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建立了单颗粒-电感耦合等离子体质谱法(SP-ICP-MS)量化与表征海水中银纳米颗粒(AgNPs)的方法。筛选了SP-ICP-MS检测海水中AgNPs时的最优驻留时间,通过探究海水基质对AgNPs检测的影响,确定了海水样品稀释倍数,并利用本方法对大连市近岸海域3个站位表层海水样品中的AgNPs进行测定。结果表明,仪器最优驻留时间为100μs, 150倍稀释海水样品可提高AgNPs浓度的测定准确度。本方法测定海水中AgNPs数量浓度检出限为9.75×103 particles/mL,粒径检出限为12 nm,标称粒径50和100 nm AgNPs的平均加标回收率均大于70%。大连市近岸海域3个站位表层海水样品中均检测出AgNPs,数量浓度最大值为(2.1±0.004)×106 particles/mL,最小值为(1.1±0.01)×105 particles/mL,粒径分布在18~200 nm之间。本方法具有样品制备简单、分析速度快、颗粒物数量浓度检出限低等优点,为近岸海水中AgNPs的监测分析提供了可靠的分析方法。 相似文献
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铂纳米颗粒在汽车行业中被广泛用作汽车尾气催化剂。随着铂纳米颗粒在工业生产中的广泛应用,它在环境中广泛分布并可能从植物累积进入食物链中。因此,建立一种在农产品中的定量分析方法是至关重要的。以酶消解的前处理方法结合单颗粒-电感耦合等离子体质谱法(Single particle ICP-MS,SP-ICP-MS)测定农产品中纳米铂颗粒(PtNPs)粒径分布及颗粒数量浓度。通过优化前处理提取条件,当Macerozyme R-10酶为10 mg、柠檬酸缓冲溶液浓度为5 mmol/L、提取时间36 h时,农产品中PtNPs提取效果较高。PtNPs粒径检出限为20 nm,颗粒浓度检出限为5×105particle/L,铂颗粒浓度回收率在(81±3)%~(91±4)%,加标后平均粒径(41±3)~(47±2) nm,与50 nm PtNPs标准溶液粒径接近。方法操作简单、检出限低、准确度高,适用于农产品中PtNPs定量分析,为客观评价农产品铂纳米毒性效应提供可靠的分析技术。 相似文献
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铂纳米颗粒在汽车行业中被广泛用作汽车尾气催化剂。随着铂纳米颗粒在工业生产中的广泛应用,它在环境中广泛分布并可能从植物累积进入食物链中。因此,建立一种在农产品中的定量分析方法是至关重要的。以酶消解的前处理方法结合单颗粒-电感耦合等离子体质谱法(Single particle ICP-MS,SP-ICP-MS)测定农产品中纳米铂颗粒(PtNPs)粒径分布及颗粒数量浓度。通过优化前处理提取条件,当Macerozyme R-10酶为10 mg、柠檬酸缓冲溶液浓度为5 mmol/L、提取时间36 h时,农产品中PtNPs提取效果较高。PtNPs粒径检出限为20 nm,颗粒浓度检出限为5×105 particle/L,铂颗粒浓度回收率在(81±3)%~(91±4)%,加标后平均粒径(41±3)~(47±2)nm,与50 nm PtNPs标准溶液粒径接近。方法操作简单、检出限低、准确度高,适用于农产品中PtNPs定量分析,为客观评价农产品铂纳米毒性效应提供可靠的分析技术。 相似文献
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建立了单颗粒-电感耦合等离子体质谱法(Single particle ICP-MS,SP-ICP-MS)测定纳米抗菌商品中纳米银颗粒(Silver nanoparticles,AgNPs)粒度分布的方法。首先采用微波消解-ICP-MS法测定了纳米抗菌商品中的总银含量,确定样品稀释倍数。然后在SP-ICP-MS模式下,测定3种AgNPs标准样品(30、50和80nm)的粒径,所得结果与供应商提供的TEM值接近,说明SP-ICP-MS法能够准确表征水溶液中AgNPs的粒径分布,同时采用SP-ICP-MS测定了纳米抗菌商品中纳米银颗粒粒径分布。方法简单快速、灵敏度高,能够为纳米抗菌材料中AgNPs表征提供准确的表征方法。 相似文献
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纳米银的单颗粒-电感耦合等离子质谱法表征及其测定 总被引:1,自引:0,他引:1
建立单颗粒-电感耦合等离子体质谱法( SP-ICP-MS)测定稀溶液中纳米银颗粒粒度分布及纳米银颗粒数量浓度的方法。当停留时间为3 ms时,两个或多个纳米银颗粒同时进入检测器的可能性降至最低。采用5倍标准偏差迭代算法(5σ)区分纳米银颗粒信号和背景信号。采用SP-ICP-MS法测定3种商品级纳米银颗粒(30,50和100 nm)粒度分布和纳米颗粒浓度。结果表明:SP-ICP-MS法测定纳米银颗粒结果与纳米银的TEM值相近,可采用SP-ICP-MS法表征纳米银颗粒。本方法测定稀溶液中纳米银颗粒粒度检出限为25 nm,纳米银颗粒浓度检出限约为8×104个/L。将纳米银颗粒加入到自来水样品中并进行测定,获得相近的纳米银粒度分布及纳米颗粒浓度。本方法简单、快捷、灵敏度高,可为研究水环境中纳米银的风险评估提供可靠分析方法,并为饮用水中纳米银的监测提供分析技术。 相似文献
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毛细管电泳-电感耦合等离子体质谱法测定藻类中6种不同形态的砷化合物 总被引:4,自引:0,他引:4
建立了一种利用毛细管电泳与电感耦合等离子体质谱联用技术(CE-ICP-MS)分析检测6种不同形态砷化合物的方法。详细研究了缓冲溶液的种类、pH值和浓度,分离电压以及进样时间等因素对6种砷化合物的分离度、灵敏度和重现性等的影响。结果表明,在最佳条件下,三价砷(As3+)、一甲基砷(MMA)、二甲基砷(DMA)、五价砷(As5+)、砷胆碱(AsC)和砷甜菜碱(AsB)6种化合物在25 min内得到完全分离。6次平行测定中,6种砷化合物峰面积的相对标准偏差(RSD)为3%~5%,检出限(以As计)(3倍信噪比)为0.08~0.12 μg/L。应用该方法成功地对海带中6种砷化合物进行了分析,回收率为90%~103%。该方法具有耗时短、灵敏度高、样品消耗量少、稳定性好等优点,可用于藻类样品中不同形态砷化合物的分析。 相似文献
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高效液相色谱-电感耦合等离子体质谱联用检测食品中的五种硒形态 总被引:7,自引:0,他引:7
建立了高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)联用检测硒酸盐(SeVI)、亚硒酸盐(SeIV)、硒代蛋氨酸(SeMet)、硒代胱氨酸(SeCys2)和硒代乙硫氨酸(SeEt)的方法。采用Hamilton PRP X-100色谱柱(250 mm×4.6 mm, 5 μm),使用5 mmol/L的柠檬酸溶液(pH 4.5)作为流动相,电感耦合等离子体质谱(ICP-MS)检测,在21 min内可以完全分离5种硒形态。各形态硒的线性相关系数均大于0.9995, SeVI、SeIV、SeMet、SeCys2、SeEt的检出限分别为0.4、0.4、5.6、0.9、1.2 μg/L。探讨了不同提取方法的提取效果,鲜蘑菇和猪肉样品加标回收实验表明,对水溶性良好的无机硒和硒代蛋氨酸而言,采用柠檬酸溶液提取的效果非常好,SeIV和SeVI的回收率均在100%左右,SeMet的回收率为85.0%~95.3%;用蛋白酶水解提取,SeCys2和SeEt的回收率为79.9%~91.5%。该方法可完全满足食品中这5种硒形态的准确定量分析。 相似文献
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电感耦合等离子体质谱技术最新进展 总被引:22,自引:0,他引:22
