ICP-MS法同时测定烟草中17种微量元素

采用微波消解前处理样品、电感耦合等离子体质谱检测的方法,同时测定了烟叶中铍(Be)、钛(Ti)、钒(V)、铬(Cr)、镍(Ni)、铜(Cu)、砷(As)、锶(Sr)、钼(Mo)、银(Ag)、镉(Cd)、铯(Cs)、钡(Ba)、铊(Tl)、铅(Pb)、钍(Th)和铀(U)共17种元素,回收率90·27%~110·4%,检出限0·3521~345·3ng/L,相对标准偏差1·65%~9·86%。实验结果表明,该方法能满足痕量分析的要求。用此方法对来自5个地区的烟叶样品进行了考察,研究了以上元素随产地、部位不同的分布特性,发现同一品种不同地区、部位的烟叶中上述元素的含量存在一定的差别。     

碰撞/反应池电感耦合等离子体质谱(ICP-MS)法测定血液中16种元素

采用直接稀释法,使用电感耦合等离子体质谱仪测定血液中元素的过程中,由于血液样本成分复杂,容易产生较大的基体效应,同时一系列多原子离子(例如,⁴⁰Ar¹⁶O⁺、⁴⁰Ar⁴⁰Ar⁺等)会影响与其有相同质荷比核素的检测,进而影响测定结果。通过使电感耦合等离子体质谱仪(ICP-MS)分别工作在标准模式、氦气模式和氢气模式下,对比仪器的氧化物离子产率(CeO/Ce)、双电荷离子产率(Ba⁺⁺/Ba)、灵敏度与检出限情况,同时对氢气模式时仪器上述指标优于其他两种模式的潜在机理进行分析;随后再使用氢气作为碰撞/反应池气体,使用直接稀释法分析全血标准品以及小鼠血液样本中16种元素的含量情况。结果表明,使用氢气作为碰撞/反应池气体时,氧化物离子产率(CeO/Ce)、双电荷离子产率(Ba⁺⁺/Ba)、灵敏度与检出限情况优于标准模式和氦气模式,且16种元素在0.5～100.0μg/L线性关系良好(R²≥0.999...     

Determination of organic and inorganic mercury species in water and sediment samples by HPLC on-line coupled with ICP-MS

This paper describes a preconcentration method for Hg²⁺ and MeHg⁺ in water samples using sodium diethyldithiocarbamate immobilized in polyurethane foam (PU-NaDDC) and an extraction method for several mercury species in sediment samples, including MeHg⁺, EtHg⁺ and PhHg⁺, which is simple, rapid, and uses a single organic solvent. Separation and measurement were done by high-performance liquid chromatography on-line with inductively coupled plasma mass spectrometry (HPLC/ICP-MS). Initially, the test of recovery was applied using procedures compatible with HPLC. Under the optimum extraction conditions, recoveries of 96.7, 96.3 and 97.3% were obtained for MeHg⁺, EtHg⁺, and PhHg⁺, respectively, from n = 4 spiked sediment samples. This study also demonstrates that the combination of solid-phase extraction on PU-NaDDC with HPLC separation and ICP-MS detection is an effective preconcentration procedure for simultaneous measurement of Hg²⁺ and MeHg⁺ at ultra-trace levels in water samples. The application of the proposed procedure to the determination of mercury species in drinking water sample was investigated. The proposed method clearly gave satisfactory average recoveries between 93.7 and 101.5%.     

珍珠中痕量稀土元素的ICP-MS测定及其分布特性

探讨了等离子体质谱(ICP-MS)分析珍珠样品中稀土元素的基体效应及多原子离子干扰,并采用干扰校正因子进行有效的校正,以In-Rh双内标校正体系进行分析信号动态漂移的监控和补偿,建立了珍珠样品中稀土元素的ICP-MS分析方法。方法的定量检出限为0．1～0．5ng／g,RSD≤15％(n=5)。所建立的方法用于标准物质Gui-1、Gui-2、Gui-3及人工养殖珍珠的分析。珍珠中稀土元素的分布与分馏特性与其生长环境密切相关。     

电感耦合等离子体质谱法测定血液和精液中的硼

采用HNO3-H2O2和氨水-甘露醇两种方法处理样品,电感耦合等离子体质谱法（ICP-MS）测定血液和精液中的硼。Be作内标补偿基体效应,并用标准加入法验证了方法的可靠性,标准加入法与外标法测定结果相吻合。在测定B的同时,还可进行Cr、Cu、Cd、Ba、Sr、Mn、Co、Tl、Li、Pb、Zn、Sc、Ti、V、As等多元素测定。两种样品处理方法的测定值呈显著正相关（r=0.99919）。方法检出限为0．11ng／mL（氨水-甘露醇法）,0.06ng／mL（HNO3-H2O2）。已用于测定某硼矿区血液和精液样品中的硼。     

