A method to fractionate the Pb-binding ligands (proteins, amino acids and peptides) in human amniotic fluid is reported. The method combines high-performance size exclusion chromatography (HPSEC) to fractionate Pb-bound ligands with inductively coupled plasma mass spectrometry (ICP-MS) for Pb detection and quantification. Using protein standards for HPSEC calibration, several Pb-binding ligands were identified in amniotic fluid that included ceruloplasmin, pre-albumin and a Zn-peptide.
{"title":"Determination of Pb-bound ligands in human amniotic fluid by HPSEC-ICP-MS","authors":"G. Hall, Xiangping Zhu, Eugene G. Martin","doi":"10.1039/A900478E","DOIUrl":"https://doi.org/10.1039/A900478E","url":null,"abstract":"A method to fractionate the Pb-binding ligands (proteins, amino acids and peptides) in human amniotic fluid is reported. The method combines high-performance size exclusion chromatography (HPSEC) to fractionate Pb-bound ligands with inductively coupled plasma mass spectrometry (ICP-MS) for Pb detection and quantification. Using protein standards for HPSEC calibration, several Pb-binding ligands were identified in amniotic fluid that included ceruloplasmin, pre-albumin and a Zn-peptide.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"5 1","pages":"93-95"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78685650","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
An electrostatic ion chromatography (EIC) method for the separation of inorganic anions with detection by suppressed conductivity has been developed, in which analyte retention times can be manipulated by variation of the composition of the mobile phase. A stationary phase prepared by coating silica-based octadecyl material with a sulfobetaine zwitterionic surfactant (Zwittergent 3-14) has been used in conjunction with aqueous hydroxide solutions as the mobile phase. Inorganic anions were eluted in the order SO42– < F– < Cl– < NO2– < Br– < NO3– < ClO3– < I–, with retention times increasing with increasing concentration of hydroxide in the mobile phase. Retention times were also dependent on the nature of the counter-cation in the mobile phase, with divalent cations such as Ca2+ and Ba2+ showing longer retention times than monovalent cations such as Li+ and Na+. A retention mechanism involving formation of a binary electrical double layer is proposed, with the thickness of the double layer (and hence analyte retention) being dependent on the concentration of the mobile phase. The EIC system showed high sensitivity for the analyte ions due to the efficiency of the suppression reaction. Detection limits for SO42–, F–, Cl–, NO2–, Br– and NO3– were less than 1.0 × 10–7 mol L–1, whilst those for ClO3– and I– were 3.0 × 10–7 mol L–1 and 7.0 × 10–7 mol L–1, respectively, for a sample injection volume of 100 µL.
{"title":"Electrostatic ion chromatography using hydroxide solutions as mobile phase with suppressed conductivity detection","authors":"Wenzhi Hu, P. Haddad, K. Hasebe, Kazuhiko Tanaka","doi":"10.1039/A904668B","DOIUrl":"https://doi.org/10.1039/A904668B","url":null,"abstract":"An electrostatic ion chromatography (EIC) method for the separation of inorganic anions with detection by suppressed conductivity has been developed, in which analyte retention times can be manipulated by variation of the composition of the mobile phase. A stationary phase prepared by coating silica-based octadecyl material with a sulfobetaine zwitterionic surfactant (Zwittergent 3-14) has been used in conjunction with aqueous hydroxide solutions as the mobile phase. Inorganic anions were eluted in the order SO42– < F– < Cl– < NO2– < Br– < NO3– < ClO3– < I–, with retention times increasing with increasing concentration of hydroxide in the mobile phase. Retention times were also dependent on the nature of the counter-cation in the mobile phase, with divalent cations such as Ca2+ and Ba2+ showing longer retention times than monovalent cations such as Li+ and Na+. A retention mechanism involving formation of a binary electrical double layer is proposed, with the thickness of the double layer (and hence analyte retention) being dependent on the concentration of the mobile phase. The EIC system showed high sensitivity for the analyte ions due to the efficiency of the suppression reaction. Detection limits for SO42–, F–, Cl–, NO2–, Br– and NO3– were less than 1.0 × 10–7 mol L–1, whilst those for ClO3– and I– were 3.0 × 10–7 mol L–1 and 7.0 × 10–7 mol L–1, respectively, for a sample injection volume of 100 µL.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"51 1","pages":"309-312"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75957490","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
This paper describes experimental equations that relate the dispersion coefficient to the geometry and hydrodynamic parameters of a flow injection system. Data are presented as isodispersion curves (similar to isothermal, isobar or isochore representations). The results present a correlated overview, which makes theoretical evaluation of the dispersion coefficient simple. Geometric and operational parameters for a flow injection system can be established when the dispersion is to be maintained within certain limits. The parameters addressed in this study are: tube length (100–1200 mm); tube diameter (0.3–0.8 mm); injected volume (93 µl); and volumetric flow rate (0.75–2.0 ml min–1).