对1998年以来电感耦合等离子体质谱技术(ICP-MS)的最新进展作一简要回顾。内容包括同位素比值分析、双聚焦扇形磁场高分辨ICP-MS、多接收器磁扇形等离子体质谱仪(MC-ICP-MS)、飞行时间等离子体质谱仪(ICP-TOF-MS)、“冷”等离子体及屏蔽炬技术以及动态碰撞/反应池技术等进展。 相似文献
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《Journal of separation science》2017,40(19):3898-3904
We report a simple and highly sensitive method for the simultaneous detection of trace zinc dimethyldithiocarbamate and zinc ethylenebisdithiocarbamate by capillary electrophoresis with inductively coupled plasma mass spectrometry. Zinc dimethyldithiocarbamate and zinc ethylenebisdithiocarbamate were chelated with trans‐1,2‐diaminocyclohexane‐N,N,N′,N′‐tetraacetic acid to form a macromolecule complex. Then, these two compounds were separated by α‐cyclodextrin‐modified capillary electrophoresis within 12 min at a separation voltage of 15 kV and measured by inductively coupled plasma mass spectrometry. The developed method is sensitive with detection limit of 1.9 and 3.0 ng Zn/mL for zinc dimethyldithiocarbamate and zinc ethylenebisdithiocarbamate, respectively. By means of ultrasound‐assisted extraction methods, zinc dimethyldithiocarbamate and zinc ethylenebisdithiocarbamate spiked into cabbage leaves were successfully extracted and determined with a relative standard deviation (n = 5) ≤ 6% and a recovery of 95–107%. 相似文献
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分别将N-(β氨乙基)-?-氨丙基三甲氧基硅烷(AEAPTMS)、3-巯丙基三甲氧基硅烷(MPTMS)与四乙氧基硅烷(TEOS)水解共聚,制备氨基\巯基键合的硅胶材料。将此材料作为固相萃取(SPE)小柱的填充材料,建立了固相萃取快速分离富集海产品样品中五价砷As(Ⅴ)和三价砷As(Ⅲ)电感耦合等离子体质谱法(ICP-MS)测定海产品中无机砷的方法。研究了固相萃取小柱对无机砷的吸附原理、性能和洗脱条件,在pH3~4范围内固相萃取小柱材料有良好的选择吸附性,利用2%硝酸可将As(Ⅴ)洗脱,利用2%硝酸+0.1mol/L KIO3可将As(Ⅲ)洗脱。实际样品检测的加标回收率在72~103%之间,方法实现了海产品样品中无机砷形态快速、方便、准确的检测。 相似文献
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We have analyzed phosphorus in an enzymatically digested DNA molecule using capillary electrophoresis (CE) hyphenated with inductively coupled plasma mass spectrometry (ICP-MS). The DNA concentration was quantified by the phosphorus value obtained in the CE-ICP-MS analysis. The CE-ICP-MS measurement, for which the interface device AIF-01 equipped three layered nebulizer was adopted, was achieved with limited μL/min nebulizing without loss of sample in the vaporizing chamber. The samples of nucleotides and free phosphate were separated well in the CE-ICP-MS measurement, and the calibration curve (0.1-10μg/mL) of the phosphorus showed a linear (R(2)=0.999) increase in intensity. After digestion of the 100-bp double-strand DNA sample to deoxyribonucleotide-5'-monophosphates (dNMPs) by phosphodiesterase-I, phosphorus was detected by CE-ICP-MS without further purification steps. In this study, we applied two calculation schemes of DNA analysis using a dNMP concentration obtained from CE-ICP-MS. Comparative CE-ICP-MS analysis with DNA digested to dNMPs showed that the assay gave an equal value obtained from the total DNA quantification using fluorescence detection. The detection limits of the DNA sample obtained from these species and phosphorus in nucleotides using CE-ICP-MS were 3.1-26ng/mL. These LOD values were equal to the conventional fluorescence determination of DNA. 相似文献
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Aleksandra Dubiella-Jackowska Żaneta Polkowska Lech Dariusz Piotr Pasławski Wojciech Staszek Jacek Namieśnik 《Central European Journal of Chemistry》2009,7(1):35-41
A solid phase extraction technique for the determination of platinum(IV) at trace levels by inductively coupled plasma mass
