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Determination of nicotine in tobacco by molecularly imprinted solid phase extraction with differential pulsed elution 分子印迹固相萃取-差分脉冲洗脱法测定烟草中的尼古丁
Analytical Communications Pub Date : 1999-01-01 DOI: 10.1039/A902509J
W. Mullett, E. Lai, B. Sellergren
{"title":"Determination of nicotine in tobacco by molecularly imprinted solid phase extraction with differential pulsed elution","authors":"W. Mullett, E. Lai, B. Sellergren","doi":"10.1039/A902509J","DOIUrl":"https://doi.org/10.1039/A902509J","url":null,"abstract":"A molecularly imprinted solid phase extraction-differential pulsed elution (MISPE-DPE) method has been developed for the determination of nicotine in tobacco. Nicotine and a trace alkaloid myosmine were able to bind to the molecularly imprinted polymer (MIP) packed in a micro-column when acetonitrile was used as the mobile phase. However, over 95% of the bound myosmine could be desorbed and washed away by a 20 µl pulse of methanol, compared to only 43% of the bound nicotine. The remaining quantity of bound nicotine was desorbed by a 20 µl pulse of 1% trifluoroacetic acid in water, for direct UV detection at 254 nm. This MISPE-DPE method provided inherent selectivity for nicotine that allowed both a shorter analysis time (3 min) and a lower analysis cost than liquid chromatographic methods. A detection limit of 1.8 µg ml–1 and a linear dynamic range up to 1000 µg ml–1 were obtained. Preconcentration of 845 µl of a 10 ng ml–1 nicotine standard solution produced a detectable peak signal. These analytical figures of merit are superior to those reported previously for several nicotine–MIP-based methods.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"105 1","pages":"217-220"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80620423","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}
引用次数: 70
An acrylamide-based molecularly imprinted polymer for the efficient recognition of optical amino acid hydantoins 一种基于丙烯酰胺的分子印迹聚合物,用于光学氨基酸醛酸的高效识别
Analytical Communications Pub Date : 1999-01-01 DOI: 10.1039/A902025J
Jie Zhou, Xiwen He, Yijun Li
{"title":"An acrylamide-based molecularly imprinted polymer for the efficient recognition of optical amino acid hydantoins","authors":"Jie Zhou, Xiwen He, Yijun Li","doi":"10.1039/A902025J","DOIUrl":"https://doi.org/10.1039/A902025J","url":null,"abstract":"Using acrylamide as a hydrogen bonding functional monomer and (5R)-5-benzylhydantoin as a template, a molecularly imprinted polymer was prepared in a polar solvent, which exhibited good enantiomeric recognition properties. The binding selectivity of the polymer was evaluated by batch methods. Scatchard analyses showed that two classes of binding sites were produced in the imprinted polymer and their dissociation constants were estimated to be (4.6 ± 0.8) × 10–5 and (1.3 ± 0.2) × 10–4 mol L–1, respectively. This was in agreement with the prediction of the binding characteristics of the polymer by a spectrophotometric method. Study of the effect of water on the separation factor of the polymer further proved that the hydrogen bonding interactions played an important role in the recognition of acrylamide-based molecularly imprinted polymers.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"23 1","pages":"243-246"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"73357786","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}
引用次数: 14
Direct measurement of atmospheric formaldehyde using gas chromatography-pulsed discharge ionisation detection 气相色谱-脉冲放电电离检测法直接测定大气中甲醛
Analytical Communications Pub Date : 1999-01-01 DOI: 10.1039/A809762C
M. Hunter, K. Bartle, P. Seakins, A. Lewis
{"title":"Direct measurement of atmospheric formaldehyde using gas chromatography-pulsed discharge ionisation detection","authors":"M. Hunter, K. Bartle, P. Seakins, A. Lewis","doi":"10.1039/A809762C","DOIUrl":"https://doi.org/10.1039/A809762C","url":null,"abstract":"A gas chromatographic system has been developed for the direct analysis of atmospheric formaldehyde and other oxygenated hydrocarbons. This method utilises the trapping of analytes in a loop cooled with liquid nitrogen, separation by gas chromatography and then subsequent detection using a pulsed discharge helium ionisation detector (pdHID). The detection limit of this instrument is estimated to be 32 parts per trillion by volume (pptv) for 