{"title":"Development of an HPLC device with water/acetonitrile with NaCl mixed solution that induces a phase-separation multiphase flow as the eluent in the separation column","authors":"Ryuto Hirose, Takeshi Iharada, Kazuhiko Tsukagoshi","doi":"10.1007/s44211-024-00599-3","DOIUrl":"10.1007/s44211-024-00599-3","url":null,"abstract":"<div><p>We developed a novel HPLC device where the phase-separation multiphase flow worked as the eluent in the separation column by using a water/acetonitrile/ethyl acetate triple mixed solution as a dual-phase-separation solution. Dual-phase-separation solutions form a phase-separation multiphase flow in a microscopic space. The new separation mechanism in the HPLC is called phase-separation mode. In this study, we used water and acetonitrile with NaCl mixed solution as a dual-phase-separation solution instead of the triple mixed solution. Octadecylsilyl (ODS)-modified particle- and porous silica particle-packed separation columns were united with the HPLC device for phase-separation mode caused by phase-separation multiphase flow. NA (1-naphthol) and NDS (2,6-naphthalenedisulfonic acid) were analyzed by the device as model sample. Using the water and acetonitrile with NaCl mixed solution at the solvent volume ratio of 5:5, NA and NDS were not separated on either column at 25 °C. On the other hand, they were separated with the order NDS and NA on the ODS column and separated with the order NA and NDS on the silica column in phase-separation mode at 0 °C. We discuss the separation mechanism of phase-separation mode using the water and acetonitrile with NaCl mixed solution at 0 °C.</p><h3>Graphical abstract</h3><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":7802,"journal":{"name":"Analytical Sciences","volume":"40 9","pages":"1779 - 1785"},"PeriodicalIF":1.8,"publicationDate":"2024-05-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141154309","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Fundamental investigation on fluorous nanoemulsion optodes: effect of matrix fluorination on selectivity","authors":"Soraka Iwamoto, Kenji Sueyoshi, Tatsuro Endo, Hideaki Hisamoto","doi":"10.1007/s44211-024-00603-w","DOIUrl":"10.1007/s44211-024-00603-w","url":null,"abstract":"<div><p>As fundamental investigation on fluorous nanoemulsion (NE) optodes for highly selective perfluorooctanesulfonate (PFOS<sup>−</sup>) sensing, the effect of matrix fluorination on selectivity was investigated. Due to the high hydrophobicity of PFOS<sup>−</sup> itself, it responded in exhaustive mode regardless of the fluorination ratio of the matrix, and the lowest detectable PFOS<sup>−</sup> concentration was on the order of 10<sup>−7</sup> to 10<sup>−6</sup> M. On the other hand, the response of non-fluorous interfering anions was suppressed as the fluorination ratio of the matrix increased. It was revealed that the relative selectivity of PFOS<sup>−</sup> for hydrophobic anions, ClO<sub>4</sub><sup>−</sup>, SCN<sup>−</sup>, and 1-octanesulfonate (OS<sup>−</sup>) was improved by more than one order of magnitude, up to nearly two orders of magnitude, and that it was also improved by less than one order of magnitude for hydrophilic anions, Br<sup>−</sup>, Cl<sup>−</sup>, and SO<sub>4</sub><sup>−</sup>, in logarithmic selectivity coefficient (log <span>({K}_{{PFOS}^{-}, j}^{opt})</span>).</p><h3>Graphical abstract</h3><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":7802,"journal":{"name":"Analytical Sciences","volume":"40 9","pages":"1787 - 1792"},"PeriodicalIF":1.8,"publicationDate":"2024-05-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141096827","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Ou Sha, Yunfan Wu, Xincheng Dai, Huiwen Li, Yuan Xu, Ziwen Wang, Pu Zhang
{"title":"Reusable magnetic molecular imprinted polymers based on magnetic graphene oxide for selective identification and detection of eugenol in environmental water samples","authors":"Ou Sha, Yunfan Wu, Xincheng Dai, Huiwen Li, Yuan Xu, Ziwen Wang, Pu Zhang","doi":"10.1007/s44211-024-00601-y","DOIUrl":"10.1007/s44211-024-00601-y","url":null,"abstract":"<div><p>In this study, a reliable method for determining eugenol content in environmental water samples was established by combining magnetic solid-phase extraction with high-performance liquid chromatography. Magnetic molecular imprinted polymers MGO@MIPs were prepared through surface molecular imprinting technique with eugenol as the template molecule. The material