Determination on Heavy Metals Content of Achyranthes bidentata Blume. through Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

[Objective] The inductively coupled plasma mass spectrometry(ICP-MS)was constructed to determine the contents of lead,cadmium,mercury and arsenic in Archyranthes bidentata Blume.[Method]Under the optimum operation condition of ICP-MS,the samples were digested by microwave.The element 114In was taken as an internal standard element to compensate body effect and ICP-MS method was used to determine the contents of lead,cadmium,mercury and arsenic.[Result]For the determined elements,the correlation coefficient(r)of standard curve was over 0.9995 and recovery rate was from 96.7% to 106.4% while RSD was less than 11.2%.The result of determination showed that the heavy metal content in Archyranthes bidentata Blume.beyond standard was serious.[Conclusion]The constructed ICP-MS method with simple operation,rapid response,accuracy and high sensitivity in this experiment could be used for quality control of Chinese medicinal materials by detecting heavy metal contents in different Chinese medicinal materials from original places.

Inductively coupled plasma mass spectrometry (ICP-MS) and its application in life sciences

Inductively-coupled plasma mass spectrometry (ICP-MS) has made much progress since its birth in the late 1990s. This paper will give a rather systematic overview on the use of this technique in new devices and technologies related to plasma source, sample-introducing device and detecting spectrometer etc. In this overview, an emphasis will be put on the evaluation of the ICP- MS technique in combination with a series of physical, chemical and biological techniques, such as laser ablation (LA), capillary electrophoresis (CE) and high performance liquid chromatograph (HPLC), along with their representative high accuracy and high sensitivity. Finally, comprehensive and fruitful applications of the ICP-MS and its combinative techniques in the detection of trace metallic elements and isotopes in complex biological and environmental samples will be revealed.

ICP-MS测定HTK液中微量钙含量

目的:基于电感耦合等离子体质谱法(ICP-MS),建立一种测定HTK液中微量钙元素的测试方法。方法:将HTK浓缩液使用1%的硝酸进行稀释,添加钙元素标准溶液制备成系列钙元素标准溶液,选择铟作为内标,采用标准加入法并扣除空白进行测定,并且对方法进行精密度、准确度和加标回收进行评估。结果:钙元素含量的测定在0~1.5mg/L的范围内呈现良好的线性关系(R=0.9999,n=7),相对误差(RE)均小于2%,日内精密度RSD均小于1%,回收率为95%~105%。结论:本研究所建立的电感耦合等离子体质谱法能够很好地测定HTK液中微量钙含量,该方法线性范围好,且具有良好的精密度和准确性,为标准完善、质量监督提供了参考依据。

ICP-MS测定黄豆中26种无机元素

本文利用微波消解对黄豆进行前处理,采用电感耦合等离子体质谱法(Inductively Coupled Plasma Mass Spectrometer,ICP-MS)对消解液中26种元素的含量进行测定,对方法的线性、精密度、准确度及质控样品进行验证。结果表明,各元素标准曲线的相关系数均≥0.9990,线性关系良好,检出限为0.000583~0.453000 mg·kg^(-1),相对标准偏差≤5.513%,加标回收率为77%~113%,说明该方法能准确检测黄豆中无机元素,满足日常监测需求。

全自动消解-电感耦合等离子体质谱(ICP-MS)法测定海洋沉积物中重金属

目前海洋沉积物前处理主要通过电热板消解,但该方法存在消解不完全、前处理时间长、重复性较差以及手工消解操作繁琐等问题。为提高海洋沉积物中重金属消解效率,通过考察硝酸、盐酸、氢氟酸和高氯酸组合酸体系比例和最高消解温度对海洋沉积物预处理的影响,确定了最优的消解条件,建立了全自动消解-电感耦合等离子体质谱(ICP-MS)法测定海洋沉积物中重金属的方法。结果显示,硝酸占比越高各元素消解效果越好,盐酸用量不宜过多,逆王水消解比例最好。最优预处理条件为9 mL硝酸、3 mL盐酸、4 mL氢氟酸和2 mL高氯酸于160℃高温消解,所得曲线各元素相关性系数均大于0.999,经海洋沉积物标准样品(GBW07314)和实际样品的验证,与国家标准方法(GB/T 20260—2006)相比,优化条件下各元素精密度和正确度均显著提高、检出限更低。各元素的相对标准偏差为0.50%~3.4%,加标回收率均在84.2%~102%。方法自动化程度高、操作简便,可实现大批量样品预处理,适用于海洋沉积物中重金属元素的测定。