本文描述了流动喷射系统中分散系数与几何参数和流体动力参数之间的关系的实验方程。数据以等色散曲线表示(类似于等温、等压线或等差线表示)。结果给出了一个相关的概述，这使得色散系数的理论计算变得简单。当分散要保持在一定范围内时，可以建立流动注射系统的几何和操作参数。本研究涉及的参数为:管长(100 - 1200mm);管径(0.3-0.8 mm);注射量(93µl);体积流速(0.75-2.0 ml min-1)。
{"title":"Isodispersion curves in flow injection analysis","authors":"D. Vãireanu, P. Fielden, R. Snook","doi":"10.1039/A909083E","DOIUrl":"https://doi.org/10.1039/A909083E","url":null,"abstract":"This paper describes experimental equations that relate the dispersion coefficient to the geometry and hydrodynamic parameters of a flow injection system. Data are presented as isodispersion curves (similar to isothermal, isobar or isochore representations). The results present a correlated overview, which makes theoretical evaluation of the dispersion coefficient simple. Geometric and operational parameters for a flow injection system can be established when the dispersion is to be maintained within certain limits. The parameters addressed in this study are: tube length (100–1200 mm); tube diameter (0.3–0.8 mm); injected volume (93 µl); and volumetric flow rate (0.75–2.0 ml min–1).","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"114 1","pages":"407-408"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79340189","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
C. Malins, H. Glever, B. MacCraith, S. Fanni, J. Vos
The synthesis of a novel ruthenium(II) polypyridyl complex incorporating silane pendant moieties is described. This fluorescent material was covalently bound to an organically modified silica glass precursor to give thin films suitable for optical oxygen sensing. These films showed good oxygen sensitivity characteristics, and possess the distinct advantage over physically entrapped dyes of being chemically attached to the support membrane. This approach to the preparation of luminescent micro-porous glass films provides sensitive membranes suitable for applications where zero dye leaching is a requirement.
{"title":"The preparation of a sol–gel glass oxygen sensor incorporating a covalently bound fluorescent dye","authors":"C. Malins, H. Glever, B. MacCraith, S. Fanni, J. Vos","doi":"10.1039/A808731H","DOIUrl":"https://doi.org/10.1039/A808731H","url":null,"abstract":"The synthesis of a novel ruthenium(II) polypyridyl complex incorporating silane pendant moieties is described. This fluorescent material was covalently bound to an organically modified silica glass precursor to give thin films suitable for optical oxygen sensing. These films showed good oxygen sensitivity characteristics, and possess the distinct advantage over physically entrapped dyes of being chemically attached to the support membrane. This approach to the preparation of luminescent micro-porous glass films provides sensitive membranes suitable for applications where zero dye leaching is a requirement.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"476 1","pages":"3-4"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77045059","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
The transmission and specular reflectance mid infra-red spectra for three polymer systems used to coat mild steel are reported. The relative absorbance of selected candidate and reference peaks show a quantitative relationship with peak metal temperature, suggesting that mid-IR spectroscopy may be useful in assessing the degree of cure or plasticisation under industrial conditions.
{"title":"The monitoring of the curing of plastic coatings on steel strip by infrared spectroscopy","authors":"Rhobert Lewis, Christopher Morgan, J. Miasik","doi":"10.1039/A903696B","DOIUrl":"https://doi.org/10.1039/A903696B","url":null,"abstract":"The transmission and specular reflectance mid infra-red spectra for three polymer systems used to coat mild steel are reported. The relative absorbance of selected candidate and reference peaks show a quantitative relationship with peak metal temperature, suggesting that mid-IR spectroscopy may be useful in assessing the degree of cure or plasticisation under industrial conditions.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"17 1","pages":"271-272"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81300514","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
M. Streďanský, A. Pizzariello, S. Stredanska, S. Miertus
An improved amperometric biosensor based on a solid binding matrix (SBM) composite transducer has been used for the determination of D-fructose in foodstuffs samples. The enzyme, D-fructose dehydrogenase (EC 1.1.99.11), was incorporated directly into a solid composite transducer containing both 2-hexadecanone as SBM and chemically modified graphite. Hexacyanoferrate(III) was used as a redox mediator and the current variation caused by the presence of D-fructose was measured amperometrically. The electrochemical properties and the characteristics of the composite fructose biosensors are described. The amperometric signals were fast, reproducible and linearly proportional to D-fructose concentrations in the range 50 × 10–6–10 × 10–3 mol l–1, with a correlation coefficient of 0.999. A set of measurements at +0.20 V versus SCE for 2 × 10–3 mol l–1D-fructose yielded a relative standard deviation for the steady-state current of 2.11%. The use of a chemically modified graphite by a mild oxidation step was shown to improve the biosensor selectivity against anionic interferents such as L-ascorbate. The biosensor proved to be stable for 6 months and the assay of D-fructose by this electrode was not influenced by the presence of sugars or other interferents commonly found in food samples. The biosensor was used for the determination of D-fructose in some food samples, and the results were consistent with those obtained with the commercially available D-fructose enzyme photometric kit.
