ICP-AES analysis of metal content in shell of mussel Mytilus galloprovincialis from Croatian coastal waters

Metal content in samples of shell of mussel Mytilus galoprovincialis was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The efficiency of conversion of crude samples into solution by acid digestion in an open plate and in a microwave oven was examined by use of certified reference material of marine sediment and laboratory made standards of calcite and aragonite. Influence of high Ca content matrix on emission intensities of Al, Ba, Cd, Cu, Fe, Mg, Mn, Na, Ni, Pb, Sr and Zn was observed as depression of emission signal for most of the measuring elements, ranging from 0.8% to 8%. Greater values were noted at Ba and Ni emission lines. Enhancement of signals was observed for Na and Mg lines. The determination of As, Sb, Se and Sn was performed by HG/ICP-AES. The greater abundance of Sn was found in samples collected near the Al-processing industry centre. No detectable concentrations of As, Sb, and Se were found in shell samples. Results of ICP-AES metal analysis showed that samples collected near harbours, city waste or sewage outlets, and chemical industry centres indicate the certain level of contamination. It is shown that shell analysis provides useful data in determination of marine environment status.     

电感耦合等离子体质谱法测定香薷中无机元素含量的研究

采用电感耦合等离子体质谱（ICP—MS）法对香薷中的Ca、Mg、Cu、Zn、Fe、Mn、Co、Ni、Se等18种无机元素进行了分析测定。该方法的回收率在84．62％～113．16％,具有良好的准确度和精密度,完全可以满足香薷样品中无机元素测定要求。研究结果表明：香薷中Ca和Mg两种必须的常量元素的含量特别高,微量元素Cu、Zn、Fe、Mn、Co、Ni、Se含量丰富。此结果可为探讨香薷中元素含量与其药效相关性提供科学依据。     

ICP-MS法测定心可舒片中的微量元素

为建立准确快速测定心可舒片中微量元素含量的方法,对该药生产进行质量控制,并为合理用药提供依据,采用电感耦合等离子体质谱法(ICP-MS),对心可舒片中的21种元素进行了分析。结果表明,心可舒片对心血管病的疗效与其中的微量元素有关。     

ICP-MS法测定栽培甘草中的十种微量元素

采用电感耦合等离子体质谱仪(ICP-MS)测定了栽培甘草中的十种微量元素。结果表明,方法中各元素标准曲线的r2值均在0.99以上,回收率为91.21%~108.65%,RSD值为3.6%~8.9%。该法精密度高、准确性好、干扰较少、快速简单,可用于甘草中微量元素的含量测定。     

电感耦合等离子体质谱(ICP-MS)法测定农产品样品中6种痕量元素

建立了电感耦合等离子体质谱(ICP-MS)法测定果蔬类、大米等农产品样品中痕量元素的方法.样品通过HNO3-H2 O2混酸体系微波消解,以Rh作为内标溶液消除基体干扰,在仪器最佳条件下测定植物样中镉、铅、铬、铜、镍、锌6种痕量元素.方法的检出限为0.002～0.5μg/g;相对标准偏差(RSD)为0.84％ ～7.4％...     

On the Traceability of the Hazelnut Production Chain by Means of Trace Elements

The production chain of hazelnuts has been studied by analyzing three sets of samples produced in purity from three different pools of hazelnuts of cultivar “Tonda Gentile Trilobata”, “Tonda Gentile Romana” and “Mortarella”, all cultivated in Italy. From each pool, five processed products were obtained: roasted hazelnuts, hazelnut paste, hazelnut cream, Gianduja paste and Gianduiotto paste. After pre-treatment by means of dry ashing, all samples from each cultivar, including raw hazelnuts, were then analyzed by means of Inductively Coupled Plasma–Optical Emission Spectroscopy (ICP-OES) and Inductively Coupled Plasma–Mass Spectrometry (ICP-MS). A good discrimination was obtained among the different chain stages according to the distribution of the trace elements, as expected. More interesting was the discrimination among the different cultivars: it was possible to distinguish the samples produced from the respective cultivar by means of specific chemical markers, particularly Mo and Ni.     