ICP-MS灵敏度及检出限测量不确定度评定

电感耦合等离子体质谱仪(Inductively Coupled Plasma Mass Spectrometer)校准过程中的不确定度评估是量值溯源过程的重要组成部分。本文依据JJF 1059.1-2012《测量不确定度评定与表示》和JJF 1159-006《四级杆电感耦合等离子体质谱仪校准规范》等技术规范,建立ICP-MS灵敏度及检出限测量结果的不确定度评定数学模型,系统分析测量不确定度来源,对测量结果进行不确定度评定。结果表明:ICP-MS灵敏度的相对扩展不确定度为6.1%,k=2,测量结果的不确定度主要来源于标准物质引入的不确定度;ICP-MS检出限的相对扩展不确定度为47%,k=2,测量结果的不确定度主要来源于灵敏度引入的不确定度。本文为系统评估ICP-MS的灵敏度及检出限的不确定度和开展该项目的校准、研制ICP-MS校准用标准物质提供参考。

Laser-Ionization TOF Mass Spectrometer Characterization of Benzene Destruction in Atmospheric Pressure Pulsed Discharge

Benzene is a major industrial air pollutant and can cause serious human health disorders. In this paper an investigation on benzene destruction, in an atmospheric-pressure fast-flow pulsed DC-discharge by means of laser ionization combined with time-of-flight （TOF） mass spectrometry, is reported. Most by-products including transient reactive species from the benzene discharge were characterized by molecular beam sampling combined with TOF mass spectrometry. It is showed that, with a gas mixture of 0.5% C6H6 in Ar, benzene can be effectively destroyed by discharge plasma. The intermediate species consisted of small fragments of CnHm （n=3-5, m = 1-11）, cycle-chain species of CnHm （n =6-9, m = 7-10） and polycyclic species CnHm （n ≥9, m = 8-12）. The alternation of mass peaks （intensity） with even/odd electrons was observed in the measured mass spectra. The results indicated that the alternation is mainly due to the different ionization potentials of the open shell and close shell species. Based on the examination of the features of the species＇ composition, the primary reaction pathways are proposed and discussed.

Determination of impurity elements in MnZn ferrites by inductively coupled plasma mass spectrometry

An inductively coupled plasma mass spectrometry(ICP-MS) method was developed for the determination of Na, Mg, Al,K, Ca, Ti, Cr, Co, Ni, Cu, Ga, As, Mo, Ag, Cd and Pb in MnZn ferrites. The sample was digested by HNO3+HCl with microwave digestion followed by dilution with ultrapure water, then the above 16 impurity elements in the solution were analyzed directly by ICP-MS. The impurity elements were introduced by the helium gas or hydrogen gas into the octopole reaction system(ORS) to eliminate the polyatomic interferences caused by the high salty matrixes. The matrix effect was minimized through matrix matching,and Be, Y and Rh were used as internal standard elements. The working parameters of the instrument were optimized. The results show that the method has good precision and high accuracy. The detection limits for the investigated elements are in the range of0.9-37.5 ng/L, the relative standard deviation of each element is within 1.1%-4.8%, and the recovery of each element is 90%-108%.