displayed good superparamagnetic properties and magnetic responsiveness in favor of rapid separation. The adsorption properties of MGO@MIPs for eugenol were evaluated through adsorption kinetics and selectivity experiments. MGO@MIPs were found to have favorable reusability and obvious selectivity for eugenol. In addition, adsorption and elution conditions were investigated. Under optimal conditions, a linear relationship was obtained between the concentration of eugenol and its peak area in the range of 0.02–5 mg/L (<i>R</i><sup>2</sup> = 0.9998) and the limit of detection was 4.0 × 10<sup>–6</sup> mg/mL. The performance of the established method was assessed with the average recovery of 96.59–102.20% and the relative standard deviation (RSD) below 3.5%. The application of this method provides a new perspective for the separation, enrichment and detection of eugenol in water environment.</p><h3>Graphical abstract</h3><p>Preparation of the molecularly imprinted polymers</p>\u0000<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":7802,"journal":{"name":"Analytical Sciences","volume":"40 9","pages":"1629 - 1639"},"PeriodicalIF":1.8,"publicationDate":"2024-05-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141096829","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Derivatization to generate a product ion containing analyte-specific moiety in ESI–MS/MS","authors":"Tatsuya Higashi","doi":"10.1007/s44211-024-00567-x","DOIUrl":"10.1007/s44211-024-00567-x","url":null,"abstract":"","PeriodicalId":7802,"journal":{"name":"Analytical Sciences","volume":"40 6","pages":"973 - 974"},"PeriodicalIF":1.8,"publicationDate":"2024-05-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141092696","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Enhanced synthesis of antibody-functionalized gold nanoparticles for multiplexed exosome detection via mass signal amplification in LDI-TOF MS","authors":"Gaon Jo, Woon-Seok Yeo","doi":"10.1007/s44211-024-00604-9","DOIUrl":"10.1007/s44211-024-00604-9","url":null,"abstract":"<div><p>We present a novel method for sensitive exosomal protein detection using organic matrix-free laser desorption/ionization time-of-flight mass spectrometry (LDI-TOF MS) and gold nanoparticles (AuNPs) functionalized with mass tags for signal amplification (Am-tags). Target exosomes were captured by specific antibodies on AuNPs and a biochip, where the antibody-presenting AuNPs (Ab/Am-tag@AuNPs) contained excess Am-tags. LDI-TOF MS analysis revealed the mass signal of Am-tags on Ab/Am-tag@AuNPs, indicating the presence of target exosomes. Thus, the target signal was amplified by a large number of Am-tags, resulting in enhanced sensitivity. We optimized the protocol to prepare stable Ab/Am-tag@AuNPs, focusing on parameters such as the concentration and ratio of thiol molecules for AuNP functionalization, suitable solvents for the coupling reaction, and amount of antibodies conjugated to the AuNPs. Subsequently, we evaluated the ability of our method to detect exosomes isolated from three cell lines, NIH3T3, MCF7, and HeLa, using an anti-Rab5 immobilized gold chip and anti-CD63/Am-tag@AuNPs with LDI-TOF MS analysis. Calibration curves constructed for the three cell lines showed a linear relationship with an excellent limit of detection. Finally, we emphasized the versatility of our method for the quantitative detection of exosomal proteins CD63 and mucin 1 (MUC1) using two types of Am-tags. LDI-TOF MS analysis revealed the presence of CD63 and MUC1 at different expression levels in HeLa and MCF7 cancer cells. Our findings clearly indicate the potential of Ab/Am-tag@AuNPs as a sensitive and reliable approach for identifying biomarkers in exosomes, providing valuable insights into their utility in biomedical research and clinical settings.</p><h3>Graphical abstract</h3>\u0000<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":7802,"journal":{"name":"Analytical Sciences","volume":"40 9","pages":"1663 - 1670"},"PeriodicalIF":1.8,"publicationDate":"2024-05-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141080454","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"A high-throughput sequence determination for one cyclic peptide immobilized on a single bead by the one-pot cyanidation followed by MALDI-TOF–MS/MS for discovery of interacting peptides","authors":"Takeshi Kasama, Kiyoshi Nokihara","doi":"10.1007/s44211-024-00594-8","DOIUrl":"10.1007/s44211-024-00594-8","url":null,"abstract":"<div><p>One cyclic peptide immobilized on one gel-type bead has been employed for the discovery of both interacting peptides and/or medicinal medium-sized molecules. Although high-throughput characterization of recognized peptides has been a bottleneck, here, we describe direct liberation from beads by a one-pot reaction using 2-nitro-5-thiocyanatobenzoic acid followed by mass spectrometry to realize faster and routine sequencing of the peptide on the beads. This is useful for the investigation of protein–protein interactions as well as discovery of drug candidates.