Seasonal variations in the profile of main phospholipids in Mytilus galloprovincialis mussels: A study by hydrophilic interaction liquid chromatography–electrospray ionization Fourier transform mass spectrometry

A systematic characterization of phosphatidylcholines and phosphatidylethanolamines in mussels of sp Mytilus galloprovincialis was performed by high‐efficiency hydrophilic interaction liquid chromatography combined with electrospray ionization and Fourier transform mass spectrometry (FTMS), based on a quadrupole‐Orbitrap hybrid spectrometer. The FTMS/MS experiments under high collisional energy dissociation conditions, complemented by low‐energy collisionally induced dissociation MSⁿ (n  = 2,3) experiments, performed in a linear ion trap mass spectrometer, were exploited for structural elucidation purposes. The described approach led to an unprecedented characterization of the mussel phospholipidome, with 185 phosphatidylcholines and 131 phosphatidylethanolamines species recognized, distributed among diacylic, plasmanylic, and plasmenylic forms. This was the starting point for the evaluation of the effects of season (in particular, of sea temperature) on the profile of those phospholipids. To this aim, a set of mussel samples retrieved from commercial sources in different periods of the year was considered. Principal component analysis revealed a clear separation between samples collected in periods characterized by cold, intermediate, or warm sea temperatures, respectively. In particular, an enrichment in phospholipids containing unsaturated side chains was observed in mussels collected from cold seawaters (winter‐early spring), thus confirming the general model previously elaborated to explain the adaptation of marine invertebrates, including some bivalve molluscs, to low temperatures. On the other hand, relevant levels of plasma(e)nylic and acylic phospholipids bearing either saturated or non‐methylene‐interrupted side chains were found in mussels collected in warm seawaters (typical of summer and early autumn, at Italian latitudes). This finding opened interesting perspectives towards the development of strategies able to prevent global warming–related mussel losses in aquacultural plants.     

ICP-MS Assessment of Essential and Toxic Trace Elements in Foodstuffs with Different Geographic Origins Available in Romanian Supermarkets

The present study was conducted to quantify the daily intake and target hazard quotient of four essential elements, namely, chromium, cobalt, nickel, and copper, and four toxic trace elements, mercury, cadmium, lead, and arsenic. Thirty food items were assigned to five food categories (seeds, leaves, powders, beans, and fruits) and analyzed using inductively coupled plasma-mass spectrometry. Factor analysis after principal component extraction revealed common metal patterns in all foodstuffs, and using hierarchical cluster analysis, an association map was created to illustrate their similarity. The results indicate that the internationally recommended dietary allowance was exceeded for Cu and Cr in 27 and 29 foodstuffs, respectively. According to the tolerable upper level for Ni and Cu, everyday consumption of these elements through repeated consumption of seeds (fennel, opium poppy, and cannabis) and fruits (almond) can have adverse health effects. Moreover, a robust correlation between Cu and As (p < 0.001) was established when all samples were analyzed. Principal component analysis (PCA) demonstrated an association between Pb, As, Co, and Ni in one group and Cr, Cu, Hg, and Cd in a second group, comprising 56.85% of the total variance. For all elements investigated, the cancer risk index was within safe limits, highlighting that lifetime consumption does not increase the risk of carcinogens.     

成年男性精液中19种元素含量的测定及影响因素研究

运用ICP-MS和ICP-AES方法同时分析丹东某硼矿周围工人组及对照组精液中19种元素的含量水平。样品经过双氧水-纯化硝酸体系消解,采用稀释分析及双内标铑(Rh)和铼(Re)进行校正。该法最低检出限、加标回收率及分析精密度能满足精液样品的分析要求。按照95%置信区间进行数据筛选,选出118人的数据统计分析成年男性精液中元素含量水平,并与国内其它研究结果进行比较。分析精液元素含量影响因素表明,硼(B)作业暴露对精液中的B含量具有显著影响;吸烟能显著影响精液中的Cd含量;饮酒对工人组精液中的Cu和Mn的含量具有显著影响。     

Determination of Trace Elements in Super Alloy by ICP-MS

 A method is described for determination of 14 trace elements in super alloy certified reference material. Inconel 718 by ICP-MS. The interferences were investigated in detail. By using appropriate settings of the operational parameters and correcting interferences the elements without interference free isotopes were also analyzed. Non-spectral interference to the analytes was studied. No matrix separation or any other sample pretreatment but acid dissolution was made. 14 trace elements (B, Sc, Ga, Ge, In, Sn, Sb, Te, Hf, Ag, Ce, Tl, Pb and Bi) were analyzed by matrix matched standard solution calibration and using Rh as internal standard. Good agreement was achieved between the found levels and the certified values for most of the elements. The RSD (n = 4) of the determination values of Ce was lower than 20%, and RSD of the other 13 elements was lower than 10%. Received July 21, 2000. Revision May 29, 2001.     

