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1.
HPLC-ICP-MS在紫菜中砷形态分析的应用 总被引:27,自引:6,他引:27
通过HPLC-ICP-MS联用技术初步探讨了紫菜中砷的形态;选用了纯水萃取,再用甲醇稀释,用阴离子交换色谱柱经HPLC分离,再用ICP-MS测定,实验发现了2个未知形态色谱峰;该技术将液相色谱的分离技术与ICP-MS高灵敏度的检测方式相结合,具有分离效果好,灵敏度高,耗样量少,速度快,线性范围宽等优点。 相似文献
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毛细管电泳是一种高效、简便的分离方法,已被用于生物、环境及临床等试样的分离及分析[1].检测技术在毛细管电泳中占有重要的地位,目前,在柱紫外可见及荧光检测是两种广为接受的检测方法,但其检测灵敏度仅为10-5~10-6mol/L[2].电感耦合等离子体光谱(ICP-AES/MS)是一种灵敏的元素选择性的分析方法,已被广泛地用于各种试样中元素分析.近年来,该方法作为色谱及毛细管电泳的检测器,被用于元素的形态分析[3].在毛细管电泳(CE)与ICP光谱连用技术中,挑战性的工作是设计一种能把CE与ICP相连的接口.目前已有几种接口… 相似文献
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水中矿物元素的ICP-MS分析 总被引:12,自引:0,他引:12
用ICP-MS对地下水、地表水和饮用水中的矿物元素进行了分析测定,实验证明用ICP-MS可以同时测定地下水,地表水和饮用水中矿物元素;该法灵敏度、精密度和准确度都能满足有关标准的要求,具有多元素同时分析,样品前处理简单,干扰少,测定快速,省事省力等优点。 相似文献
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本文论述了电感耦合高频等离子体(ICP)作为一种新的离子源与成熟的质谱分析技术(MS)相结合的必然性。与ICP发射光谱法和火花源质谱法两者比较,ICP/MS联合技术在超痕量元素分析和同位素测定中显示了某些优越性。以ELAN250型ICP/MS元素分析器为例,介绍了该仪器系统的主要结构和作用及其分析性能。简述了ICP/MS在地质、环保和生物试样分析中的初步应用。 相似文献
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HPLC-ICP-MS或HPLC-FAAS法分离测定硒化合物(英文) 总被引:4,自引:0,他引:4
提出了一种用高效液相色谱(HPLC)分离和用电感偶合等离子体质谱仪(ICP-MS)或火焰原子吸收光谱仪(FAAS)作元素专一检测器在线测定硒的化学形态的方法。在优化的HPLC条件下,用ESAⅢ阴离子色谱柱(250mm×4.6mm),以柠檬酸铵为流动相(5.5mmol/L,pH5.5,流速1.5mL/min),进样量100μL,分离和测定三甲基硒离子、硒代蛋氨酸、亚硒酸和硒酸盐只需8min。HPLC-FAAS在线分析4种硒化合物的检测限为p(Se)=1mg/L。用超声雾化器作ICP-MS的接口,HPLC-ICP-MS在线分析4种硒化合物的检测限分别为P(Se)=0.34μg/L(亚硒酸),0.18μg/L(硒代蛋氨酸),0.08μg/L(三甲基硒离子)和0.07μg/L(硒酸盐)。与气动雾化器接口相比,信号强度增加7至31倍。 相似文献
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综述了水环境中元素形态分析技术研究进展。水环境中元素形态分析技术主要包括电感耦合等离子体质谱法、原子荧光法、气相色谱法、比色法、毛细管电泳法、原子吸收光谱法等技术及其联用技术。电感耦合等离子体质谱与液相色谱联用技术选择性好、分析速度快、分离效果好;原子荧光与液相色谱联用技术灵敏度高、检出限低、操作简单;气相色谱与电感耦合等离子体质谱联用技术可以实现非常低的检测限和良好的回收率。探索新技术的相互融合,提高元素形态分析技术的灵敏度,获得更低的检测下限,降低分析成本,是未来研究的重点。 相似文献
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逆流色谱分离感应耦合等离子质谱在线测量超痕量钚 总被引:3,自引:0,他引:3
将逆流色谱(CCC)与感应耦合等离子质谱(ICP-MS)相联,研究了几种两相体系在CCC中的固定相保留率,从中选择1%TNOA-正庚烷作固定相,通过CCC富集分离钚并去除基体及干扰元素,通过研究在线分离条件及定量方法等,建成了CCC分离ICP—MS在线测量超痕量钚的方法。采用该方法分析得到实际土壤样品中^239Pu的含量与由传统的分离方法给出的结果相吻合。 相似文献
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环境样品中砷、硒形态分析研究进展 总被引:2,自引:0,他引:2
综述了近年来环境样品中砷、硒形态分析的研究进展,主要内容包括样品的前处理技术、分离技术、检测技术。前处理技术主要是用各种提取液采用各种方式提取样品中的砷、硒形态,分离技术主要有高效液相色谱分离、气相色谱分离、毛细管电泳分离等,检测技术主要有原子吸收光谱法、原子发射光谱法、原子荧光光谱法、电感耦合等离子体质谱法等。最后对其研究前景进行了展望。 相似文献
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《Spectrochimica Acta Part B: Atomic Spectroscopy》2001,56(3):233-260
Applications of solid phase microextraction (SPME) for trace element speciation are reviewed. Because of the relative novelty of the technique in the inorganic analytical field, the first part of this review provides a short overview of the principles of SPME operation; the second part describes typical SPME applications to elemental speciation. Volatile organometallic compounds can be collected by SPME from the sample headspace or liquid phase, directly or after derivatization. The usual separation method for the collected volatile species is gas chromatography. Non-volatile analyte species can be collected from the sample liquid phase and separated by liquid chromatography or capillary electrophoresis. Currently, most SPME applications in the inorganic field comprise analyte ethylation and headspace extraction followed by gas chromatographic separation of tin, lead and mercury species. The use of SPME for the study of equilibria in complex systems is also discussed and future roles of solid phase microextraction in the inorganic analytical field are raised. 相似文献
