Beryllium solubility in occupational airborne particles: Sequential extraction procedure and workplace application

Modification of an existing sequential extraction procedure for inorganic beryllium species in the particulate matter of emissions and in working areas is described. The speciation protocol was adapted to carry out beryllium extraction in closed-face cassette sampler to take wall deposits into account. This four-step sequential extraction procedure aims to separate beryllium salts, metal, and oxides from airborne particles for individual quantification. Characterization of the beryllium species according to their solubility in air samples may provide information relative to toxicity, which is potentially related to the different beryllium chemical forms. Beryllium salts (BeF₂, BeSO₄), metallic beryllium (Be_met), and beryllium oxide (BeO) were first individually tested, and then tested in mixtures. Cassettes were spiked with these species and recovery rates were calculated. Quantitative analyses with matched matrix were performed using inductively coupled plasma mass spectrometry (ICP-MS). Method Detection Limits (MDLs) were calculated for the four matrices used in the different extraction steps. In all cases, the MDL was below 4.2 ng/sample. This method is appropriate for assessing occupational exposure to beryllium as the lowest recommended threshold limit values are 0.01 µg.m^?3 in France^[1 Agence nationale de sécurité sanitaire de l'alimentation, de l'environnement et du travail (ANSES): Avis de l'Agence nationale de sécurité sanitaire de l'alimentation, de l'environnement et du travail relative à la proposition de valeurs limites d'exposition à des agents chimiques en milieu professionnel: Le béryllium et ses composés. [Notice from the French National Agency for Food Safety, Environment and Labour on the proposed exposure limits to chemical agents in the workplace: beryllium and its compounds]. Paris: ANSES, 2010. [Google Scholar]^] and 0.05 µg.m^?3 in the USA.^{[2 ACGIH: 2010 Threshold Limit Values (TLVs®) and Biological Exposures Indices (BEIs®) – Beryllium and Compounds. Cincinnati, OH: ACGIH, 2010. [Google Scholar]]}

The protocol was then tested on samples from French factories where occupational beryllium exposure was suspected. Beryllium solubility was variable between factories and among the same workplace between different tasks.     

抗栓胶囊中9种重金属有害元素的含量测定及风险评估

目的：测定抗栓胶囊中重金属有害元素的含量,对有害元素进行潜在的健康风险评估。方法：微波消解对样品进行前处理后,使用电感耦合等离子体质谱仪（ICP-MS）测定钒（V）、铬（Cr）、钴（Co）、镍（Ni）、铜（Cu）、砷（As）、镉（Cd）、汞（Hg）、铅（Pb）9种元素的含量。采用元素指纹图谱和热图对测定结果进行直观分析;使用风险评估模型评估9种有害元素的健康风险。结果：9种元素线性关系良好,r≥0.9990;回收率为78.81%～104.52%,平均回收率为80.87%~102.83%,RSD为0.72%~3.30%（n=6）。测定了9种重金属有害元素的含量,绘制的元素指纹图谱具有一定的特征性,热图表明,样品间Pb、Cr、Hg、As 4种元素的含量差异明显,Pb、As残留量较高,可能存有一定的潜在健康风险。结论：通过探究抗栓胶囊中的重金属有害元素,为该药的质量控制和安全性评价提供参考。     

ICP-MS同时分析中药材中7种微量元素的方法研究

 目的建立用电感耦合等离子体质谱(ICP-MS)同时分析中药材中铜(Cu)、砷(As)、镉(Cd)、汞(Hg)、铅(Pb)、硒(Se)、锗(Ge)7种元素的方法。方法样品经微波消解后,以钪(⁴⁵Sc)、钇(⁸⁹Y)、铟(¹¹⁵In)、铋(²⁰⁹Bi)作为内标物质,直接用ICP-MS分析上述7种元素,并通过标准曲线计算含量。结果7种元素标准曲线的线性关系良好,相关系数(r)在0.999 3～0.999 9之间;检出限0.019～0.107μg·L^-1;加样回收率88.92%～115.0%;5次平行实验的分析结果在3 d内稳定性良好,且所有元素的相对标准偏差(RSD)均小于10%;除砷(As)略低外,标准物质茶叶(GBW 07605)中其他元素的测定值都在标准值范围内。结论该方法是一个灵敏、可靠、稳定的中药材多元素分析方法。     

Trace Element Composition of Municipal Waters in the United States: A Comparison of ICP-AES and ICP-MS Methods

A collaborative project was outlined by representatives of the Nutrient Data Laboratory and the Food Composition Laboratory of the United States Department of Agriculture. The purpose of the project was to obtain trace element (Ca, Cu, Fe, Mg, P, K, Na, Mn, Zn, Co, Cr, Ni and V) composition data for municipal waters sampled around the United States during three different seasons. Several sub-goals were outlined: (1) Compare inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS) methods for the direct determination of nutritionally important elements in water; (2) Compare data from this study with a national, probability-based sampling plan, to existing published data in U.S. Department of Agriculture's Standard Reference Database SR-13; (3) Consider the variability of values comparing different locations; (4) Evaluate seasonal variability; (5) Conclude as to whether or not this high consumption product is a reasonable source of trace elements in the human diet. Results from the study indicated that the excellent detection capability of ICP-MS provided Cr, Ni and V results at the ppb level and also provided P and K data, all of which will be significant positive additions to USDA's Standard Reference Database SR-13. Correlation studies comparing ICP-MS and ICP-AES data showed excellent agreement (Ca, Cu, Mg, Na R=0.99+; K R=0.96). No real significant seasonal variability was identified during the course of the study. This study highlighted the fact that water is not a significant source of most trace elements in the U.S. diet.     

