ICP-MS对茶叶中6种重金属定量分析方法的研究

采用湿法和微波消解在不同条件下对茶叶进行前处理,对不同方法消除茶叶中有机碳的效果进行了研究,并通过对GBW10016茶叶标准物质中Cr、Ni、Cu、Zn、Cd和Pb等重金属分析结果的验证,建立了茶叶基体中6种重金属定量适宜的前处理方法和电感耦合等离子体质谱定量测定方法。同时对市场上几种绿茶、乌龙茶和花茶中重金属的污染状况进行了评估,为健康安全饮茶提供有益参考。     

超级微波ICP-MS法测定食用猪油中5种微量元素

建立了超级微波ICP-MS(电感耦合等离子体质谱)法测定食用猪油中5种微量元素。使用超级微波对食用猪油消化前处理,直接定容,采用ICP-MS法进行分析。结果表明:在0~20μg/L浓度范围内,5种元素标准曲线的线性关系良好,相关系数在0.9998~1.0000之间,检出限在0.003~0.017μg/L,加标回收率在98.3%~109.2%,RSD在2.62%~5.26%之间。相比于传统微波,该方法耗时短,效率高,可以满足日常大量样品分析。     

ICP—MS总量法测定原煤中45种元素

Determinationof45ElementsofRawCoalbyMicrowaveAcidDigestionICP－MS1微波消解样品1．1微波消解的优点微波消解技术是近年来国际上出现的一种新的样品处理技术，其消解方式可分为常压微波消解和高压微波消解。由于原煤样品十分难溶，采用高压消解，具有以下优点：（1）由于封闭容器的压力、酸的沸点升高，使封闭消解达到高温、高压，样品分解完全，大大缩短了消解所需时间；门）封闭容器消解时几乎没有蒸气损失，消除了易挥发成分损失的可能性；（3）封闭消解样品只需少量酸，不需要继续加入酸以保持体积，所以避免样品被沾污，同时…     

湿法消化ICP-MS法与微波消解ICP-MS法测定圆白菜标准物质中铅、镉、砷的比较

建立了电感耦合等离子体质谱法（ICP-MS）测定圆白菜标准物质中铅、镉、砷含量的分析方法。采用湿法消化和微波消解两种前处理方法,消解样品后对其进行了ICP-MS分析,在线内标溶液校正仪器的信号漂移,通过比较两种前处理方法对元素铅、镉、砷的测定结果分析显示,两种前处理方式测定值均在参考值范围内,无显著性差异,且相对标准偏差在0.41%～4.0%之间,测定结果准确可靠。湿法消化和微波消解两种前处理方式均可做为ICP-MS的前处理方法。     

快速测定稀土铝合金中稀土总量的新方法

介绍了一种采用二溴-氯偶氮氯磷（DBC-CPA）分光光度法快速测量稀土铝合金中稀土总量的新方法。     

高纯金属铕及其氧化物中14个稀土杂质的ICP-MS测定

本文针对单同位素元素铥与氧化铕基体的氧化物离子的质量数重叠,在ICP-MS谱法中无法测定的问题,研究了P_(507)萃淋树脂小型柱分离。在试验选择的分离条件下,分离周期(进样-淋洗-洗脱-再生)为2.5h。结合直接测定大部分稀土杂质,最终建立了高纯铕中14个稀土杂质元素的ICP-MS分析方法。方法测定下限(ΣRE)<5μg/g,加标回收率在92～111％范围内,RSD％<10％。方法灵敏、快速、简便,满足4～5N高纯金属铕及其氧化物产品分析的要求。     

微波消解ICP-MS法测定某肺癌高发区居民饮食中28种元素

采用真空冷冻干燥和硝酸 过氧化氢体系微波消解处理饮食样品,ICP-MS法测定样品中28种元素的含量。在优化仪器工作参数后,以铑(Rh)和铼(Re)双内标对基体影响和信号漂移进行校正,并采用4种国家标准物质验证该方法的准确度和精密度。结果表明,28种元素检出限为0.01~0.40 μg/L,加标回收率为82%~114%,国家标准物质测定值与标准值或参考值一致,精密度(RSD)为0.4%~16.9%。用该方法测定60份肺癌高发区居民饮食样品中28种元素含量,结果可为研究微量元素与肺癌的关系和指导合理膳食提供参考。     