</p><h3>Graphical abstract</h3>\u0000<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":7802,"journal":{"name":"Analytical Sciences","volume":"40 7","pages":"1219 - 1223"},"PeriodicalIF":1.8,"publicationDate":"2024-05-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141074584","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Optical lateral flow assays in early diagnosis of SARS-CoV-2 infection","authors":"Rushi Liang, Aiping Fan, Feiqian Wang, Yajing Niu","doi":"10.1007/s44211-024-00596-6","DOIUrl":"10.1007/s44211-024-00596-6","url":null,"abstract":"<div><p>So far, the 2019 novel coronavirus (COVID-19) is spreading widely worldwide. The early diagnosis of infection by the severe acute respiratory syndrome coronavirus-2 (SARS-CoV-2) is essential to provide timely treatment and prevent its further spread. Lateral flow assays (LFAs) have the advantages of rapid detection, simple operation, low cost, ease of mass production, and no need for special devices and professional operators, which make them suitable for self-testing at home. This review focuses on the early diagnosis of SARS-CoV-2 infection based on optical LFAs including colorimetric, fluorescent (FL), chemiluminescent (CL), and surface-enhanced Raman scattering (SERS) LFAs for the detection of SARS-CoV-2 antigens and nucleic acids. The types of recognition components, detection modes used for antigen detection, labels employed in different optical LFAs, and strategies to improve the detection sensitivity of LFAs were reviewed. Meanwhile, LFAs coupled with different nucleic acid amplification techniques and CRISPR–Cas systems for the detection of SARS-CoV-2 nucleic acids were summarized. We hope this review provides research mentalities for developing highly sensitive LFAs that can be used in home self-testing for the early diagnosis of SARS-CoV-2 infection.</p><h3>Graphical abstract</h3><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":7802,"journal":{"name":"Analytical Sciences","volume":"40 9","pages":"1571 - 1591"},"PeriodicalIF":1.8,"publicationDate":"2024-05-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140955543","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Comprehensive extraction study using N,N-dioctylthiodiglycolamic acid: effect of S donor on metal extraction","authors":"Kojiro Shimojo, Iori Fujiwara, Takumi Saito, Tatsuya Oshima","doi":"10.1007/s44211-024-00577-9","DOIUrl":"10.1007/s44211-024-00577-9","url":null,"abstract":"<div><p>Extraction ability of <i>N,N</i>-dioctylthiodiglycolamic acid (T-DODGAA), a soft-base sulfur donor ligand with an amide group and a carboxylic acid connected by a thioether chain, for 56 metal ions have been comprehensively investigated and compared with that of <i>N,N</i>-dioctyldiglycolamic acid (DODGAA) with an etheric oxygen atom, a hard-base donor. The acid dissociation constant (p<i>K</i><sub>a</sub>) of the thiodiglycolamic acid framework was determined to be 3.71 ± 0.06 in water (0.1 M LiCl, 25 °C) by potentiometric titration, indicating that T-DODGAA is a slightly weaker acid than DODGAA (p<i>K</i><sub>a</sub> = 3.54 ± 0.03). T-DODGAA can quantitatively extract various metal ions from the 56 metal ions into the organic phase (isooctane) through a proton-exchange reaction. T-DODGAA provided higher extraction performance than DODGAA for Hf(IV), Cr(III), Fe(III), Ni(II), Cu(II), Pd(II), Ag(I), Au(III), Hg(II), Al(III), and Ga(III), especially for soft metal ions. Furthermore, to demonstrate the practical feasibility of T-DODGAA for hydrometallurgy and metal recycling, we performed selective separation tests of rare metal ions such as Sc(III), Ni(II), Co(II), Pd(II), Au(III), In(III), and Ga(III) in metal-mixed extraction systems.