微波消解ICP-MS法测定市售薏苡仁中5种重金属有害元素的含量

目的基于微波消解ICP-MS法对国内市售薏苡仁药材中5种重金属元素含量的测定,建立控制薏苡仁药材重金属的限量检测方法。方法通过微波消解进行样品处理电感耦合等离子质谱法,测定60批市售薏苡仁药材中As、Cd、Cu、Hg、Pb的含量。结果薏苡仁中重金属平均含有量As为0.0139 mg/kg、Cd为0.0038 mg/kg、Cu为4.0909 mg/kg、Hg为0.0015 mg/kg、Pb为0.1019 mg/kg、总量为4.2119 mg/kg。市售薏苡仁药材中Cu和Pb的含有量差别最大,且Cu的含有量最高,As、Cd、Hg的含有量差别不大,且含量普遍较低;国内市售的60批薏苡仁药材中5种重金属元素和重金属总量均符合现行标准。结论国内市售薏苡仁药材中重金属含量普遍合格;微波消解ICP-MS法测定方法简便、快速、准确,可用于中药材中这5种重金属元素的含量测定。     

Evaluation of microwave-assisted ultraviolet digestion method for rice and wheat for subsequent spectrometric determination of As,Cd, Hg and Pb

The aim of this study was to optimize a sample preparation method for rice and wheat using microwave-assisted ultraviolet digestion (MW-UV) for subsequent determination of toxic elements. Cadmium and Pb were determined by sector-field inductively coupled plasma mass spectrometry (SF-ICP-MS), while As and Hg were determined by chemical vapor generation coupled to atomic absorption spectrometry (CVG-AAS). A systematic evaluation of the microwave heating program, nitric acid concentrationand sample mass was performed to optimize the MW-UV digestion method for rice and wheat samples. The relationship between nitric acid concentration and sample mass was monitored by determination of the residual carbon content (RCC) and residual acidity (RA) in order to obtain a high efficiency of digestion. The MW-UV method was successful at digesting up to 1100 mg of rice and wheat using 4 mol L⁻¹ HNO₃ with RCC and RA lower than 1.5 %, and 10 %, respectively. Recovery results ranging from 88 % to 117 % and agreement with certified reference values (t-test, 95 % confidence level) were obtained after digestion using the MW-UV method for spiked samples and certified reference materials (peach leaves-NIST 1547 and tomato leaves-NIST 1573), respectively. The optimized method was suitable for analysis of toxic elements in rice and wheat in compliance with the maximum levels reported in official directives.     

ICP-MS法测定酒石酸长春瑞滨中有害元素及催化剂银残留

目的：建立电感耦合等离子体质谱法测定酒石酸长春瑞滨中有害元素及催化剂银残留的方法。方法：用微波消解处理样品,电感耦合等离子体质谱内标法测定银、钒、铬、钴、镍、铜、砷、钼、镉、锡、锑、钡、铅、汞的含量。结果：上述14种元素的方法检出限分别为0.003、0.020、0.141、0.069、0.077、0.362、0.031、0.057、0.022、0.078、0.017、0.724、0.095、0.005 ng·mL^-1,线性关系良好（r≥0.9988）,回收率为86%~110%,RSD小于15%;同时,给出了此方法各元素的不确定度评定程序。结论：本方法采用在线加内标,可有效校正仪器漂移,抑制基体干扰,提高准确率,多元素测定便捷、准确、灵敏、可靠,可用于酒石酸长春瑞滨中有害元素及催化剂银残留的测定。     

电感耦合等离子体-质谱法测定注射用益气复脉(冻干)中的硫元素

目的 采用电感耦合等离子体-质谱（ICP-MS）法建立注射用益气复脉（冻干）中硫元素的含量测定方法。方法 以微波消解法处理样品,硝酸为消解试剂,样品经微波消解后,以锗（Ge）元素为内标元素,采用ICP-MS法测定药液中硫元素的量。结果 硫元素质量浓度在1～15 μg/mL内线性关系良好（r=0.999 0）;准确度试验（n=6）平均回收率为95.4%,RSD值为5.9%;结论 该方法简便、快速、准确,可用于测定注射用益气复脉（冻干）中硫元素的含量,为其质量控制、安全性评价提供一定参考。     

Effects of surface finishing conditions on the biocompatibility of a nickel-chromium dental casting alloy

Objectives

To assess the effects of surface finishing condition (polished or alumina particle air abraded) on the biocompatibility of direct and indirect exposure to a nickel-chromium (Ni-Cr) d.Sign^®10 dental casting alloy on oral keratinocytes. Biocompatibility was performed by assessing cellular viability and morphology, metabolic activity, cellular toxicity and presence of inflammatory cytokine markers.

Methods

Discs of d.Sign^®10 were cast, alumina particle air abraded and half were polished before surface roughness was determined by profilometry. Biocompatibility was assessed by placing the discs directly or indirectly (with immersion solutions) into contact with TR146 monolayers. Metal ion release was determined by ICP-MS. Cell viability was assessed by trypan blue dye exclusion, metabolic activity by XTT and cellular toxicity by LDH. Inflammatory cytokine analysis was performed using sandwich ELISAs.

Results

The mean polished Ra value was significantly reduced (P < 0.001) compared with the alumina particle air abraded discs but metal ion release was significantly increased for the polished discs. Significant reductions in cell density of polished compared with alumina particle air abraded discs was observed following direct or indirect exposure. A significant reduction in metabolic activity, increase in cellular toxicity and an increase in the presence of inflammatory cytokine markers was highlighted for the polished relative to the alumina particle air abraded discs at 24 h.

