电感耦合等离子体质谱法同时检测红枣中铅、砷、镉、汞、铜、锌和16种稀土元素

为了研究哈密、若羌和和田红枣中铅、砷、镉、汞、铜、锌和16种稀土元素的含量情况,了解红枣重金属及稀土元素摄入的风险,建立同时检测红枣中铅、砷、汞、铜、锌和16种稀土元素的方法。红枣样品用微波消解法进行样品前处理,以电感耦合等离子体质谱法测定红枣中铅、砷、镉、汞、铜、锌和16种稀土元素的含量。各元素校准曲线的相关系数均大于0.999 0,检出限为0.01~0.05μg/L。加标回收率为92.1%~105.2%,测定结果的相对标准偏差为1.2%~3.6%(n=6)。用该方法测定苹果标准物质(GBW 10019),测定值与标准值一致。该方法适用于红枣类样品中多元素污染物快速检测及风险评估,红枣样品分析结果表明铅、砷、镉、汞、铜和稀土元素在3种红枣中的含量较低,风险监测数据表明红枣中存在重金属铅、镉摄入性风险。     

青海省西宁种植山莨菪中重金属元素特征

青海地道中藏药材山莨菪人工引种栽培试验成功。采集两年生和三年生种植山莨菪在不同生长期的植物全植株,采用流动注射氢化法原子吸收光谱分别测试了其不同组织中铅、砷、汞、镉等重金属元素含量。结果表明,山莨菪在生长周期内吸收的重金属元素并非全部蓄积在根组织器官中,部分重金属元素通过年生长周期内的生长发育而随着地上茎叶部分等组织器官的枯萎被代谢排出植物体外。     

黑苦荞保健茶中重金属的分析评价

采用原子吸收光谱法和原子荧光光度法测定了四川省凉山州某几个品牌黑苦荞保健茶中的重金属铅、镉、铬、无机砷和汞的含量,并以NY/T 1510-2007标准绿色食品麦类制品为依据,对黑苦荞保健茶重金属污染状况进行了分析评价。结果表明,黑苦荞保健茶受重金属元素污染的程度由高到低表现为铅、铬、镉、无机砷和汞,但含量均未超过国家标准规定;黑苦荞叶芽茶和全株茶的重金属污染较为严重,全胚茶未受重金属污染。     

水产品重金属含量快速检测试纸问世

<正>由于自然环境的污染以及水产养殖环境的恶化,水产品中铅、砷、汞、镉等重金属超标的风险大大增加。为了能快速检测出水产品中是否含有重金属及其含量,青岛市药检所历时两年研制了4种快速检测试纸,采用化学显色反应试纸的方法,能检测出铅、砷、汞、镉4种重金属及其含量。先把水产品打成匀浆,再放入试纸,仅需两步,就能查出螃蟹、蛤蜊等水产品中是否含有重金属。据了解,该技术为全国首创,能检出铅、砷、汞、镉4种重金属及其含量。"以往在实验室条件下用仪器进行分析,仪器往往比较     

基于石墨消解法测定海洋沉积物中7种重金属的含量

鉴于目前常用的海洋沉积物中重金属测定的消解方法存在工作效率低、操作复杂、交叉污染、人员危险性高等问题,通过比对和参考现行规范、标准和文献资料中海洋沉积物重金属的不同消解方法,提出了全自动石墨消解海洋沉积物的方法,并以原子荧光光谱法测定汞和砷的含量,以电感耦合等离子体质谱法测定铜、铅、锌、镉、铬的含量。以6 mL盐酸、2 mL硝酸和8 mL水为消解酸,于100℃消解0.2 g样品1.5 h;消解结束后,冷却至室温,用水定容至50 mL,按照原子荧光光度计的工作条件测定汞和砷的含量。以5 mL盐酸、5mL硝酸为消解酸,先于120℃消解0.2 g样品1 h;然后加入2 mL硝酸、5 mL氢氟酸和2 mL高氯酸,于180℃继续消解4 h;消解结束后,冷却至室温,用水定容至50 mL,按照电感耦合等离子体质谱仪的工作条件测定铜、铅、锌、镉、铬的含量。结果表明：汞、砷标准曲线的线性范围分别在1.00μg·L^-1以内和10.0μg·L^-1以内,铜、铅、锌、镉、铬标准曲线的线性范围在100μg·L^-1以内,汞、砷、铜、铅、锌、镉、铬的检...     