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高效液相色谱及其联用技术在汞形态分析中的应用 总被引:14,自引:0,他引:14
本文对近二十年来高效液相色谱及其联用技术在汞的形态分析中的应用进行了综述,着重讨论了样品的前处理方法,高效液相色谱用于汞化合物的形态分离以及检测器的选择。 相似文献
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Summary Gradient reversed-phase liquid chromatography was examined with a view to using it as a separation technique for the speciation of vanadyl and nickel porphyrins in oil extracts. Poor separations were obtained when precipitation of the sample constituents occurred in the starting mobile phase. The reasons for the precipitation phenomena were found to be highly complex. Mixed crystal formation, slow dissolution kinetics and saturation may influence the elution behaviour of species present in the oil extracts. When precipitation was avoided the separation of the vanadyl porphyrins was significantly improved. Thus far, no satisfactory separations have been obtained for the nickel porphyrinic species.Although the occurrence of precipitation of the extracts hinders the distinct speciation of metalloporphyrins with reversed phase chromatography, the precipitation/dissolution phenomena showed some interesting features as a clean-up step for diluted crude oil samples and oil fractions. 相似文献
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It is known that while many elements are considered essential to human health, many others can be toxic. However, because the intake, accumulation, transport, storage and interaction of these different metals and metalloids in nature is strongly influenced by their specific elemental form, complete characterization of the element is essential when assessing its benefits and/or risk. Consequently, interest has grown rapidly in determining oxidation state, chemical ligand association, and complex forms of a many different elements. Elemental speciation, or the analyses that lead to determining the distribution of an element’s particular chemical species in a sample, typically involves the coupling of a separation technique and an element specific detector. A large number of methods have been developed which utilize a multitude of different separation mechanisms and detection instruments. Yet, because of its versatility, robustness, sensitivity and multi-elemental capabilities, the coupling of liquid chromatography to inductively coupled plasma mass spectrometry (LC–ICP–MS) has become one of the most popular techniques for elemental speciation studies. This review focuses on the basic principles of LC–ICP–MS, its historical development and the many ways in which this technique can be applied. Different liquid chromatography separations are discussed as well as the factors that must be considered when coupling each to ICP–MS. Recent applications of LC–ICP–MS to the speciation of environmental, biological and clinical samples are also presented. 相似文献