钢铁及合金中稀土总量快速测定方法研究

本文建立钢铁及其合金中稀土总量快速测定方法。试样用硫酸和硝酸的混合酸溶解,用草酸做掩蔽剂,偶氮氯膦mA与稀土生成蓝色络合物,于分光光度计波长670nm处测量其吸光度。样品的加标回收率为96.0%~101.8%,相对标准偏差(RSD)为3.0%。方法操作简便、快速、准确。     

国产微波消解仪ICP/MS法测定大米中重金属元素

采用快速高效的微波消解前处理方法,结合电感耦合等离子体质谱对大米标准物质中砷、铅、镉、硒、铝等元素进行测定,结果表明,选用HNO3∶H2O2=6∶1的酸配比消解效果最好,所得各元素均在质控范围内,回收率均在90%~101%之间,RSD(n=6)均在2.4%~6.1%之间。高通量的微波前处理结合电感耦合等离子体质谱的方法,具有处理量大,操作快速简便等优点,能够满足大米等食品样品的日常监测需求。     

ICP-MS法检测带鱼中汞、砷、钒、锑、钡重金属污染物残留

目的:实验建立了全自动微波消解法消解带鱼样品,电感耦合等离子体质谱(ICP-MS)法定量检测的分析方法。方法:带鱼样品粉碎后,精密称取0.35g,置消解罐中,加浓硝酸和双氧水,按程序消解,消解完毕后,消解液定容至25mL,上ICP-MS仪,在线内标法定量检测。结果:在浓度范围0.01～10.0μg/L范围内,汞、砷、钒、锑、钡线性关系良好;汞、砷、钒、锑、钡检出限分别为0.018、0.032、0.034、0.045和0.027μg/kg;平均加标回收率在83.9%～104.2%;方法重复性良好。结论方法前处理简单、快速、检测准确,适用于带鱼等水产品中汞、砷、钒、锑、钡等重金属的检测。     

国产电感耦合等离子体质谱仪测定地球化学样品中稀土和铀钍元素的含量

用国产电感耦合等离子体质谱仪（IC P -M S ）建立了测量地球化学样品中稀土和铀钍元素含量（L a、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu、U、Th）的方法。样品在高温密闭环境下用氢氟酸-硝酸-高氯酸三酸混合消解。溶液通过在线三通进入雾化器,选择元素Re作为内标测量样品中各元素的含量,选择质谱干扰较少的元素谱线进行测量。采用多点标准获得的标准曲线的线性相关系数大于0.999,通过测量空白溶液得出大部分元素的仪器的检出限在0.001～0.01ng · mL -1左右。实验测量得到仪器的氧化物产率为2.8％,双电荷产率为2.1％,短期稳定性（20min）优于3％,长期稳定性（2h）优于5％。实验测试了多种国家标准物质,测量值与参考值吻合。     

The application of inductively coupled plasma mass spectrometry in clinical pharmacological oncology research

Metal-based anticancer agents are frequently used in the treatment of a wide variety of cancer types. The monitoring of these anticancer agents in biological samples is important to understand their pharmacokinetics, pharmacodynamics, and metabolism. In addition, determination of metals originating from anticancer agents is relevant to assess occupational exposure of health care personnel working with these drugs. The high sensitivity of inductively coupled plasma mass spectrometry (ICP-MS) has resulted in an increased popularity of this technique for the analysis of metal-based anticancer drugs. In addition to the quantitative analysis of the metal of interest in a sample, ICP-MS can be used as an ultrasensitive metal selective detector in combination with speciation techniques such as liquid chromatography. In the current review we provide a systematic survey of publications describing the analysis of platinum- and ruthenium-containing anticancer agents using ICP-MS, focused on the determination of total metal concentrations and on the speciation of metal compounds in biological fluids, DNA- and protein-adducts, and environmental samples. We conclude that ICP-MS is a powerful tool for the quantitative analysis of metal-based anticancer agents from multiple sample sources.     