ICP-MS同时测定骨折挫伤胶囊中重金属的含量

目的 建立测定骨折挫伤胶囊中铅（Pb）、镉（Cd）、铜(Cu)、砷（As）、汞(Hg)元素含量的电感耦合等离子体-质谱（ICP-MS）法。方法 样品经人工胃液提取,以锗（Ge）、铟（In）、铋（Bi）为内标,采用ICP-MS法同时测定5种元素。结果 5种元素质量浓度在线性范围内与响应强度线性关系良好,平均回收率97.4%～102.7%,RSD均小于3.5%（n=6）。结论 该方法准确,灵敏,无干扰,可用于骨折挫伤胶囊中5种重金属及有害元素的测定。     

Identification of an exposure risk to heavy metals from pharmaceutical-grade rubber stoppers

Exposure to low concentrations of heavy metals and metalloids represents a well-documented risk to animal and human health. However, current standards (European Pharmacopeia [EP], United States Pharmacopoeia [USP], International Organization for Standardization [ISO], YBB concerned with rubber closures) only require testing for Zn in pharmaceutical-grade rubber stoppers and then using only pure water as a solvent. We extracted and quantified heavy metals and trace elements from pharmaceutical-grade rubber stoppers under conditions that might occur during the preparation of drugs. Pure water, saline, 10% glucose, 3% acetic acid (w/v), 0.1 mol/L hydrochloric acid, and diethylenetriaminepentaacetic acid (4 mg/mL, 0.4 mg/mL, and 0.04 mg/mL) were used as extraction agents. We quantified the extracted arsenic, lead, antimony, iron, magnesium, aluminum, and zinc using inductively coupled plasma mass spectrometry. The concentration of extracted metals varied depending on the different extraction solutions used and between the different rubber stopper manufacturers. Rubber stoppers are ubiquitously used in the pharmaceutical industry for the storage and preparation of drugs. Extraction of heavy metals during the manufacturing and preparation of drugs represents a significant risk, suggesting a need for industry standards to focus on heavy metal migration from rubber stoppers.     

ICP-MS测定片仔癀肝宝中6种重金属的含量

目的：建立电感耦合等离子体质谱法（ICP-MS）测定片仔癀肝宝中铬（Cr）、铅（Pb）、镉（Cd）、砷（As）、汞（Hg）、铜（Cu）6种重金属的含量。方法：样品微波消解处理后,采用电感耦合等离子体质谱法测定。结果：Cr、Cu、As、Cd、Hg、Pb标液的工作曲线线性良好,相关系数大于0.999 3。其中Cr的平均回收率101.2%,相对标准偏差（RSD）7.6%;Cu的平均回收率96.4%,RSD3.5%;As的平均回收率101.3%,RSD1.8%;Cd的平均回收率100.2%,RSD0.3%;Hg的平均回收率100.5%,RSD4.2%;Pb的平均回收率104.2%,RSD5.6%。结论：该方法稳定可靠,灵敏度高,重现性好,可用于测定片仔癀肝宝中Cr、Cu、As、Cd、Hg、Pb 6种重金属的含量。     

稀土放射性分析的比对研究

目的 总结多年来放射性分析的经验,解决当前稀土放射性分析遇到的一些实际问题。方法 通过不同测量方法的比对,以及实验室之间样品传递分析,进行比对研究。结果 证实标准参考物质的正确选择,是分析准确与否的重要保证;γ能谱分析是稀土放射性分析的重要手段,但对于非放射性平衡的样品,必须配合其它分析手段,才能获取样品的更多信息。结论 对于一些复杂、未知样品,时常开展实验室之间的比对分析,不断提高分析检测水平,充分发挥国家开放实验室的平台效应,是很有必要的。     

微波样ICP—MS测定海产品中元素方法研究

本文利用微波消解电感藕合等离子体质谱法（ICP－MS）测定了海产品中Na、Mg、Al、P、Cr、Mn、Fe、Ni、Ca、Zn、As、Sr、Mo、Cd、Pb、Hg,并利用国家标准物质贻贝GBW08571验证了方法的准确度、准确度在85％－115％,平均值为96．7％,测定值与标准值吻合,相对标准偏差均小于5％,并用多内标法有效地校正了基体干扰,方法简便、快速、准确、可靠。     

男宝胶囊中重金属及有害元素的残留量测定及风险评估

目的：研究男宝胶囊中重金属及有害元素的残留情况并进行风险评估。方法：采用微波消解-电感耦合等离子体质谱法,测定10个生产单位的80批样品中铅、镉、砷、汞、铜、钒、铬、钴、镍9种元素的残留量,并采用热图及多变异源图对测定结果进行差异性比较,同时对其进行健康风险评估。结果：9种元素线性关系良好,相关系数r≥0.999 9,平均回收率在76.64%～102.49%,RSD为1.09%～6.92%(n=6)。80批次男宝胶囊样品中铅、镉、砷、汞、铜、钒、铬、钴、镍的残留量分别为0.384～2.887、0.060～0.289、0.213～13.904、0.002～35.412、2.250～10.382、0.302～1.676、0.348～5.388、0.187～0.878、1.608～4.962 mg·kg-1。铬、砷、铅和汞4种元素的残留量存在一定的差异性,其中汞最为显著,分析差异主要是由生产单位原材料质量控制不稳定导致的;风险评估结果表明,有1批次样品的汞残留量高于最大限量理论值和香港中成药注册安全性技术指引中相关规定值,提示此批次样品存在一定的健康风险。结论：本研究可为男宝胶囊重金属及有害...