ICP-MS法同时测定金属包装材料中8种可溶性有害元素

建立了电感耦合等离子体质谱(ICP-MS)法同时测定金属包装材料中砷、钡、镉、铬、铅、锑、硒、汞等8种可溶性有害元素的分析方法,全面考察了消解剂种类及其用量、内标元素的选择及方法的干扰等影响其测量的各种因素,确定了最佳的实验测定条件。方法的检出限为0.03~0.18μg/L,相对标准偏差(RSD)小于5%,加标回收率为87.4%~118.1%。采用该法对金属包装材料实际样品进行了分析,结果表明,此方法简单、准确、重现性好。     

电感耦合等离子质谱法测定石英砂中十四种痕量杂质元素

文章根据不同石英砂的矿相、加工工艺,建立了密闭消解和微波消解等样品处理方法,利用电感耦合等离子体质谱仪（ICP-MS）对石英砂中痕量杂质元素进行检测。采用Sc为内标补偿基体效应和仪器漂移。检测结果表明,密闭酸溶法与微波消解法无显著性差异（P≥0.05）;ICP-MS检测石英砂中痕量杂质元素准确度和精确度高,检测线性范围宽,检出限低,分析快速。测定结果的相对标准偏差（RS D）0.2%～5.0%,检出限为0.009～0.093 ng/ml。     

ICP-MS法比较肉苁蓉在传统中药和中药饮片中7种无机元素的含量

建立微波消解-电感耦合等离子体质谱(ICP-MS)法同时测定肉苁蓉及其饮片中锶、铬、钴、镍、铜、锌、铅等7种无机元素含量的方法.以硝酸-高氯酸-氢氟酸为消解体系对样品进行微波消解,采用ICP-MS法同时测定.方法 学验证表明:7种元素均在0 ～ 500μg/L的质量浓度范围内线性关系良好(r2＞0.999);检出限在0...     

ICP-MS法在测定痕量贵金属中的应用探析

ICP-MS技术测量手法是对元素的含量进行分析的一种技术手段,主要的测定的范围是痕量与超痕量元素。随着时代的进步与科技的发展,这种技术也得到了革新与完善。文中主要针对ICP-MS技术分析性能在贵金属中的应用进行了简要分析,仅供专业人士的参考与借鉴。     

ICP-MS测定5种中药注射液中重金属及有害元素

建立电感耦合等离子体质谱法(ICP-MS)测定复方蒲公英注射液、野菊花注射液、肿节风注射液、白花蛇舌草注射液和夏天无注射液中铜(Cu)、砷(As)、镉(Cd)、铅(Pb)和汞(Hg)5种重金属及有害元素含量的方法。样品用2%硝酸(V/V)直接稀释,以72Ge、115In、185Re为内标,采用ICP-MS测定溶液中元素含量。方法学验证表明:Cu、As、Cd、Pb在0.5～50μg/L和Hg在0.5～10μg/L的质量浓度范围内线性关系良好(r2>0.999);低、中、高3种浓度水平,复方蒲公英注射液、夏天无注射液、肿节风注射液、野菊花注射液、白花蛇舌草注射液中5种元素的平均回收率(n=3)分别为90.7%～121.2%、83.4%～119.9%、90.8%～116.3%、86.4%～109.0%、85.0%～118.0%,重复性RSD(n=3)分别为1.4%～9.8%、0.2%～6.7%、0.4%～7.4%、0.6%～10.0%、0.1%～11.1%;5种注射液中Cu、As、Cd、Pb、Hg的LOQ分别为0.002 1 mg/L、0.001 6 mg/L、0.000 56 mg/L、0.001 8 mg/L、0.001 7 mg/L,满足方法学验证的要求。各3批次实际中药注射液样品的测试结果表明,5种元素含量均小于限量值,说明其安全风险较小。方法操作简便、快速、灵敏度高、准确度好,适合5种注射液中的Cu、As、Cd、Pb、Hg等有害元素含量的测定,为其他中药注射液中元素杂质分析方法的建立提供参考。     

ICP-MS法同时测定一次性可降解餐饮具中10种重金属含量

探究了一次性可降解餐饮具中Cr、Co、Ni、Cu、Zn、As、Se、Mo、Cd、Pb等10种重金属含量的电感耦合等离子体质谱法。样品经剪碎后取样,以硝酸+过氧化氢（5∶3）为消解液,微波消解后用水定容,用ICP-MS测定,通过标准曲线对一次性可降解餐饮具中重金属进行定量分析。结果表明：通过优化检测条件,10种重金属元素在线性范围内有着良好的线性关系,相关系数在0.99902～0.99999之间,方法检出限在0.0065～0.1002mg/kg之间,各重金属元素的加标回收率在87.1%～106.3%之间,精密度RSD在1.07%～5.29%之间。该方法准确度高、操作简单、测量快速,可以满足一次性可降解餐饮具中10种重金属同时测定的要求。     