0.2 l of gas sampled at a flow rate of 30 ml min–1 (S/N at 4:1). A number of other compounds have been monitored simultaneously using this method, including higher molecular weight aldehydes and acetone. Continuous measurement of formaldehyde can be performed with a time resolution of 15 min, with longer analysis times required for inclusion of other species. Calibrations were performed using a permeation tube instrument for both formaldehyde and acetone. A linear response has been observed for formaldehyde sample volumes of 60–200 ml of a 272 ppbv sample (20–68 ng). For acetone a linear response was observed from 175–360 ml of a 30 ppbv standard (12–26 ng). A flame ionisation detector (FID) was also utilised during system development to confirm separation of formaldehyde from atmospheric hydrocarbons.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"94 1","pages":"101-104"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86743579","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}
引用次数: 33
The estimation of lanthanum by air-acetylene atomic absorption spectrophotometry using an indirect procedure 空气-乙炔原子吸收分光光度法间接测定镧
Analytical Communications Pub Date : 1999-01-01 DOI: 10.1039/A900331B
S. J. Wilson, P. Marquis
{"title":"The estimation of lanthanum by air-acetylene atomic absorption spectrophotometry using an indirect procedure","authors":"S. J. Wilson, P. Marquis","doi":"10.1039/A900331B","DOIUrl":"https://doi.org/10.1039/A900331B","url":null,"abstract":"A method for measuring the release of lanthanum from some ceramic dental materials was required using air–acetylene atomic absorption spectrophotometry (AA-AAS), and an analytical procedure was devised based on the release of calcium in the presence of phosphate by lanthanum addition. The extent of phosphate interference in the determination of calcium by AA-AAS was assessed, and it was shown that the absorbance of a 10 ppm Ca standard was reduced by 45% in the presence of 20 ppm or more of phosphate (as PO4). Analysis of standards containing 10 ppm Ca, 20 ppm PO4, and lanthanum added at concentrations up to 100 ppm showed rapid increase of calcium absorbances from 10 to 40 ppm La, after which absorbance increased slowly to a constant value at 90 ppm La. This corresponded to the value of a 10 ppm Ca standard solution containing no phosphate. Closer examination of solutions containing 10–40 ppm La revealed a quantitative relationship between lanthanum levels and calcium absorbances which deviated slightly from Beer’s law. Consequent analysis of solutions containing various amounts of lanthanum in the presence of 10 ppm Ca and 20 ppm PO4 followed by repeated analysis of standards demonstrated good precision and reproducibility. The relative standard deviation for repeated standard analyses was 4.2%, and the detection limit was 0.6 ppm La representing an increase of sensitivity of approximately 100 times over lanthanum determinations using nitrous oxide–acetylene techniques. The method indicates that similar procedures may be used to estimate elements which exercise similar release effects.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"163 1","pages":"31-33"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78068773","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}
引用次数: 2
Depth profiling of a Co-implanted silicon wafer by total-reflection X-ray fluorescence analysis after repeated oxidation and HF-etching 重复氧化和hf刻蚀后共植入硅片的全反射x射线荧光分析
Analytical Communications Pub Date : 1999-01-01 DOI: 10.1039/A809804B
R. Klockenkämper, A. Bohlen
{"title":"Depth profiling of a Co-implanted silicon wafer by total-reflection X-ray fluorescence analysis after repeated oxidation and HF-etching","authors":"R. Klockenkämper, A. Bohlen","doi":"10.1039/A809804B","DOIUrl":"https://doi.org/10.1039/A809804B","url":null,"abstract":"A new method of depth profiling has been developed and applied to a Co-implanted Si-wafer. A square section of only some cm2 was chosen, a thin near-surface sublayer oxidized by an oxygen plasma and the oxidized sublayer precisely etched by a solution of hydrofluoric acid. The mass of Si within the sublayer was determined via differential weighing of the wafer piece and the mass of Co determined by TXRF (total reflection X-ray fluorescence) of the loaded acidic solution. These steps were repeated time and again in order to record a total depth profile showing the relative concentration of Co dependent on the depth within the wafer. The integration of this profile gave a total dose of 1.13 × 1017 ions cm–2 with high accuracy. The depth resolution of the new method might be in the order of a few nm, the detection limit about 0.01% or 5 × 1018 atoms cm–3 of Co.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"178 1","pages":"27-29"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80012153","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}