电感耦合等离子体质谱(ICP-MS)法同时测定荞麦秸秆中的8种重金属元素

基于硝酸-盐酸-氢氟酸消解体系,建立了马弗炉-微波消解-电感耦合离子体质谱(ICP-MS)法同时测定荞麦秸秆中的Cr、Cu、Ag、Mn、Fe、As、Ni、Pb等重金属含量测定方法。在微波消解的过程中,分别考察5种不同组合的混合酸体系及两种消解方法对荞麦秸秆中8种重金属测试结果的影响。实验结果表明,浓硝酸-浓盐酸-氢氟酸(6∶2∶2)混酸体系和马弗炉-微波消解样品前处理优于其他方法。在优化条件下,8种重金属加标回收率为91.2%~102%,相对标准偏差(RSD,n=5)为0.22%~4.7%,检出限为0.18~9.41μg/L。方法操作简便、快速、准确,结果可靠,能同时测定荞麦秸秆中8种重金属元素。     

微波消解-ICP/MS测定烤烟中微量元素含量

以3 mL HNO3和2 mL H2O2的混合消解液对烟草样品进行微波消解,采用电感耦合等离子体质谱测定了烤烟中的Mn、Zn、Cu、Se、N i、Co、Cr、As、Cd、Pb 10种微量元素的含量.结果表明：方法的检出限均低于0.02μg/g,各元素测定的RSD（n=5）均小于3%,样品加标回收率为97.35%-101.30%.方法消耗试剂少,快速准确,适合烟草中多种微量元素的同时测定.     

ICP-MS法测定彭泽贝母中微量元素的含量及形态分析

目的:测定彭泽贝母中微量元素含量,研究彭泽贝母中微量元素的存在形态,探讨微量元素的含量和形态.方法:采用HNO3-H2O2微波消解体系,电感耦合等离子质谱法(ICP-MS)测定彭泽贝母中铅、钙、铁、锰、锌、镉、钡、铬等10种微量元素的含量,初步探究微量元素的存在形态.结果:Ca元素在彭泽贝母中含量最高,而Mo元素含量最低;彭泽贝母中微量元素是以无机态为主、多种形态共存的复杂体系.结论:彭泽贝母中含有丰富的人体必需微量元素,可能促进其有效成分作用的发挥.     

Monitoring of Polycyclic Aromatic Hydrocarbon Levels in Mussels (Mytilus galloprovincialis) from Aquaculture Farms in Central Macedonia Region,Greece, Using Gas Chromatography–Tandem Mass Spectrometry Method

A new sensitive and selective gas chromatography tandem mass spectrometry (GC-MS/MS) method was developed for the analysis of 26 polycyclic aromatic hydrocarbons (PAHs), including 16 Environmental Protection Agency (EPA) and 15 + 1 European Union (EU) PAHs, in mussel samples from aquaculture farms in Thermaikos and Strymonian Gulf, Central Macedonia Region, in three sampling periods. Concentrations were found at moderate to low values at all sampling sites, without exceeding maximum levels set by EU. Low molecular weight PAHs were predominant in all samples. Seasonal variation of the concentrations was observed; values were slightly higher in the winter period. Use of diagnostic ratios for potential sources of PAHs showed both petrogenic and pyrolitic origin. In comparison to other related studies of mussels from the Mediterranean Sea, Greek mussels cultivated in the studied gulfs are low in contaminants due to minimal environmental pollution effects. Low concentrations of PAHs are in compliance with the low values of other POPs which were found in the mussels.     

电感耦合等离子体质谱(ICP-MS)法测定生物制药用一次性储液瓶中34种可提取无机元素

为建立同时测定生物制药用一次性储液瓶中34种可提取无机元素含量的方法,采用5种溶剂对样品分别提取1天、21天和70天,利用电感耦合等离子体质谱仪（ICP-MS）检测其中的元素含量,通过比较各检出元素的含量与人每日最大允许暴露量（PDE）进行风险评估。结果表明,该方法下各元素拟合曲线线性良好,相关系数≥0.999,不同提取溶剂中,方法的检出限为0.001-25.772 μg/L,相对标准偏差范围为0.2%-2.3%,低、中、高加标平均回收率在86.0%-115.7%之间。实际样品测定时,不同提取条件下可提取元素的含量在水和碱性溶液中较高,而随提取时间的增加趋势并不显著,各检出元素的含量均远低于其PDE值。该方法检出限低,线性良好,具有较高的准确度和精密度,可以满足生物制药用一次性储液瓶中多种可提取无机元素同时检测的需求。     