ICP-MS测定罗库溴铵原料药中11种元素杂质含量

建立电感耦合等离子体质谱（ICP-MS）法测定罗库溴铵原料药中汞(Hg)、镉(Cd)、钴(Co)、铅(Pb)、钒(V)、砷(As)、镍(Ni)、铜(Cu)、锂(Li)、锑(Sb)、硼(B) 11个元素杂质含量,并对所建立的方法进行方法学验证。验证结果表明,11个元素标准曲线的相关系数均大于0.999;加样回收率在92.6%～108.2%之间;重复性试验RSD为2.0%～6.4%(n=6);进样精密度试验RSD为1.9%～6.3%;5 h内测定结果的RSD为2.2%～7.7%,均满足《中华人民共和国药典》（2020年版）9101分析方法验证指导原则要求。样品中各元素杂质含量远小于其限度值。     

用带八极杆碰撞／反应池的ICP-MS同时测定电镀废水中的12种重金属元素

为准确而简便地测定电镀废水中各重金属元素的含量,利用带八极杆碰撞／反应池（ORS）和屏蔽炬技术的电感耦合等离子体质谱（ICP．MS）,通过向碰撞池中引入氦气或氢气,消除高盐基体可能带来的多原子离子干扰,同时测定了电镀废水中的V,Cr,Mn,Co,Ni,Cu,Zn,As,Ag,Cd,Sb,Pb12种重金属元素。结果表明：各元素的检出限为1．81～57．13ng／L,加标回收率在91．53％～108．00％,相对标准偏差RSD不高于3．25％。本法简便,灵敏和精度高,能一次性准确地测出电镀废水中多种重金属元素含量。     

微波消解-电感耦合等离子体质谱(ICP-MS) 同时测定塑料包装材料中有毒有害元素

采用硝酸-过氧化氢消解体系,及高压密闭微波技术处理塑料包装材料,建立了电感耦合等离子体质谱法同时测定塑料包装材料中铅、镉、砷、铬、锑、汞、硒、钡、镍、锡、锶、铊多种有毒有害元素的方法。方法的检出限为0.02~0.20μg/L,相对标准偏差(RSD)小于10%,加标回收率为88.0%~117.0%。该方法简单、快速、灵敏、准确度好。     

电感耦合等离子体质谱法同时测定土壤中46个元素的研究

应用电感耦合等离子体质谱（简称ICP—MS）技术,HF—HNO3-HCIO4三酸溶样同时测定土壤中46个元素。考察了测定中的各种干扰和影响因素,选择Rh作内标元素补偿基体效应和灵敏度漂移。方法的检出限0．001～1．13μg·g^-1．RSD为0．01～4．95％,标准加入回收率80．4～119．5％。     

顶空-气相色谱法测定卷烟主流烟气粒相物中吡啶

为研究气相色谱测定卷烟主流烟气粒相物中吡啶含量,采用碳酸钠水溶液作基质校正剂,通过顶空进样、DB-WAXETR色谱柱分离、火焰离子化检测器检测。结果表明:吡啶在0.20~16.20μg/mL质量浓度范围内线性拟合度为0.9998,加标回收率在98.4%~104.7%之间,定量限为0.08μg/支,RSD小于5%,该方法可以快速、准确地测定卷烟主流烟气粒相物中吡啶。     

电感耦合等离子体质谱法测定土壤中痕量铊

在使用王水-HClO4-HF消解法对土壤进行消解后,采用ICP-MS法测定土壤中痕量的铊。对王水-HClO4-HF消解法中王水冷浸时间、HClO4和HF的用量进行优化,发现在土壤取样量为0.500 0 g,王水冷浸时间为4 h,HF用量为4 m L,并且在保证测定值准确的情况下不需要加入HClO4,是测量土壤中痕量的铊的最佳条件。通过一系列的实验建立一种更加准确,经济,灵敏检测土壤中痕量铊的ICP-MS方法。     

Fluorescent approach to quantitation of reactive oxygen species in mainstream cigarette smoke

A novel approach to monitoring of mainstream smoke reactive oxygen species (ROS) has been developed and applied to the quantitation of smoke oxidants. Redox-active fluorescent probe dihydrorhodamine 6G (DHR-6G) was selected as the molecular probe because it is sensitive to typical smoke ROS. The experimental system couples an automatic cigarette smoke machine fiber-optic fluorometer for real-time monitoring of the reaction progress between cigarette smoke and DHR-6G. Quantitation was achieved based on the amount of rhodamine 6G, which is the sole product from DHR-6G oxidation. With the optimization of the trapping efficiency, we detected 391 nmol of ROS/cigarette in the mainstream CS for a standard cigarette 2R4F under standard Federal Trade Commission smoking protocol. Applying this method, we quantified the ROS of selected cigarettes and found that the cigarettes made of burley tobacco have much ( approximately 10 times) higher ROS content in the smoke than that in the tobacco made of bright tobacco. The smokeless cigarette, Eclipse, has comparable ROS with cigarettes made of bright tobacco.     