Uncertainty Evaluation of Simultaneous Determination of Lead, Cadmium and Arsenic in Cosmetics by Inductively Coupled Plasma Mass Spectrometry

This study aimed to evaluate the uncertainty of simultaneous determination of lead(Pb),cadmium(Cd)and arsenic(As)in cosmetics by microwave digestion-inductively coupled plasma mass spectrometry(ICP-MS)with ^72Ge,^115In and ^209Bi as internal standards.According to the method of Safety and Technical Standards for Cosmetics(2015),a mathematical model was established to evaluate the sources and components of uncertainty for the determination of lead,cadmium and arsenic in cosmetics.The results showed that the uncertainties in the determination of lead,cadmium,and arsenic elements in cosmetics were(10.1±0.6)mg/kg,k=2,(4.84±0.28)mg/kg,k=2,(2.04±0.18)mg/kg,k=2,respectively.The main factors that affect the uncertainty of determination results were standard substance,calibration curve,recovery and measurement repeatability.

封闭酸溶-ICP-MS分析超细地质样品的条件优化

Using ultra-fine sample for determination 42 elements by pressurized acid digestion -ICP-MS, the mass of test portion can be reduced to 2 mg yet maintain the representation. And acid used for digestion could be reduced to less than 0.5 mL, reaction time also largely reduced.

ICP-MS法分析过氧化氢、硝酸、硫酸中的金属杂质

Inductively coupled plasma mass spectrometry (ICP-MS) was used to detect trace metal impurities in reagents such as H2O2, HNO3and H2SO4. The limit of detection to metal elements can be down to 2-20 ng/L in H2O2 and HNO3 and 0.1-1.0 ng/L in H2SO4.

应用ICP-MS与AAS测定食品中铅、镉、铜方法研究及比较

目的:建立微波消解、电感耦合等离子体质谱法(ICP-MS)同时测定食品中微量元素的方法,并与国标法原子吸收分光光度法(AAS)进行了比较。方法:应用微波消解进行样品前处理,使用电感耦合等离子体质谱与原子吸收分光光度计分别测定三十余种食品中铅、镉、铜含量。结果:线性相关系数均大于三个9,方法的精密度均小于8.0%,国家标准物质:小麦粉(GBW08503b)、杨树叶(GBW08513)、贻贝(GBW08571)测定值均在标准值范围内,两种方法的测定值基本吻合。结论:ICP-MS法3种元素可同时分析,抗干扰强,但仪器成本高;AAS法每一元素需分别测定,测定周期较长,干扰较大,特别是高盐样品需稀释后测定,但仪器成本低,普及率高。

样品粒度对封闭酸溶-ICP-MS分析性能的影响

To improve precision of analytical results of pressurized acid digestion-ICP-MS, the first step is to improve the homogeneity by reducing the particle size of sample. Using of ultra-fine sample (-500 mesh) can reduce the mass of the sample and the acid. The satisfactory precision is achieved at 2 mg sampling mass.

MC-ICP-MS高精度测定Li同位素分析方法

以不同浓度Li元素标准样品和K、Ca、Na、Mg、Fe单元素标准样品的混合溶液为研究对象,采用3根阳离子交换树脂（AG50 W-X8,200-400目）填充的聚丙烯交换柱和石英交换柱对Li进行分离富集,淋洗液分别为2.8 mol/L HCl、0.15 mol/L HCl以及0.5 mol/L HCl 30%乙醇,淋洗液体积小,仅为38 mL。分离回收率高,均大于97.6%。国际标样AGV-2（相对于IRMM-016）、BHVO-2（相对于IRMM-016）和IRMM-016（相对于L-SVEC）的δ7Li值分别为（5.13±0.94）‰（2σ,n=10）、（4.08±0.60）‰（2σ,n=4）和（0.038±0.73）‰（2σ,n=10）,与前人分析结果吻合,分析精度与国际同类实验室水平相当。并对比了马里兰大学同位素实验室和笔者实验室对同种岩石矿物样品的分析结果,在误差范围内具有很好的一致性。此外,对美国地质调查局提供的准标样NKT-1霞石岩（相对于IRMM-016）给出了定值,δ7Li值为（8.71±0.46）‰（2σ,n=4）。因此,本方法可用于测定天然样品的Li同位素组成。

