 0.0539 ng/mL. The whole detection time of the assay was approximately 1.5 h. Moreover, the minimal content of DON that could be detected in rice flour and corn flour was 2.5 μg/kg. This method offers a promising alternative for DON detection and broadens the application of the CRISPR technique for non-nucleic acid target detection, satisfying the urgent demand in the field of grain analysis.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113202"},"PeriodicalIF":4.9,"publicationDate":"2025-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143547824","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}

引用次数: 0

Fluorescence sensor array based on pore-size sieving effect of Zr-MOFs for monitoring ATP hydrolysis and ATP-related physiological phosphates

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-02-28 DOI: 10.1016/j.microc.2025.113219

Xiaoyan Niu , Jiahui Zhang , Zhen Wang , Huaiyu Bu , Gang Xie

Monitoring the hydrolysis of adenosine triphosphate (ATP) and differentiating its associated phosphates are critical but challenging. Herein, we presented a high-throughput fluorescence sensor array based on three zirconium metal–organic frameworks (Zr-MOFs), namely PCN-221, PCN-222, and PCN-224, with different topological structures and pore sizes for the accurate recognition of ATP-related phosphates. Initially, these Zr-MOFs exhibit weak fluorescence due to ligand-to-metal charge transfer (LMCT) phenomenon. Interestingly, interaction between Zr clusters and phosphates enhance the fluorescence of Zr-MOFs, because the formation of robust Zr-O-P bonds effectively disrupt the LMCT process. Notably, benefiting from the pore-size screening effects of three Zr-MOFs, meanwhile, ATP-related phosphates with different phosphate group numbers, molecular sizes, and steric effects could alter the LMCT of each Zr-MOF to varying degrees, leading to the diverse fluorescence responses. Consequently, this multi-dimensional sensor array generates unique fluorescence “fingerprints” for precise identification of ATP-related phosphates rely on the modulating MOF-phosphate interactions, along with real-time ATP hydrolysis monitoring. Moreover, the proposed array achieved superior sensitivity and anti-interference capabilities, even for multi-component phosphate detection in complex biological environments. This study not only provides a versatile tool for investigating ATP hydrolysis, but also opens new avenues for MOF-based multimolecular detection in biological sensing applications.

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引用次数: 0

Sustainable and scalable detection: Paper-based analytical devices and miniaturized detection systems for modern diagnostics

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-02-28 DOI: 10.1016/j.microc.2025.113210

Ahmed Isa , Mahdi Gharibi , Ahmet Cetinkaya , Sibel A. Ozkan

The evolution of detection systems has played a transformative role in advancing healthcare, particularly through the emergence of paper-based analytical devices (PAD) and miniaturized detection systems (MDS). These innovative platforms address critical challenges associated with traditional diagnostic methods, including high costs, complexity, and limited accessibility. This review explores the historical progression and the growing motivations driving the development of paper-based and miniaturized technologies. A comprehensive analysis of fabrication methodologies and characterization techniques underscores these systems’ engineering precision and adaptability. Key detection technologies, including electrochemical methods, colorimetric, and other advanced approaches, are critically examined, emphasizing their selectivity and adaptability. The integration of these technologies into point-of-care diagnostics, environmental health monitoring, and personalized medicine underscores their transformative potential and broad applicability. The applications of MDS and paper-based platforms are reviewed across diverse domains, focusing on detecting bacteria, viruses, biomarkers, and molecules critical to food safety. A comprehensive table encapsulates these applications, highlighting their wide-ranging impact. Looking ahead, this review explores emerging trends and challenges, providing insights into the future development of detection systems to improve healthcare accessibility and efficiency. In this review, recent studies using PAD and MDS for modern diagnosis of specific analytes in biological samples during the period between 2009 and 2024 were discussed in detail.

{"title":"Sustainable and scalable detection: Paper-based analytical devices and miniaturized detection systems for modern diagnostics","authors":"Ahmed Isa , Mahdi Gharibi , Ahmet Cetinkaya , Sibel A. Ozkan","doi":"10.1016/j.microc.2025.113210","DOIUrl":"10.1016/j.microc.2025.113210","url":null,"abstract":"<div><div>The evolution of detection systems has played a transformative role in advancing healthcare, particularly through the emergence of paper-based analytical devices (PAD) and miniaturized detection systems (MDS). These innovative platforms address critical challenges associated with traditional diagnostic methods, including high costs, complexity, and limited accessibility. This review explores the historical progression and the growing motivations driving the development of paper-based and miniaturized technologies. A comprehensive analysis of fabrication methodologies and characterization techniques underscores these systems’ engineering precision and adaptability. Key detection technologies, including electrochemical methods, colorimetric, and other advanced approaches, are critically examined, emphasizing their selectivity and adaptability. The integration of these technologies into point-of-care diagnostics, environmental health monitoring, and personalized medicine underscores their transformative potential and broad applicability. The applications of MDS and paper-based platforms are reviewed across diverse domains, focusing on detecting bacteria, viruses, biomarkers, and molecules critical to food safety. A comprehensive table encapsulates these applications, highlighting their wide-ranging impact. Looking ahead, this review explores emerging trends and challenges, providing insights into the future development of detection systems to improve healthcare accessibility and efficiency. In this review, recent studies using PAD and MDS for modern diagnosis of specific analytes in biological samples during the period between 2009 and 2024 were discussed in detail.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113210"},"PeriodicalIF":4.9,"publicationDate":"2025-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143548562","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}