原子吸收光谱法测定益寿回春口服液中砷铅镉铬汞的含量

采用原子吸收光谱法测定了益寿回春口服液中砷、铅、镉、铬和汞的含量，并参照食品中重金属的限量规定进行了比较。结果表明，益寿回春口服液中的砷、铅、镉、铬和汞均低于限量标准，为该产品的质量控制提供了依据。     

原子吸收光谱法测定大承气颗粒剂中砷铅镉铬汞的含量

采用原子吸收光谱法测定了大承气颗粒剂及其原料药材中砷、铅、镉、铬和汞的含量，并参照食品中重金属的限量规定进行了比较。结果表明，大承气颗粒剂及其原料药材中的砷、铅、镉、铬和汞均低于限量标准，成品中重金属的含量均低于原料药材中的平均含量，这为大承气颗粒剂生产中的质量控制提供了依据。     

布洛芬注射液包材相容性研究中铅、镉、砷、锑的测定

建立中性硼硅玻璃包材加速试验后布洛芬注射液中铅、镉、砷、锑含量的检测方法。采用微波消解仪以硝酸分解样品,用石墨炉原子吸收光谱仪测定铅、镉含量,测定波长铅为283.3 nm,镉为228.8 nm,铅、镉分别在5.0~50.0,0.5~5.0μg/L范围内有良好的线性,相关系数分别为0.999 7,0.996 2,检出限分别为0.26,0.01μg/L,测定结果的相对标准偏差分别为1.06%,2.40%(n=6),加标回收率分别为100.2%~101.9%,97.1%~105.1%。用原子荧光光谱仪测定砷、锑含量,测定波长砷为193.7 nm,锑为217.6 nm,砷、锑在1~10μg/L范围内均有良好的线性,相关系数分别为0.999 9,0.999 5,检出限分别为0.03,0.01μg/L,测定结果的相对标准偏差分别为1.04%,2.65%(n=6),加标回收率分别为94.2%~96.5%,92.6%~96.5%。该测定方法快速,灵敏度高,适用于内包装材料加速试验后药品中重金属元素含量变化的研究。     

ICP–MS法测定食品接触纸制品中铬、镍、砷、镉、铅、汞

建立电感耦合等离子体质谱法(ICP–MS)测定食品接触纸制品中铬、镍、砷、镉、铅、汞6种重金属含量的方法。样品经微波消解处理后用ICP–MS进行测定,内标法定量。在优化实验条件下,测定汞元素的线性范围在0~10μg/L之间,测定铅、镉、铬、镍、砷元素的线性范围在0~100μg/L之间,相关系数均大于0.999。各元素的检出限为0.001~0.1 mg/kg,加标回收率为89.3%~116.0%,测定结果的相对标准偏差为3.5%~7.9%(n=6)。该方法样品处理简单,检测灵敏度高,适用于食品接触纸制品中铬、镍、砷、镉、铅、汞的检测。     

电感耦合等离子体质谱(ICP-MS)法检测市售鱿鱼中5种重金属

基于硝酸消解体系,建立了微波消解-电感耦合离子体质谱(ICP-MS)法同时测定市售鱿鱼中铅、砷、镉、汞、铬5种重金属元素的检测方法。样品加入HNO₃进行微波消解,优化ICP-MS 相关检测参数后,进行外标法定量。结果表明,5种重金属在各自浓度范围内线性关系均＞0.999,平均回收率为96%-101%,精密度RSD均小于5%。用该法检测广州市农贸市场随机购买的6个批次冰鲜鱿鱼,结果有1个批次砷含量超标,1个批次镉含量超标。该法前处理简单,检测准确、快速,适用于鱿鱼等水产品中铅、砷、镉、汞、铬等重金属的检测。     

Phenolic compounds,antioxidant activity and Cu,Zn, Cd and Pb content in wild and cultivated cranberries and blueberries

The aim of this study was to determine the content of Cu, Zn, Cd and Pb and the total polyphenol (TP) content as well as the total antioxidant capacity (TAC) in wild cranberries and blueberries collected from different localities of the Slovakia and to compare them with properties of six cranberry and six highbush blueberry cultivars obtained from the research centre. Compared with cultivated cranberries (Cu, Zn, Cd and Pb content: 0.642, 1.496, 0.015 and 0.050 mg/kg FM) in wild fruits, higher Cu (by 37%) and lower Zn, Cd and Pb (by 8%, 7% and 44% respectively) were determined using atomic absorption spectrometry method. In wild blueberries, higher Cu, Zn and Pb (by 16%, 209% and 80% respectively) and similar Cd contents were determined compared with cultivated fruits (Cu, Zn, Cd and Pb content: 0.483, 0.541, 0.003 and 0.055 mg/kg FM). The TP contents estimated by spectrophotometry using Folin–Ciocalteau reagent were in intervals 1405–3161 (cranberries) and 1300–3077 (blueberries) expressed as mg GAE/kg FM. While the average TP content determined in wild cranberries was by 31% lower than that in cultivated cranberries, in wild blueberries it was by 97% higher compared with highbush blueberry cultivars. The values of TAC determined by spectrophotometry method using 2,2-diphenyl-1-picrylhydrazyl were in range 20.67–22.22 (cranberries) and 14.03–24.79 (blueberries) expressed as mmol TE/kg FM. In wild cranberries and blueberries, the lower average TAC values compared with cultivated berries were determined (by 1% and 28%, respectively).     