{"title":"Determination of D-fructose in foodstuffs by an improved amperometric biosensor based on a solid binding matrix","authors":"M. Streďanský, A. Pizzariello, S. Stredanska, S. Miertus","doi":"10.1039/A900048H","DOIUrl":"https://doi.org/10.1039/A900048H","url":null,"abstract":"An improved amperometric biosensor based on a solid binding matrix (SBM) composite transducer has been used for the determination of D-fructose in foodstuffs samples. The enzyme, D-fructose dehydrogenase (EC 1.1.99.11), was incorporated directly into a solid composite transducer containing both 2-hexadecanone as SBM and chemically modified graphite. Hexacyanoferrate(III) was used as a redox mediator and the current variation caused by the presence of D-fructose was measured amperometrically. The electrochemical properties and the characteristics of the composite fructose biosensors are described. The amperometric signals were fast, reproducible and linearly proportional to D-fructose concentrations in the range 50 × 10–6–10 × 10–3 mol l–1, with a correlation coefficient of 0.999. A set of measurements at +0.20 V versus SCE for 2 × 10–3 mol l–1D-fructose yielded a relative standard deviation for the steady-state current of 2.11%. The use of a chemically modified graphite by a mild oxidation step was shown to improve the biosensor selectivity against anionic interferents such as L-ascorbate. The biosensor proved to be stable for 6 months and the assay of D-fructose by this electrode was not influenced by the presence of sugars or other interferents commonly found in food samples. The biosensor was used for the determination of D-fructose in some food samples, and the results were consistent with those obtained with the commercially available D-fructose enzyme photometric kit.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"118 1","pages":"57-61"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87654152","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
N. Torto, L. Gorton, E. Mikeladze, E. Csöregi, T. Laurell
An in-house microdialysis probe equipped with 3 different inner cannulae exhibiting different inner and outer radii was used to sample glucose, maltotriose, maltopentaose and maltoheptaose as model analytes in order to evaluate its performance by means of optimised internal probe geometry. The results were correlated to the inner cannula ratio (Rir), defined as the inner cannula’s inner radius divided by the inner cannula’s outer radius. Extraction fraction (EF) or relative recovery (RR) showed a dependency on Rir for all the investigated analytes at all the perfusion rates. The EF for glucose improved up to 10% for a nominal increase of 0.27 in Rir. The sensitivity of the EF of saccharides to Rir decreased with the size of molecule. Therefore the Rir represents a parameter that should be further investigated in order to maximise the performances of concentric type microdialysis probes.
{"title":"Maximising microdialysis sampling by optimising the internal probe geometry","authors":"N. Torto, L. Gorton, E. Mikeladze, E. Csöregi, T. Laurell","doi":"10.1039/A901175G","DOIUrl":"https://doi.org/10.1039/A901175G","url":null,"abstract":"An in-house microdialysis probe equipped with 3 different inner cannulae exhibiting different inner and outer radii was used to sample glucose, maltotriose, maltopentaose and maltoheptaose as model analytes in order to evaluate its performance by means of optimised internal probe geometry. The results were correlated to the inner cannula ratio (Rir), defined as the inner cannula’s inner radius divided by the inner cannula’s outer radius. Extraction fraction (EF) or relative recovery (RR) showed a dependency on Rir for all the investigated analytes at all the perfusion rates. The EF for glucose improved up to 10% for a nominal increase of 0.27 in Rir. The sensitivity of the EF of saccharides to Rir decreased with the size of molecule. Therefore the Rir represents a parameter that should be further investigated in order to maximise the performances of concentric type microdialysis probes.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"8 1","pages":"171-174"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"91428381","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
An enantioselective chemical sensor has been designed and fabricated. The sensor is based on a molecularly imprinted polymer, serving as the recognition element, and a quartz crystal microbalance (QCM), used as the transducer. The polymer, imprinted with the chiral β-blocking drug S-propranolol, was cast as a thin permeable film onto a gold electrode deposited on the quartz crystal vibrator. The mass increase of the polymer due to analyte binding was quantified by piezoelectric microgravimetry with the QCM. The sensor was able to discriminate between the R- and S-propranolol enantiomers in acidified acetonitrile solutions owing to the enantioselectivity of the imprinted sites. Detectability of S-propranolol was 50 µmol dm–3. The general procedure developed here for preparation of the sensor can be adapted for fabrication of a range of different stable analytical sensing devices for numerous analytes by using conventional molecular imprinting protocols.