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Joanna Szpunar-obiska Claudia Witte Ryszard obinski Freddy C. Adams 《Fresenius' Journal of Analytical Chemistry》1995,351(4-5):351-377
A comprehensive review of the state-of-the-art of the separation of various organically-bound metals and metalloids for speciation analysis is presented. Recent developments in chromatographic (gas, liquid and supercritical fluid), electrophoretic (free-flow and gel) and fractionation techniques are discussed, followed by a survey of pertinent applications to speciation analysis for organometals and metalloids. The required sample characteristics for a given separation technique are specified and appropriate derivatization procedures are characterized. Methods applicable to the speciation of organic species of a particular element in various matrices are critically evaluated.List of abbreviations APS
ammonium pentanesulfonate
- CCC
counter current chromatography
- CZE
capillary zone electrophoresis
- DBT
dibutyltin
- DCyT
dicyclohexyltin
- DDTC
diethyldithicarbamate
- DEAE
diethylaminoethyl gel (anion exchanger)
- DEL
diethyllead
- DET
diethyltin
- DMA
dimethylarsinic acid
- DMGe
dimethylgermanium
- DMHg
dimethylmercury
- DML
dimethyllead
- DMSb
dimethylstibinic acid
- DMT
dimethyltin
- DPhT
diphenyltin
- DPrT
dipropyltin
- EDTA
ethylenediaminetetraacetate
- FFF
field flow fractionation
- GC
gas chromatography
- HEPES
4-(2-hydroxyethyl)-1-piperazine-ethanesulfonic acid
- HPLC
high performance liquid chromatography
- ICP
inductively coupled plasma
- IEC
ion exchange chromatography
- IIC
ion interaction chromatography
- LC
liquid chromatography
- MBT
monobutyltin
- MCyT
monocyclohexyltin
- MEA
monoethylarsinic acid
- MEHg
monoethylmercury
- MEL
monoethyllead
- MET
monoethyltin
- MIP
microwave induced plasma
- MMA
monomethylarsonic acid
- MMGe
monomethylgermanium
- MMHg
monomethylmercury
- MML
monomethyllead
- MMSb
monomethylstibonic acid
- MMT
monomethyltin
- MPhHg
monophenylmercury
- MPhT
monophenyltin
- MPrT
monopropyltin
- MS
mass spectrometry
- NAA
neutron activation analysis
- NaBS
sodium 1-butanesulfonate
- NaDS
sodium dodecylsulfonate
- NaPS
sodium pentanesulfonate
- PAGE
polyacrylamide gel electrophoresis
- PAR
4-(2-pyridylazo)resorcinol
- PIXE
proton induced X-ray emission
- QF
quartz furnace
- RPC
reversed phase partition chromatography
- SDS
sodium dodecyl sulfate
- SEC
size exclusion chromatography
- SFC
supercritical fluid chromatography
- TBAP
tetrabutylammonium phosphate
- TAL
tetraalkyllead
- TBT
tributyltin
- TCyT
tricyclohexyltin
- TeEL
tetraethyllead
- TEL
triethyllead
- TeML
tetramethyllead
- TET
triethyltin
- TGME
thioglycolic methyl ester
- THF
tetrahydrofuran
- TMA
trimethylarsinic acid
- TMAH
tetramethylammonium hydroxide
- TMGe
trimethylgermanium
- TML
trimethyllead
- TMT
trimethyltin
- TPhT
triphenyltin
- TPrT
tripropyltin
- Tris
tris(hydroxymethyl)aminomethane 相似文献
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Sarah Fitzpatrick Les Ebdon Michael E. Foulkes 《International journal of environmental analytical chemistry》2013,93(11-12):835-841