spectromA solid phase extraction technique for the determination of platinum(IV) at trace levels by inductively coupled plasma
mass spectrometry (ICP-MS) was developed. The method was based on retention of platinum in a sample on silica gel modified
with aminepropyl groups. The retention of platinum(IV) from the sample solution and the recovery of platinum with 1.0 mol
L−1 thiourea solution were quantitative. The relative standard deviation (RSD) was calculated as 5% (n = 7) at the 10 ng L−1 level. The enrichment factor was found to be (50-fold) for 250 mL of water sample. Under optimum conditions, the method detection
limit (MDL) was found to be 1 ng L−1 for platinum in water matrices. Recoveries of Pt from spike addition to atmospheric water samples were quantitative (80–95%).
The present method was used for the determination of platinum in precipitation, throughfall and runoff water samples.
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Mario Menendez-Miranda Maria T. Fernandez-ArguellesJose M. Costa-Fernandez Jorge Ruiz Encinar Alfredo Sanz-Medel 《Analytica chimica acta》2014
Separation and identification of nanoparticles of different composition, with similar particle diameter, coexisting in heterogeneous suspensions of polymer-coated CdSe/ZnS quantum dots (QDs) have been thoroughly assessed by asymmetric flow field-flow fractionation (AF4) coupled on-line to fluorescence and inductively coupled plasma mass spectrometry (ICPMS) detectors. Chemical characterization of any previously on-line separated nanosized species was achieved by the measurement of the elemental molar ratios of every element involved in the synthesis of the QDs, using inorganic standards and external calibration by flow injection analysis (FIA). Such elemental molar ratios, strongly limited so far to pure single nanoparticles suspensions, have been achieved with adequate accuracy by coupling for the first time an ICP-QQQ instrument to an AF4 system. This hyphenation turned out to be instrumental to assess the chemical composition of the different populations of nanoparticles coexisting in the relatively complex mixtures, due to its capabilities to detect the hardly detectable elements involved in the synthesis. Interestingly such information, complementary to that obtained by fluorescence, was very valuable to detect and identify unexpected nanosized species, present at significant level, produced during QDs synthesis and hardly detectable by standard approaches. 相似文献
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On‐line coupling of LC and ICP‐MS has been used for fractionation and detection of species of Cu, Fe, I, Se and Zn in human serum. It has been shown that anion exchange chromatography provided better separation capability (both intra‐ and inter‐element) than size‐exclusion chromatography. The mobile phases for ion exchange chromatography consisted of Tris–HNO3 buffer and ammonium salt (nitrate, acetate or formate). Formate was found to be the best mobile phase counter ion, enabling good chromatographic separation, and is acceptable for mass spectrometry too. The quantitative evaluation of element concentrations adhering to individual fractions was performed by the peak area normalization method. The repeatability of results ranged from 3 to 15% (depending on the element concentration level) and represented the main part of the result uncertainty. The accuracy of Cu and Zn fraction determinations was confirmed by comparison with the isotope dilution technique. Copyright © 2006 John Wiley & Sons, Ltd. 相似文献