</p><h3>Graphical abstract</h3>\u0000<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":7802,"journal":{"name":"Analytical Sciences","volume":"40 8","pages":"1429 - 1436"},"PeriodicalIF":1.8,"publicationDate":"2024-05-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140943764","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Application of on-line sample preconcentration by large-volume dual preconcentration by isotachophoresis and stacking (LDIS) on straight-channel microchips","authors":"Fumihiko Kitagawa, Kazuki Takahashi, Reina Osanai, Ryota Sasaki, Takayuki Kawai","doi":"10.1007/s44211-024-00597-5","DOIUrl":"10.1007/s44211-024-00597-5","url":null,"abstract":"<div><p>In this study, large-volume dual preconcentration by isotachophoresis and stacking (LDIS) which is an on-line sample preconcentration technique coupling large-volume sample stacking with an electroosmotic flow pump (LVSEP) with transient isotachophoresis (tITP) was applied to microchip electrophoresis (MCE) for improving both detection sensitivities and peak shapes. To realize LDIS in MCE, we investigated experimental procedures for injecting a short plug of a leading electrolyte (LE) solution into a straight microchannel without any sophisticated injector apparatus. We found that a short LE plug could be injected into a sample-filled straight-channel only by making the liquid level of the LE solution in an outlet reservoir higher than that in an inlet one. By applying a reversed-polarity voltage to the microchip, anionic analytes injected throughout the microchannel were first enriched by LVSEP, followed by tITP. Through the second preconcentration effect by tITP in LDIS, sensitivity enhancement factor (SEF) and asymmetry factor for a standard dye were improved from 878 and 0.62 to 1330 and 1.14, respectively, relative to those in conventional LVSEP. It should be noted that more viscous running buffer containing sieving polymers could be employed to the LDIS analysis, which was effective for improving the SEF and the separation efficiencies, especially for bio-polymeric compounds. Finally, LDIS was applied to the oligosaccharide and protein analyses in MCE, resulting in the SEFs of 1410 and <i>ca</i>. 50 for maltotriose and bovine milk casein, respectively.</p><h3>Graphical Abstract</h3>\u0000<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":7802,"journal":{"name":"Analytical Sciences","volume":"40 9","pages":"1611 - 1617"},"PeriodicalIF":1.8,"publicationDate":"2024-05-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140943791","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Teruki Nii, Shoichi Hijii, Ryosuke Kaneko, Kenta Tanito, Kota Yamanaka, Akihiro Kishimura, Takeshi Mori, Yoshiki Katayama
{"title":"In vitro evaluation of novel SN-38 prodrug activated by α-rhamnosidase of exogenous enzyme","authors":"Teruki Nii, Shoichi Hijii, Ryosuke Kaneko, Kenta Tanito, Kota Yamanaka, Akihiro Kishimura, Takeshi Mori, Yoshiki Katayama","doi":"10.1007/s44211-024-00593-9","DOIUrl":"10.1007/s44211-024-00593-9","url":null,"abstract":"<div><p>This study introduces the α-rhamnose (Rham)-conjugated prodrug of SN-38 (Rham-SN-38) as a promising alternative to irinotecan. α-rhamnosidase, responsible for SN-38 release from Rham-SN-38, does not express in human cells, minimizing individual variability and side effects. The injection of the α-rhamnosidase into the tumor tissues makes it possible, for the first time, to activate the Rham-SN-38. Furthermore, α-rhamnosidase demonstrates significantly higher activity than carboxylesterase, the specific enzyme activating irinotecan. SN-38 release mediated by α-rhamnosidase completes within 2 h, with a <i>k</i><sub><i>cat</i></sub>/K<sub>m</sub> value approximately 5.0 × 10<sup>4</sup>-fold higher than that of irinotecan. The 50% inhibition concentration (IC<sub>50</sub>) of Rham-SN-38 against three types of cancer cells and one normal cell exceeds 4.5 × 10<sup>3</sup> nM. The addition of α-rhamnosidase significantly increases cytotoxicity, with IC<sub>50</sub> comparable to free SN-38. The QIC<sub>50</sub>, an index reflecting the difference in cytotoxicity with and without α-rhamnosidase, exceeds approximately 1.0 × 10<sup>2</sup>-fold. Rham-SN-38, synthesized in this study, demonstrates significant potential as a prodrug for cancer therapy.</p><h3>Graphical abstract</h3>\u0000<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":7802,"journal":{"name":"Analytical Sciences","volume":"40 8","pages":"1529 - 1535"},"PeriodicalIF":1.8,"publicationDate":"2024-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140921092","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}