A method is presented for arsenic speciation analysis of an oyster sample using ion chromatography coupled with an inductively coupled plasma mass spectrometry (ICP-MS) instrument. A strong anion exchange resin was employed with a step gradient elution of 0.1 mM/0.1 M K 2 SO 4 at pH 10.2. Arsenobetaine and dimethylarsinic acid were determined following extraction based on trypsin enzymolysis with 95-100% extraction efficiency. Limits of detection in the range 0.1-0.3 mg kg m 1 of arsenic were obtained for organic arsenic species. No inorganic arsenic was detected. Validation was performed using TORT-2 as a certified reference material. Although high performance liquid chromatography (HPLC) coupled to ICP-MS is an effective method for speciation analysis it is not always necessary to obtain such a detailed picture. A simple liquid chromatographic separation technique based upon mini-column technology is presented. It was developed to obtain a fast, efficient and reliable separation of inorganic from organic, i.e. assumed toxic from non-toxic, arsenic and selenium species suitable for use as an initial screening method for environmental analysis. Two types of strong anion exchange resin were tested. Excellent separation was obtained for both min-column resins and analysis times were within 7 min. Limits of detection obtained for inorganic arsenic, organic arsenic, selenomethionine, Se IV and Se VI were 1.6, 1.8, 66, 32 and 22 µg kg m 1 , respectively. 相似文献
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HPLC-ICP-MS在食品中硒和砷形态分析及其生物有效性研究中的应用 总被引:6,自引:0,他引:6
食品中含有与人体健康密切相关的多种微量元素,微量元素的毒性和生物有效性取决于它们的化学形态。食品中的微量元素形态分析及其生物有效性研究对食品安全控制与营养评价具有至关重要的意义。本文扼要介绍了高效液相色谱与电感耦合等离子质谱(HPLC-ICP-MS)联用情况,该技术以不同的色谱分离柱完成各种分析物的分离,具有高灵敏度、高选择性、线性范围宽、检测限低、多元素同时检测等特点,在微量元素形态分析中占有重要的地位。综述了HPLC-ICP-MS在食品微量元素形态分析及其生物有效性研究中的应用,重点介绍了富硒酵母、蒜类植物、富硒营养保健品等食品中硒形态和海产品、农产品等食品中砷形态的研究,以及其它多种微量元素的形态分析和这些微量元素在生物体内的代谢。 相似文献
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An analytical procedure for selenium speciation of analysis of selenourea (SeU), selenoethionine (SeE), selenomethionine (SeM), Se(VI), Se(IV), dimethylselenide (dMeSe) and dimethyldiselenide (dMedSe) was developed, based on two complementary liquid chromatography (LC) techniques coupled with inductively coupled plasma-mass spectrometry (ICP-MS). Specifically, strong anion exchange (SAX) chromatography coupled with ICP-MS was used for the separation and quantification of all the earlier mentioned Se compounds, except for the two methyl selenides, which could be separated and determined by reversed phase chromatography coupled with ICP-MS. This procedure was applied to a soil sample from the warm springs area of Thermopyles (Greece). For leaching the Se species from the soil sample, four extraction methods, using water at ambient temperature, hot water, methanol and 0.5 M HCl, were tested for their efficiency of extracting the different Se species. The speciation results obtained by the LC-ICP-MS methods were compared with those obtained by voltammetric techniques. The determination of total selenium in the sample was achieved by graphite furnace atomic absorption spectrometry, as well as by ICP-atomic emission spectrometry, after suitable digestion of the sediment sample. 相似文献