Study on the interference elimination of trace cadmium in superalloy by ICP-MS / MSEI北大核心CSCD

A triple quadrupole inductively coupled plasma mass spectrometry (ICP-MS / MS) method was developed for the determination of trace Cd in superalloys. Meanwhile, the interference elimination effects of different collision / reaction gases (He, O2 and NH3) in single quadrupole mode (SQ) and double quadrupole mode (QQQ) were investigated. The results indicated that the modes of QQQ-O2 and QQQ-NH3 possessed satisfactory interference elimination effect than the others. The optimal flow rates of O2 and NH3 were 0. 75 mL / min and 0. 50 mL / min, respectively. In order to verify the interference elimination effect, the recovery rate of 0. 1 μg / g Cd in 0. 10 mg / g to 100 mg / g Mo content solutions, as well as the determination results of superalloy standard substance and the actual sample were investigated. The measured value was within the range of the standard value, and the measured value of the actual sample was consistent with that of the hydride generation atomic fluorescence method. Therefore, the proposed method can eliminate the polyatomic ions interference of Mo on trace Cd. © 2022, Youke Publishing Co.,Ltd. All rights reserved.     

ICP-MS 法测定高纯氧化铕中稀土杂质的研究

深入考察了ＩＣＰ－ＭＳ法测定高纯氧化铕时基体对稀土杂质测定的影响,研究了Ｐ５０７萃淋树脂分离大量基体Ｅｕ２Ｏ３的实验条件,建立了采用内标补偿直接测定大部分稀土杂质和经Ｐ５０７萃淋树脂分离基体后测定被干扰离子Ｔｍ相结合的高纯Ｅｕ２Ｏ３中稀土杂质的ＩＣＰ－ＭＳ分析方法。方法检出限为０．００５～０．０２１μｇ／Ｌ,加标回收率为８４％～１１２％。ＲＳＤ为１．４％～８．１％。本法适用于质量分数为９９．９９％～９９．９９９９％的高纯Ｅｕ２Ｏ３中稀土杂质的分析。     

微波消解法-电感耦合等离子体质谱(ICP-MS)法测定韭菜中11种元素

为快速、准确测定韭菜中多元素含量,采用微波消解法对韭菜中样品进行消解处理,优化了前处理方法、ICP-MS工作条件和检测方法,利用微波消解-电感耦合等离子体质谱法测定韭菜中Pb、Cd、Se、As、Zn、Cu、Ni、Fe、Cr、Ca、K等11种元素含量。结果表明,在硝酸-双氧水(7:1)体系中,消解功率1550W,温度梯度为120℃-160℃-195℃,总时长为45min,赶酸温度选择150℃,可将韭菜完全消解,并且ICP-MS射频功率设为1550W,运用在线内标的检测方式降低非质谱干扰。11种元素回归系数R₂^{均大于0.999,方法检出限为}0.002～0.100μg/kg,方法定量限为0.006～0.300μg/kg。方法回收率88.0%～102.7%,相对标准偏差为1.8%～4.6%,可以满足韭菜中多种元素同时测定的需求。方法具有灵敏度高、线性范围宽、准确性高等特点,可为韭菜样品的多元素同时测定提供可靠的方法支撑。     

电感耦合等离子体质谱法同时测定成品烟烟丝中7种微量元素

采用微波消解前处理样品,电感耦合等离子体质谱检测,同时测定了成品烟烟丝中Cr、Ni、Cu、As、Se、Cd、Pb等7种微量元素。方法的回收率92.8%~120%,检出限25.2~245 ng/L,相对标准偏差均小于10%。分析和比较了5种国外卷烟和10种国内卷烟烟丝中7种元素的含量。     

ICP-MS法测定中成药中微量砷铅镉和汞

对药品中毒性较大的有害元素指标进行严格限量控制是国际通用法规的重要规定。目前,已报道的光学分析方法归纳起来有：原子吸收光谱法、电感耦合等离子体原子发射光谱法、分光光度法、荧光分析法、化学发光法。在诸多方法中ICP-AES由于检出限低,精密度高、基体效应小、线性范围宽和多元素同时测定等优点,已在中草药微量元素分析中得到广泛应用。而ICP-MS比ICP-AES检出限改善了2-3个数量级,在中药微量分析中的应用开始受到人们的重视。本文利用微波消解ICP-MS法对几种中药及中成药中的As、Pb、Cd、Hg进行了测定,结果满意。     