Significance

Finishing condition of the Ni-Cr dental alloy investigated has important clinical implications. The approach of employing cell density and morphology, metabolic activity, cellular toxicity levels and inflammatory marker responses to TR146 epithelial cells combined with ICP-MS afforded the authors an increased insight into the complex processes dental alloys undergo in the oral environment.     

ICP-MS分析不同产地黄连中39种无机元素

目的:建立黄连中39种无机元素的含量分析方法,为黄连后续的相关研究提供参考。方法:采用微波高压消解法对样品进行消解,采用电感耦合等离子体质谱法(ICP-MS)对样品中39种无机元素的含量进行检测,并对检测方法进行方法学考察。结果:分析方法符合测定要求,67批次样品中K、Mg、Mn、Zn、Fe 5种元素的平均含量最高,稀土元素的含量则普遍较低。各产地黄连在遗传距离为10时,表现出了较好的产地聚集性特征。结论:该方法操作简便、快速、准确,结果可靠,适用于黄连中无机元素的含量分析。     

50批市售中药材中汞含量考察及结果分析

目的:考察不同品种、不同批次的常见市售中药材中汞(Hg)含量,为中药材中汞的限量控制及市场监管提供有力依据。方法:采用微波消解法消解样品,以铋(Bi)元素为内标,用电感耦合等离子体质谱法测定不同批次的11种中药材(人参、白芍、甘草、枸杞子、海藻、黄芪、金银花、山楂、水蛭、西洋参、昆布)中Hg元素的含量,并采用SPSS软件进行聚类分析。结果:汞元素线性关系良好,相关系数r≥0.999 0,汞元素的检出限为0.006μg/L,平均回收率为100.9%,RSD为1.9%,重复性和精密度的RSD分别为1.06%和2.48%,均≤5%;有12批中药材汞含量超标,Hg含量受中药材自身特性及产地影响较大,系统聚类分析结果表明有11批次的中药材Hg含量差异较大。结论:该方法适用于大批量市售中药材中汞元素的含量考察及结果分析。     

Trace element concentrations in breast cancer patients

Alterations in the circulating levels of trace elements have been observed in breast cancer (BC) patients. However, the relationships between these alterations and the metabolic and clinical consequences of BC are unknown. The treatment-of-choice of BC is surgery followed by radiation therapy (RT). The present study was aimed at investigating: 1) the concentrations of several trace elements in BC patients, and their relationships with the intrinsic molecular subtypes of tumors; 2) the toxicological effect of RT. We studied 49 women with BC who were scheduled to receive RT following excision of the tumor. Plasma samples were obtained before and after the irradiation procedure. The control group was composed of 49 healthy women. Patients had significantly lower pre-RT concentrations of B, Cu, and Zn, and significantly higher concentrations of Sr than the control group. Irradiation was associated with a striking increase in plasma B concentrations, while Cu, Fe, Sr and Zn concentrations were not significantly different from pre-RT levels, albeit Sr and Zn showed non-significant trends towards increases. The plasma concentrations of B, Cu, Fe, Sr, and Zn were associated with the tumor expression of hormone receptors, epidermal growth factor receptor 2, Ki67 antigen, as well as dermatitis and asthenia, all of which represent the main toxicological responses to RT.     

七制香附丸中无机元素的分析及健康风险评估

目的:建立电感耦合等离子体质谱(inductive coupled plasma mass spectrometer, ICP-MS)测定七制香附丸中23种无机元素含量的方法,并对分析结果进行化学计量学分析,为七制香附丸中无机元素的评价提供参考。方法:30批样品经微波消解后,采用ICP-MS测定23种无机元素的含量并建立无机元素指纹图谱,进行聚类分析、主成分分析和健康风险评估。结果:23种无机元素线性关系良好(r≥0.998 3);精密度和重复性试验的RSD值均小于5%;加样回收率在81.91%～109.4%,RSD值小于13%;对30批七制香附丸和23种无机元素进行层级聚类,30批七制香附丸分为3类,23种无机元素分为2类;主成分分析中Mg、Ca、Cr、Fe、Ni、Zn、As、Se、Cd、Tl元素经旋转后均大于0.8;健康风险评估结果显示Cu、As、Cd、Pb元素的危害指数(HI)分别为0.004 9,0.046 7,0.047 7,0.276 5,HI均小于1。结论:所建立的ICP-MS方法准确、灵敏、快速,可用于七制香附丸中23种无机元素的含量测定,30批次七制香附丸中Cu、As...     

ICP-MS法测定不同产地红参中9种无机元素

目的 考察不同产地红参中铁（Fe）、锰（Mn）、锌（Zn）、铜（Cu）、硒（Se）、铅（Pb）、砷（As）、汞（Hg）和镉（Cd）9种无机元素的含量差异。方法 采用微波消解技术及电感耦合等离子体质谱（ICP-MS）法测定28批不同产地红参中9种无机元素含量,并采用SPSS 22.0软件进行聚类分析。结果 不同产地红参Fe、Mn、Zn含量均较高,Se含量极低,有害元素Pb、As、Hg、Cd、Cu含量均符合《中国药典》限量标准。28批样品聚类为两类。结论 不同产地红参均富含Fe、Mn、Zn,其重金属及有害元素污染程度小,安全性相对较好。不同产地红参Fe、Zn、Cu、Se、As元素含量差异性均较小,Mn、Pb、Hg、Cd元素差异性较大。