引用次数: 0

Optimization of CRISPR/Cas12f1 guide RNAs using AlphaFold 3 for enhanced nucleic acid detection 利用 AlphaFold 3 优化 CRISPR/Cas12f1 引导 RNA，增强核酸检测能力

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-02-28 DOI: 10.1016/j.microc.2025.113194

Lulu Pan , Yongcheng Ma , Rui Sang , Xia Lu , Xiaxia Fan , Ming Li , Qianfei Zuo , Aifeng Wang , Fei Deng

The CRISPR/Cas12f1 system, known for its unique trans-cleavage activity, has emerged as a promising tool for nucleic acid detection. However, the optimization of guide RNAs in Cas12f1 remains a critical challenge. This study employs AlphaFold 3, a cutting-edge AI-driven structural prediction tool, to increase the trans-cleavage efficiency of Cas12f1 ribonucleoprotein (RNP) complexes through strategic guide RNA modifications. Initial structural simulations of wild-type tracrRNA and crRNA sequences revealed unexpected pairing within tracrRNA, which disrupted its interaction with crRNA, thereby reducing Cas12f1 activity. To address this, we truncated the 3′ end of tracrRNA, eliminating disruptive pairing and significantly improving the system’s trans-cleavage activity. To this end, we designed a single guide RNA (sgRNA) by linking the optimized tracrRNA and crRNA. Structural simulations confirmed that the sgRNA formed stable duplexes between tracrRNA and crRNA parts similar to those in the optimized tracrRNA-crRNA complex. Compared with the truncated tracrRNA system, the sgRNA further increased the trans-cleavage activity of the Cas12f1 RNP, with improved sensitivity compared to the truncated tracrRNA system. These findings underscore the potential of structure-based guide RNA optimization via AlphaFold 3 to advance the development of more efficient CRISPR/Cas12f1 biosensing systems for nucleic acid detection. This approach offers a novel and effective strategy for improving the performance of CRISPR-based technologies in various diagnostic applications.

{"title":"Optimization of CRISPR/Cas12f1 guide RNAs using AlphaFold 3 for enhanced nucleic acid detection","authors":"Lulu Pan , Yongcheng Ma , Rui Sang , Xia Lu , Xiaxia Fan , Ming Li , Qianfei Zuo , Aifeng Wang , Fei Deng","doi":"10.1016/j.microc.2025.113194","DOIUrl":"10.1016/j.microc.2025.113194","url":null,"abstract":"<div><div>The CRISPR/Cas12f1 system, known for its unique <em>trans</em>-cleavage activity, has emerged as a promising tool for nucleic acid detection. However, the optimization of guide RNAs in Cas12f1 remains a critical challenge. This study employs AlphaFold 3, a cutting-edge AI-driven structural prediction tool, to increase the <em>trans</em>-cleavage efficiency of Cas12f1 ribonucleoprotein (RNP) complexes through strategic guide RNA modifications. Initial structural simulations of wild-type tracrRNA and crRNA sequences revealed unexpected pairing within tracrRNA, which disrupted its interaction with crRNA, thereby reducing Cas12f1 activity. To address this, we truncated the 3′ end of tracrRNA, eliminating disruptive pairing and significantly improving the system’s <em>trans</em>-cleavage activity. To this end, we designed a single guide RNA (sgRNA) by linking the optimized tracrRNA and crRNA. Structural simulations confirmed that the sgRNA formed stable duplexes between tracrRNA and crRNA parts similar to those in the optimized tracrRNA-crRNA complex. Compared with the truncated tracrRNA system, the sgRNA further increased the <em>trans</em>-cleavage activity of the Cas12f1 RNP, with improved sensitivity compared to the truncated tracrRNA system. These findings underscore the potential of structure-based guide RNA optimization via AlphaFold 3 to advance the development of more efficient CRISPR/Cas12f1 biosensing systems for nucleic acid detection. This approach offers a novel and effective strategy for improving the performance of CRISPR-based technologies in various diagnostic applications.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113194"},"PeriodicalIF":4.9,"publicationDate":"2025-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143529784","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}

引用次数: 0