电感耦合等离子体质谱法测定高纯铼中26种痕量杂质元素

以电感耦合等离子体质谱法(ICP-MS)测定了高纯铼中26种杂质元素含量。应用反应池技术消除了复合离子对K、Ca、Fe等元素的干扰,采用干扰方程校正技术消除了Re氧化物对Tl的质谱重叠干扰,未受干扰的其它杂质元素采用内标校正法直接测定。考察了溶液酸度、基体效应等条件对测定的影响,优化选择了测定同位素和内标元素。方法测定下限介于0.12～5.0μg/g,加标回收率在90%～110%之间,相对标准偏差小于10%。方法可以满足4N5高纯铼的测定。     

Determination of mercurial species in fish by inductively coupled plasma mass spectrometry with anion exchange chromatographic separation

This work demonstrated the feasibility of mercury speciation analysis by anion exchange chromatographic separation with inductively coupled plasma mass spectrometry detection. For the first time, by complexing with the mobile phase containing 3-mercapto-1-propanesulfonate into negatively charged complexes, fast separation of inorganic mercury (Hg²⁺), monomethylmercury (MeHg), ethylmercury (EtHg) and phenylmercury (PhHg) was achieved within 5 min on a 12.5-mm strong anion exchange column. The detection limits for Hg²⁺, MeHg, EtHg and PhHg were 0.008, 0.024, 0.029 and 0.034 μg L⁻¹, respectively. The relative standard deviations of peak height and peak area (5.0 μg L⁻¹ for each Hg species) were all below 3%. The determined contents of Hg²⁺, MeHg and total Hg in a certified reference material of fish tissue by the proposed method were in good accordance with the certified values with satisfactory recoveries. The relative errors for determining MeHg and total mercury were −2.4% and −1.2%, respectively, with an acceptable range for spike recoveries of 94–101%. Mercury speciation in 11 fish samples were then analyzed after the pretreated procedure. The mercury contents in all fish samples analyzed were found compliant with the criteria of the National Standards of China.     

Development of an ICP-MS immunoassay for the detection of anti-erythropoietin antibodies

A sandwich-type immunoassay linked with inductively coupled plasma mass spectrometry (ICP-MS) has been developed for the detection of anti-erythropoietin antibodies (anti-EPO Abs). Recombinant human erythropoietin (rhEPO) was immobilized on the solid phase to capture anti-rhEPO Abs specifically. After the immunoreactions with Au-labeled goat-anti-rabbit IgG, a diluted HNO₃ (2%) was used to dissociate Au nanoparticles which was then introduced to the ICP-MS for measurements. Under the optimized conditions, the calibration graph for anti-EPO Abs was linear in the range of 35.6-500 ng mL⁻¹ with a detection limit of 10.7 ng mL⁻¹ (3σ, n = 9). The relative standard deviation (R.S.D.) for three replicate measurements of 30.9 ng mL⁻¹ of anti-EPO Abs was 8.43%. The recoveries of anti-EPO Abs in sera at the spiking level of 50, 100, 150, 200 and 400 ng mL⁻¹ were 99.2%, 101.5%, 95.0%, 94.0% and 102.9%, respectively. For the real sample analysis, 26 samples from healthy people and 53 samples from patients with rhEPO treatments were studied. One sample from patients showed significantly higher anti-EPO Abs from other samples, indicating a possibility of immune response of this patient.     

电感耦合等离子体质谱法测定包头地区土壤中的钍

采用电感耦合等离子体质谱法(ICP-MS)对土壤中痕量的钍进行了分析。讨论了基体干扰和质谱干扰,采用稀释法降低基体干扰,并进行了内标选择实验,确定了238U作为方法的内标补偿基体效应。通过对土壤标准物质分析,用王水和HF混合酸微波消解样品,加HC lO4蒸干后用王水溶解残渣。观察到仪器对于Th的测定在不同稀释程度下的线性关系良好。标准加入回收率在93%~106%。方法检出限为0.6μg/L(232Th)。     

电感耦合等离子体质谱法测定黄沙土壤中铅同位素比

用电感耦合等离子体质谱法（ＩＣＰ—ＭＳ）测定了５个黄沙原土样品中铅同位素比２０７Ｐｂ／２０６Ｐｂ、２０８Ｐｂ／２０６Ｐｂ，样品来自被认为是黄沙气溶胶源地区，为了使铅同位素测量中质量偏差和漂移减至最少，在样品中加入了铊标准溶液，测量２０５Ｔｌ／２０３Ｔｌ比，校正质量数差别选择的影响．同时，采用ＩＣＰ—ＭＳ和电感耦合等离子体原子发射光谱法（ＩＣＰ一ＡｌＳ）测定了随粒径变化样品中１２种元素浓度的变化．     