{"title":"Imprinted polymer-based enantioselective acoustic sensor using a quartz crystal microbalance","authors":"K. Haupt, K. Noworyta, W. Kutner","doi":"10.1039/A907844D","DOIUrl":"https://doi.org/10.1039/A907844D","url":null,"abstract":"An enantioselective chemical sensor has been designed and fabricated. The sensor is based on a molecularly imprinted polymer, serving as the recognition element, and a quartz crystal microbalance (QCM), used as the transducer. The polymer, imprinted with the chiral β-blocking drug S-propranolol, was cast as a thin permeable film onto a gold electrode deposited on the quartz crystal vibrator. The mass increase of the polymer due to analyte binding was quantified by piezoelectric microgravimetry with the QCM. The sensor was able to discriminate between the R- and S-propranolol enantiomers in acidified acetonitrile solutions owing to the enantioselectivity of the imprinted sites. Detectability of S-propranolol was 50 µmol dm–3. The general procedure developed here for preparation of the sensor can be adapted for fabrication of a range of different stable analytical sensing devices for numerous analytes by using conventional molecular imprinting protocols.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"77 1","pages":"391-393"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83356395","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Significantly improved performance in electrothermal atomic absorption spectrometry is possible using an internal standardisation technique. A Perkin-Elmer SIMAA 6000 simultaneous multielement spectrometer was used to study the correlation between two integrated absorbance signals. The behaviour of Pb (analyte) in different urine, blood and placenta samples was compared to that of Bi or Tl used as the internal standards. All samples were spiked with known amounts of Pb and Bi or Tl. A satisfactory signal correlation (r = 0.94) between the integrated absorbances for spikes of the analyte and internal standard was observed with Bi as the internal standard. After signal correction, the relative standard deviation of the integrated absorbance for Pb spikes reduced from 29 to 7% for urine, from 19 to 2% for blood and from 22 to 4% for placenta. The mean difference between Pb concentration found in analysed samples by the method of additions and using an internal standard was 10%.
{"title":"Evaluation of internal standardisation in electrothermal atomic absorption spectrometry","authors":"B. Radziuk, N. Romanova, Y. Thomassen","doi":"10.1039/A809096C","DOIUrl":"https://doi.org/10.1039/A809096C","url":null,"abstract":"Significantly improved performance in electrothermal atomic absorption spectrometry is possible using an internal standardisation technique. A Perkin-Elmer SIMAA 6000 simultaneous multielement spectrometer was used to study the correlation between two integrated absorbance signals. The behaviour of Pb (analyte) in different urine, blood and placenta samples was compared to that of Bi or Tl used as the internal standards. All samples were spiked with known amounts of Pb and Bi or Tl. A satisfactory signal correlation (r = 0.94) between the integrated absorbances for spikes of the analyte and internal standard was observed with Bi as the internal standard. After signal correction, the relative standard deviation of the integrated absorbance for Pb spikes reduced from 29 to 7% for urine, from 19 to 2% for blood and from 22 to 4% for placenta. The mean difference between Pb concentration found in analysed samples by the method of additions and using an internal standard was 10%.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"3 1","pages":"13-16"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"91075992","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
This preliminary study presents the laboratory adaptation of the methylene blue method for the analysis of sulfide in hydrothermal seawater to flow injection analysis (FIA) before its integration on an in situ analyser. The manifold used after optimisation enables us to work on a 0–450 µmol l–1 sulfide range with a detection limit between 0.1 and 0.4 µmol l–1 and a relative standard deviation < 1%. The following steps will be the adaptation of the manifold on the in situ analyser and field tests.
{"title":"Laboratory adaptation of the methylene blue method to flow injection analysis: towards in situ sulfide analysis in hydrothermal seawater","authors":"P. Sarradin, N. Bris, J. Caprais, D. Birot","doi":"10.1039/A809759C","DOIUrl":"https://doi.org/10.1039/A809759C","url":null,"abstract":"This preliminary study presents the laboratory adaptation of the methylene blue method for the analysis of sulfide in hydrothermal seawater to flow injection analysis (FIA) before its integration on an in situ analyser. The manifold used after optimisation enables us to work on a 0–450 µmol l–1 sulfide range with a detection limit between 0.1 and 0.4 µmol l–1 and a relative standard deviation < 1%. The following steps will be the adaptation of the manifold on the in situ analyser and field tests.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"35 1","pages":"157-160"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78546464","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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