引用次数: 13
At-line coupling of surface-enhanced resonance Raman spectroscopy and reversed-phase ion-pair chromatography 表面增强共振拉曼光谱与反相离子对色谱的联机耦合
Analytical Communications Pub Date : 1999-01-01 DOI: 10.1039/A903254A
R. M. Seifar, R. J. Dijkstra, U. Brinkman, C. Gooijer
{"title":"At-line coupling of surface-enhanced resonance Raman spectroscopy and reversed-phase ion-pair chromatography","authors":"R. M. Seifar, R. J. Dijkstra, U. Brinkman, C. Gooijer","doi":"10.1039/A903254A","DOIUrl":"https://doi.org/10.1039/A903254A","url":null,"abstract":"At-line coupling of surface-enhanced resonance Raman spectroscopy (SERRS) and reversed-phase ion-pair chromatography with an excitation wavelength of 514.5 nm was applied for the isocratic separation and identification of four representative basic dyes (basic fuchsin, nile blue, crystal violet and ethyl violet). The effluent from a chromatographic column was deposited on a thin layer chromatography (TLC) plate by means of a spray-jet interface and analysed by Raman spectroscopy. The presence of non-volatile ion-pair reagents (1-heptanesulfonic acid sodium salt, sodium perchlorate) did not interfere with the deposition process and also not with the SERRS experiments. In fact higher SERRS intensities were observed in the presence of the ion-pair reagents. Reliable spectra could be recorded down to 90 pg of dyes deposited on the TLC plate.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"89 1","pages":"273-276"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80386732","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}
引用次数: 14
An approach to the identification of selenium species in yeast extracts using pneumatically-assisted electrospray tandem mass spectrometry 利用气动辅助电喷雾串联质谱法鉴定酵母提取物中硒的种类
Analytical Communications Pub Date : 1999-01-01 DOI: 10.1039/A900319C
C. Casiot, V. Vacchina, H. Chassaigne, J. Szpunar, M. Potin-Gautier, R. Łobiński
{"title":"An approach to the identification of selenium species in yeast extracts using pneumatically-assisted electrospray tandem mass spectrometry","authors":"C. Casiot, V. Vacchina, H. Chassaigne, J. Szpunar, M. Potin-Gautier, R. Łobiński","doi":"10.1039/A900319C","DOIUrl":"https://doi.org/10.1039/A900319C","url":null,"abstract":"An approach to the identification of unknown signals in selenium speciation analysis of yeast by reversed-phase chromatography with ICP-MS detection is described. The analytical strategy was based on: (i), heart-cutting of a Se-containing fraction in the reversed-phase chromatographic eluate followed by its lyophilization; (ii), pneumatically-assisted electrospray (ESI) MS and ESI tandem MS of the lyophilizate; and (iii) confirmation of the fragmentation pattern obtained using the sulfur analogue of the seleno compound that was expected to have been identified. The approach developed allowed the identification of Se–adenosylhomocysteine as the major selenium species in an extract of a selenized yeast sample.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"78 1","pages":"77-80"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84060520","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}
引用次数: 100
Determination of the palladium content in a solid plastic material by electrothermal vaporization ICP-mass spectrometry (ETV-ICPMS) 电热汽化icp -质谱法测定固体塑料中钯的含量
Analytical Communications Pub Date : 1999-01-01 DOI: 10.1039/A809318K
F. Vanhaecke, Marieke Verstraete, L. Moens, R. Dams