Determination of rhodium: Since the origins until today: ICP-OES and ICP-MS

Rh is contained in catalyst in much smaller quantities than Pt. For this reason, the database for this metal with respect to emissions from catalytic converters is much smaller than that for platinum, thus precluding a quantitative risk assessment.Accurate determinations of the rhodium have always been difficult tasks. The metal is often present at trace levels in sample types of complex composition. This situation has improved recently due to developments of instrumental methods and their applications to analyses of rhodium in a variety of matrices. The purpose of this review is to describe the analytical sensitive methods by inductively coupled plasma spectrometry.     

电解分离-电感耦合等离子体质谱法测定高纯铜中的杂质元素

建立了电解分离-电感耦合等离子体质谱法测定纯铜中17种杂质元素(Be,Mg,Al,P,Ti,Cr,Mn,Co,Ni,As,se,Zr,Cd,Sn,Sb,Te和Pb)的方法.通过控制电流分离基体铜,大于99%的铜沉积至阴极,各杂质元素的回收率大于90%.研究了电解后电解液的酸效应、残余铜的影响和基体效应.结果表明,选用合...     

ICP-MS法测定土壤中有效态砷的研究

分别以等离子体质谱法和原子荧光法,测定了国标土壤样品中有效态砷的含量,研究了两种方法的准确度;对等离子体质谱测定方法做消除基体干扰的对比研究。两种方法的测定值均在土壤样中有效砷的允许误差范围内,ICP-MS法的检出限为2.8 ng/g,精密度(RSD)在10％以下,符合分析测定要求。     

On‐Line Determination of Arsenic Species in Sea Water by Selective Hydride Generation Coupled with Inductively Coupled Plasma — Mass Spectrometry

A method for direct de termination of total in organic arsenic (III+V), arsenic (III) and dimethylarsinate (DMA) in sea water was developed by combining continuous‐flow selective hydride generation and inductively coupled plasma mass spectrometry (ICP‐MS) is presented. The principle underlying selective hydride generation is based on proper control of the reaction conditions for achieving separation of the respective arsenic species. The effects of pH and composition of reaction media on mutual interference between the arsenic species were investigated in detail. The results indicate that the appropriate media for the selective determination of total in organic arsenic, DMA and As(III) are 6 M HNO₃, acetate buffer at pH = 4.63 and citrate buffer at pH = 6.54, respectively. The concentrations of total inorganic arsenic species, As(III+V), and As(III) were respectively deter mined and that of As(V) was obtained by the difference between them. As to the concentration of DMA, it was obtained after correction from the interference caused by As(III) and As(V). By following the established procedure, the detection lim its (as based on 3‐sigma criterion) for As(III+V), As(III) and DMA were 0.050, 0.009, and 0.002 ng/mL, respectively. There liability of the pro posed method was evaluated in terms of precision and spike addition. The results indicated that the precision of better than 3% and spike recovery of 95 to 105% for all the arsenic species tested in the natural sea water samples can be obtained.     

Determination of chromium, iron and selenium in foodstuffs of animal origin by collision cell technology, inductively coupled plasma mass spectrometry (ICP-MS), after closed vessel microwave digestion

The determination of chromium (⁵²Cr), iron (⁵⁶Fe) and selenium (⁸⁰Se) isotopes in foodstuffs of animal origin has been performed by collision cell technology (CCT) mode using an inductively coupled plasma mass spectrometry (ICP-MS) as detector after closed vessel microwave digestion. To significantly decrease the argon-based interferences at mass to charge ratios (m/z): 52 (⁴⁰Ar¹²C), 56 (⁴⁰Ar¹⁶O) and 80 (⁴⁰Ar⁴⁰Ar), the gas-flow rates of a helium and hydrogen mixture used in the hexapole collision cell were optimised to 1.5 ml min⁻¹ H₂ and 0.5 ml min⁻¹ He and the quadrupole bias was adjusted daily between −2 and −15 mV. Limits of quantification (LOQ) of 0.025, 0.086 and 0.041 mg kg⁻¹ for Cr, Fe and Se, respectively, in 6% HNO₃ were estimated under optimized CCT conditions. These LOQ were improved by a factor of approximately 10 for each element compared to standard mode.Precision under repeatability, intermediate precision reproducibility and trueness have been tested on nine different certified reference materials in foodstuffs of animal origin and on an external proficiency testing scheme. The results obtained for chromium, iron and selenium were in all cases in good agreement with the certified values and trueness was improved, compared to those obtained in standard mode.