HPLC-ICP-MS在工业废渣中硒形态分析中的应用

由于我国大量工业废渣的堆放方式原始、粗放,导致了大量重金属离子和有毒有害元素在自然环境中极易迁移并造成污染。为了掌握废渣中硒在多重氧化态中含量及形态,采用改进的SES法,连续浸提了废渣样品中硒的水溶态、交换态、酸溶态、有机态、单质态及残渣态,以ICP-MS测定提取液中总硒含量,同时,利用HPLC-ICP-MS研究了硒的形态。研究表明:CCT动态反应碰撞模式能有效降低多原子离子检测的干扰,优化ICP-MS检测环境;工业废渣中的硒含量极高,在自然环境中易发生迁移,尤其是酸性环境下;前三态的硒含量超过了总硒的50%,且主要以毒性较高的亚硒酸盐形式存在,小部分以硒酸盐形式存在,含硒工业废渣存在较大的潜在环境风险。

应用ICP-MS的ORS技术进行人体铁稳定同位素代谢示踪研究的初探

目的应用四极杆型电感耦合等离子体质谱仪(ICP-MS)配合最新的八极杆碰撞/反应池(ORS)消干扰技术进行Fe的同位素比测定研究。方法于现场进行人体代谢试验,受试者口服57Fe稳定性同位素示踪剂,以卡红为标志,粪便监测法收集试验期内的所有粪样,测定粪样中57Fe/56Fe的比值。结果运用ICP-MS的ORS技术可消除由Ar等离子体本身以及样品中存在的Ca等产生的多原子离子对Fe带来的干扰;稀释实际样品到一定范围,基体干扰可忽略不计;标准样品和实际样品短期及长期精密度均小于0.3%;测定两组受试者粪样中的57Fe/56Fe的比值,发现代谢后排泄出的57Fe遵循一定的变化趋势,从而可以测定人体对Fe的代谢吸收比率。结论该技术可准确测定粪样中57Fe/56Fe的比值,可以用来计算评价膳食中铁吸收率的情况,追踪铁在人体中的代谢过程。

MC-ICP-MS测量Ru同位素丰度比值的质量歧视校正

采用MC-ICP-MS测量Ru同位素丰度比时,存在较大的质量偏倚。利用IsoprobeMC-ICP-MS测量了RuCl3中Ru同位素丰度比值,并利用幂、指数以及通用幂校正规律(GPL)对Ru同位素丰度比值测量的质量偏倚进行了校正。结果表明,以100Ru/102Ru、104Ru/102Ru作为内标,采用GPL校正质量偏倚,得到的Ru同位素丰度更接近于天然值,与天然值的偏差在(20～650)×10-6之间。

ICP-MS测定小麦中的铅、镉、汞、砷

重金属污染及其测量方法一直以来都是粮食检测部门关注的重点。本文探索采用微波消解结合ICP-MS的方法同时测定小麦中铅、镉、砷、汞含量,并根据此法测量结果评价了江苏小麦重金属污染情况。结果表明,该方法测试铅、镉、砷、汞含量的相关系数(r2)分别为0.9991、0.9999、0.9999、0.9997;检测限分别为0.05μg/kg、0.01μg/kg、0.02μg/kg、0.06μg/kg;精密度分别为3.7%±2.8%、3.8%±2.8%、2.8%±1.9%、3.7%±3.5%;加标回收率分别为99.5%±4.4%、98.2%±4.6%、100.6%±7.1%、97.9%±10.8%;2014年江苏小麦铅、镉、砷、汞含量未见超标。结果认为,微波消解结合ICP-MS是一种高效、准确的小麦铅、镉、汞、砷含量测定方法。

ICP-MS法测定金属铅及氧化铅中痕量金

研究金属铅及氧化铅中痕量金的ICP-MS测定方法。通过向金属铅试样中加入适量的银,直接在850～900℃进行灰吹,使金与铅及杂质分离并富集,对于氧化铅采用造渣制成铅扣再灰吹的方法,实现金与铅及杂质的分离。合金颗粒用王水溶解,溶液用ICP-MS方法测定。测定方法可准确测定金属铅及氧化铅样品中10^(-9)级的金。样品加标回收率在98％～102％之间。

HPLC-ICP-MS或HPLC-FAAS法分离测定硒化合物（英文）

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。