{"title":"Determination of the palladium content in a solid plastic material by electrothermal vaporization ICP-mass spectrometry (ETV-ICPMS)","authors":"F. Vanhaecke, Marieke Verstraete, L. Moens, R. Dams","doi":"10.1039/A809318K","DOIUrl":"https://doi.org/10.1039/A809318K","url":null,"abstract":"Electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICPMS) was used for the determination of the Pd content in a solid aliphatic polyketone. The presence of Pd in this material has to be attributed to the use of a Pd-containing homogeneous catalyst for its production. By application of a multi-step heating programme, the organic matrix could be selectively and completely removed prior to the vaporization of the analyte element. The accuracy attainable when using (i) external calibration and (ii) single standard addition using an aqueous standard solution was evaluated by comparison of the results obtained with a reference value obtained by means of neutron activation analysis (NAA). On the basis of its similar furnace behaviour, Ir was shown to be perfectly suited to be used as an internal standard. Also the argon dimer signal (Ar2+) shows some potential to be used as an internal standard. When using Ir or Ar2+ as an internal standard and single standard addition for calibration, the ETV-ICPMS result (∼5 µg g–1) agreed within 10% with the NAA result on each occasion (deviation between average ETV-ICPMS result and reference value ∼2%). The absolute limit of detection (3s-criterion) was observed to be ∼1 pg, corresponding to a relative value of ∼1 ng g–1, taking 1 mg as a typical sample mass. However, when using Ir as an internal standard, it was established that the detection limit deteriorated to ∼20 pg, due to the presence of a measurable amount of Pd in the Ir standard solution.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"39 1","pages":"89-92"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84294838","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}
引用次数: 17
Influence of functional and cross-linking monomers and the amount of template on the performance of molecularly imprinted polymers in binding assays 功能单体和交联单体及模板量对结合试验中分子印迹聚合物性能的影响
Analytical Communications Pub Date : 1999-01-01 DOI: 10.1039/A901339C
E. Yilmaz, K. Mosbach, K. Haupt
{"title":"Influence of functional and cross-linking monomers and the amount of template on the performance of molecularly imprinted polymers in binding assays","authors":"E. Yilmaz, K. Mosbach, K. Haupt","doi":"10.1039/A901339C","DOIUrl":"https://doi.org/10.1039/A901339C","url":null,"abstract":"","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"60 1","pages":"167-170"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84638272","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}
引用次数: 153
A new sandwich-type assay of estrogen using piezoelectric biosensor immobilized with estrogen response element 用雌激素反应元件固定压电生物传感器的新型三明治式雌激素检测方法
Analytical Communications Pub Date : 1999-01-01 DOI: 10.1039/A902872B
Mo Zhihong, Long Xiaohui, F. Weiling
{"title":"A new sandwich-type assay of estrogen using piezoelectric biosensor immobilized with estrogen response element","authors":"Mo Zhihong, Long Xiaohui, F. Weiling","doi":"10.1039/A902872B","DOIUrl":"https://doi.org/10.1039/A902872B","url":null,"abstract":"A new methodology, sandwich-type monitoring assay system using an estrogen response element (ERE)-immobilized piezoelectric biosensor in combination with flow injection technique, has been developed for analysis of estrogen (E). The principle of the assay is that the estrogen receptor (ER) captures estrogen and then the complex is bound with ERE immobilized on the sensor. It was confirmed that initial binding of the ERE with ER is significantly accelerated by the formation of an E–ER complex. This kinetic difference was monitored by real-time measurement of the resonance frequency of the ERE piezoelectric biosensor and applied to detect 17β-estradiol. The calibration graph was linear in the range 10–100 nmol l–1 with a detection limit of 7.8 nmol l–1, an RSD of 5.9% for 50 nmol l–1 (6 replicates), and one run time of 4 min. Gradient flow injection on-line connection to an array of ERE piezoelectric biosensors is in progress for the simultaneous determination of endogenous and synthetic estrogens in drinking water and urine. In comparison with present chromatographic methods coupled with MS, the proposed technique is simple, flexible and cheap and has great potential in applications such as field and on-site monitoring and screen testing of endocrine disruptors.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"2 1","pages":"281-283"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84101921","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}
引用次数: 39
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