缅甸进口姜黄无机元素分析研究

目的：通过测定缅甸进口姜黄中26种无机元素,并对进口姜黄中重金属含量进行风险评价,为缅甸进口姜黄的质量控制奠定基础。方法：采用微波消解ICP-MS法对24批来自缅甸地区的姜黄进行26种无机元素的测定,通过靶标危害系数（THQ）和总危害指数（HI）对Pb、Cd、Cu 3种元素进行非致癌风险评价,用终生致癌风险（R）对As进行致癌风险评价。结果：结果表明,缅甸进口姜黄中含有24种无机元素,其中K、Na、Mg、Ca 4种营养元素含量占比24种无机元素的92.39%。缅甸姜黄中均未检出Sn、Hg 2种金属元素,Pb、Cd、As、Cu 、Hg5种重金属元素含量均符合2020版中国药典限定值。经过缅甸姜黄中Cu、Pb、Cd 3种重金属元素健康风险评价,THQ和HI均小于1,表明人体通过缅甸姜黄摄入的Cu、Pb、Cd不会对人体造成非致癌伤害。经过对姜黄中As的致癌健康风险评价,致癌风险R为7.72 x10-6,低于世界卫生组织建议的致癌风险值（1.00 x 10-5）,通过缅甸姜黄摄入的总As不存在致癌风险。结论：总体而言,缅甸进口姜黄重金属元素保持在较好水平。     

电感耦合等离子体质谱（ICP-MS）法测定沙虫中10种重金属

建立了密闭高压消解-电感耦合等离子体质谱快速测定了沙虫中10种重金属元素(Pb、Tl、Cd、As、Cr、Ni、V、Cu、Sn、Sb)的方法,并分析了重金属的分布特征。试样经粉碎后,以HNO3和H2O2为消解剂进行消解处理,得到的消解液使用电感耦合等离子体质谱仪测定各元素的含量。结果表明,10种重金属元素元素的方法检出限在0.05～3.4μg/kg之间,相对标准偏差（RSD,n=3）小于4%,在0.05-100μg/L线性范围内线性关系良好,相关系数均大于0.999,方法用于国家有证标准物质（GBW10050）的测定,结果与标示值相符。方法灵敏度高,重现性好,定量准确,适用于沙虫样品的检测。     

ICP－MS分析人血清中微量元素

用ＩＣＰ－ＭＳ分析人血清中２２种元素。为克服基体抑制效应。采用内标元素Ｓｃ和Ｉｎ分别校正质量数８０以下和８０以上元素的测定，获得满意的结果。通过对牛血清标准物质的测定，检验分析结果的准确性和方法的可靠性。     

生、炒决明子中无机元素的分析测定

为测定生决明子中无机元素水平,探讨其药效物质基础及炒制对其含量的影响,采用原子荧光法和等离子发射光谱法等测定了不同产地、批次的生、炒决明子中重金属及微量元素的含量。结果表明,不同产地的生、炒决明子含有的重金属元素均没有超过食品卫生标准。决明子经过炮制后,无机元素变化情况:硫、钠、铬、钡、锂、镍、锶等元素炮制前后变化不大;钙、钾、镁、锰、锌有益元素的含量略有增高;汞、铅、砷有害元素的含量略有下降。可见决明子饮片药用是安全的,炒制工艺对决明子无机元素含量有一定影响,其特有无机元素的种类和含量对揭示决明子药效的物质基础具有意义。     

微波消解-ICP-MS法测定药用明胶空心胶囊中微量重金属元素

采用微波消解技术,建立了一种电感耦合等离子体质谱法测定明胶空心胶囊中Cr,Co,Ni,Cu,Zn,As,Cd,Hg和Pb 9种微量重金属元素的方法。确定了微波消解仪和等离子体质谱仪的最佳操作参数,研究共存离子的干扰和消除方法,选择了各元素的测定同位素,以Ge,Rh和Tl为内标补偿基体效应,建立了样品测定方法。应用拟定的方法测定了不同生产厂家、不同批次的空心胶囊中微量重金属的含量。方法对试样中各元素测定的相对标准偏差为1.5%~14.1%,加标回收率在90.0%~102.0%。结果表明,方法简便、快速、灵敏,满足于空心胶囊中9种重金属元素的测定要求。