Analysis of mainstream and sidestream cigarette smoke particulate matter by laser desorption mass spectrometry

Laser desorption ionization Fourier transform ion cyclotron resonance mass spectrometry (LDI-FTICRMS) was used to investigate particulate matter (PM) associated with mainstream (MSS) and sidestream cigarette smokes (SSS). The high mass resolution and the high mass measurement accuracy allowed a molecular formula for each detected signal in the 150-500 m/z range to be assigned. The high number of peaks observed in mass spectra required additional data processing to extract information. In this context, Kendrick maps and Van Krevelen diagrams were drawn. These postacquisition treatments were used to more easily compare different cigarette smokes: (i) MSS from different cigarettes and (ii) MSS and SSS from the same cigarette. In both ion detection modes, most of the detected species were found to be attributed to C(6-31)H(2-35)N(0-7)O(0-9) compounds. The compounds observed in the study of SSS appeared to be more unsaturated and less oxygenated than those observed when MSS of the same cigarette was investigated.     

ICP-MS测定土壤和水系沉积物中的微量银

样品经三酸(HF+HNO3+H2SO4)完全分解后采用ICP-MS测定银时,锆会产生强烈干扰。为消除这种干扰,提高结果准确度,建立离线干扰校正方法。通过测试4件水系沉积物及9件土壤国家标准物质,选择最适测定条件:溶液酸度为1.0%,内标为10 ng/m L Rh、In,采用94Zn消除锆对107Ag干扰。实测结果表明该方法检出限为5.8 ng/g,精密度为5.80%,测试值与推荐值吻合,误差在标准物质允许范围内。该方法具有简便、快捷、准确的优点,还能实现多元素同时测定。     

The detection of nitro pesticides in mainstream and sidestream cigarette smoke using electron monochromator-mass spectrometry

Over the past decade, electron monochromator-mass spectrometry (EM-MS) has been shown to be a selective and sensitive technique for the analysis of a wide variety of electrophilic compounds in complex matrixes. Here, for the first time, three different dinitroaniline pesticides, flumetralin, pendimethalin, and trifluralin, have been shown to be present in both mainstream and sidestream tobacco smoke using an EM-MS system. A number of cigarettes were tested that included three pure-tobacco-type cigarettes, an experimental reference cigarette, and 11 commercial cigarettes. Due to the complexity of the smoke particulate matter, the pesticides were identified only after each sample was subjected to a multistep cleanup process that included phenyl solid-phase extraction; an acid wash; aminopropyl solid-phase extraction; and finally, normal phase LC fractionation. All cigarette types tested showed the presence of the three pesticides in the tobacco smoke, with flumetralin ranging from trace levels up to 37 (+/- 9) ng/cig, pendimethalin ranging from trace levels up to 10.4 (+/- 0.6) ng/cig, and trifluralin ranging from trace levels up to 47 (+/- 17) ng/cig. Acute toxicity information is presented for the three pesticides.     

Determination of trace elements in BGO by neutron activation analysis

We report on the determination of trace elements in a set of Bi₄Ge₃O₁₂ (BGO) crystals by neutron activation analysis. By using doped polycrystalline BGO powders as calibration standards, we have measured the concentrations of Al, Mn, Cu, Co, Cr and Fe in the crystals with a sensitivity of 0.5–500 ppb, and we have determined the segregation coefficients. We have also studied the correlation between the trace elements and the “radiation damage” (color center formation) effect.     

Quantitative method for the analysis of tobacco-specific nitrosamines in cigarette tobacco and mainstream cigarette smoke by use of isotope dilution liquid chromatography tandem mass spectrometry

An improved liquid chromatography tandem mass spectrometry (LC-MS/MS) method has been developed for the determination of tobacco specific nitrosamines (TSNA). It utilizes four stable isotope-labeled internal standards instead of two as reported by others. A separate internal standard for each analyte is required to minimize sample matrix effects on each analyte, which can lead to poor analyte recoveries and decreases in method accuracy and precision if only one or two of the internal standards are used, especially for complex sample matrixes and when no sample cleanup steps are performed as in this study. In addition, two ion-transition pairs (instead of one) are used for each analyte for the confirmation and quantification, further enhancing the method's accuracy and robustness. These improvements have led to a new LC-MS/MS method that is faster, more sensitive, and selective than the traditional methods and more accurate and robust than the published LC-MS/MS methods. The linear range of the method was from 0.2 to 250 ng/mL with a limit of detection of each TSNA varied from 0.027 to 0.049 ng/mL. Good correlations between the results obtained by the new method and the traditional method were observed for the samples studied.