In vivo monitoring of the transfer kinetics of trace elements in animal brains with hyphenated inductively coupled plasma mass spectrometry techniques

The roles of metal ions to sustain normal function and to cause dysfunction of neurological systems have been confirmed by various studies. However, because of the lack of adequate analytical method to monitor the transfer kinetics of metal ions in the brain of a living animal, research on the physiopathological roles of metal ions in the CNS remains in its early stages and more analytical efforts are still needed. To explicitly model the possible links between metal ions and physiopathological alterations, it is essential to develop in vivo monitoring techniques that can bridge the gap between metalloneurochemistry and neurophysiopathology. Although inductively coupled plasma mass spectrometry (ICP‐MS) is a very powerful technique for multiple trace element analyses, when dealing with chemically complex microdialysis samples, the detection capability is largely limited by instrumental sensitivity, selectivity, and contamination that arise from the experimental procedure. As a result, in recent years several high efficient and clean on‐line sample pretreatment systems have been developed and combined with microdialysis and ICP‐MS for the continuous and in vivo determination of the concentration‐time profiles of metal ions in the extracellular space of rat brain. This article reviews the research relevant to the development of analytical techniques for the in vivo determination of dynamic variation in the concentration levels of metal ions in a living animal. © 2009 Wiley Periodicals, Inc. Mass Spec Rev 29:392‐424, 2010     

微波消解电感耦合等离子体质谱测定糖果中钛含量

建立了电感耦合等离子质谱（ICP-MS）测定糖果中钛含量的方法,从而推断出食品生产中添加二氧化钛量及食品中的钛残留量是否超标。结果表明,该方法在1．0～100．0g／L范围内呈良好线性关系（r=0．9999）,加标回收率为97．7％～102．2％,测定结果的相对标准偏差为1．04％（n=6）。该方法检出限低,操作简便、快捷、准确,线性范围宽,适用于糖果等食品中钛含量的准确测定。     

微波消解-电感耦合等离子体质谱法测定铁矿石中的26种痕量元素

建立了一套完整的电感耦合等离子体质谱法测定铁矿石中26种痕量元素的检测分析方法。实验中,将微波消解与电感耦合等离子体质谱法相结合,优化了电感耦合等离子体质谱仪的仪器参数,利用基体匹配法和内标法校正基体效应。检出限、加标回收、精密度相关实验表明:该方法检出限在0.03～0.87μg/g之间;加标回收率在95～105%之间;精密度在0.1～3.0%之间。该方法简单、快速、高效,可满足目前市场上对铁矿石中杂质元素含量检测的需求。     

Determination of total polyphenols in tea by a flow injection-fiber optic spectrophotometric system

A flow injection-fiber optic spectrophotometric system was established for the online determination of total polyphenol content in tea samples. The method was based on the chromogenic reaction between the phenolic compounds (gallic acid) and ferrous tartrate which was used as the colorimetric reagent and the absorption was determined at the maximum absorption wavelength of 540?nm at 20°C and pH 7.5. The calibration curve from standard solutions of gallic acid was linear in the range from 0.010 to 0.100?mg/mL with a correlation coefficient of 0.9970. The relative standard deviation of polyphenol measurements for eight tea samples was between 0.55 and 3.18%. It can be concluded that the proposed method has allowed simple, fast, and accurate determination of total polyphenol content in tea products.     

阳离子交换分离ICP/MS测定U_3O_8中的微量稀土元素

用硝酸溶解 U3 O8,通过阳离子交换柱 ,实现稀土元素与铀的分离。铀中的稀土元素回收率为 98%～1 0 6%。方法的检测限为 0 .1 ng/ g(3 σ,n=6) ,并讨论了分离条件、仪器参数的最优化选择及残留铀量对稀土元素测量的影响。     

ICP/MS法测定中国参考人组织样品中痕量钍、铀、铯含量的研究

本文采用ICP-MS法对成年人器官组织中痕量钍、铀、铯进行了研究,选择了测定的仪器参数,检查了测定中的干扰和影响;用铼(Re)作为内标元素补偿基体抑制效应和灵敏度的漂移~(1,2,3)。钍、铀、铯的检出限为(0.0057-0.0178)μg·L~(-1)。随同样品分析了NIST SRM 1566a牡蛎、8414牛肌肉、1486骨粗粉标准参考物质,测得值与标准参考值基本相符。在严格分析质控基础上,用混酸消解样品,不须分离富集,直接对成年人肝、肾、肺、肌肉、骨粉中钍,铀,铯元素进行测定。