Determination of Hg,As, Pb,and Cd in Orchard Soils by Sequential Injection Vapor Generation Atomic Fluorescence Spectrometry

An analytical procedure was developed for determination of Hg, As, Pb, and Cd in soil samples using sequential injection vapor generation atomic fluorescence spectrometry (SI-VG-AFS) with sample preparation by microwave digestion system. The effects of analytical conditions on the fluorescence intensity were investigated and optimized. Under the optimized condition, the detection limits of the method were 5, 68, 40, and 3 ng L^?1 for Hg, As, Pb, and Cd, respectively. The accuracy of method was verified by the determination of the certified reference soil, and the recoveries for Hg, As, Pb, and Cd were in the range of 98.7–106.1%. The proposed method has been successfully applied to determine the heavy metals in navel orange orchard soils in Ganzhou, and the environmental quality of the orchard soils was assessed based on the content of the heavy metals. According to the second criterion of environmental quality standard for soils, Pb content in all soil samples collected from the orchards of 18 districts were within safe limits, but a few orchards were slightly contaminated with Hg, As, and Cd. Comparison of heavy metal mean concentrations with the safe limits of environmental quality standard for soils, the quality of Ganzhou navel orange orchard soils were in line with the request of the green food production base.     

青藏高原白刺、枸杞和沙棘果粉中微量元素含量比较研究

采用原子吸收光谱法、氢化物原子荧光光谱法对青藏高原白刺、枸杞、沙棘果粉中的13种元素进行了分析测定。结果表明,3种植物果粉中的Cu、Fe、Mn、Zn、K、Ca、Na、Mg等8种元素含量丰富且差异显著,Pb、As、Cr、Cd、Hg等5种重金属元素含量均较低,为3种植物资源深度开发利用提供了基础数据。     

Direct sample introduction of wines in graphite furnace atomic absorption spectrometry for the simultaneous determination of arsenic, cadmium, copper and lead content

A multi-element graphite furnace atomic absorption spectrometry (GFAAS) method was elaborated for the simultaneous determination of As, Cd, Cu, and Pb in wine samples of various sugar contents using the transversally heated graphite atomizer (THGA) with end-capped tubes and integrated graphite platforms (IGPs). For comparative GFAAS analyses, direct injection (i.e., dispensing the sample onto the IGP) and digestion-based (i.e., adding oxidizing agents, such as HNO(3) and/or H(2)O(2) to the sample solutions) methods were optimized with the application of chemical modifiers. The mixture of 5 microg Pd (applied as nitrate) plus 3 microg Mg(NO(3))(2) chemical modifier was proven to be optimal for the present set of analytes and matrix, it allowing the optimal 600 degrees C pyrolysis and 2200 degrees C atomization temperatures, respectively. The IGP of the THGA was pre-heated at 70 degrees C to prevent the sputtering and/or foaming of sample solutions with a high organic content, dispensed together with the modifier solution, which method also improved the reproducibility of the determinations. With the digestion-based method, the recovery ranged between 87 and 122%, while with the direct injection method it was between 96 and 102% for Cd, Cu, and Pb, whereas a lower, compromise recovery of 45-85% was realized for As. The detection limits (LODs) were found to be 5.0, 0.03, 1.2, and 0.8 microg l(-1) for As, Cd, Cu, and Pb, respectively. The characteristic mass (m(0)) data were 24 pg As, 1.3 pg Cd, 13 pg Cu, and 35 pg Pb. The upper limits of the linear calibration range were 100, 2, 100, and 200 microg l(-1) for As, Cd, Cu, and Pb, respectively. The precisions were not worse than 4.8, 3.1, 3.7, and 2.3% for As, Cd, Cu, and Pb, respectively. For arsenic, a higher amount of the modifier (e.g., 20 microg Pd plus 12 microg Mg(NO(3))(2)) could be recommended to overcome the interference from the presence of sulphate and phosphate in wines. Although this method increased the sensitivity for As (m(0)=20 pg), it also enhanced the background noise, thus only a slight improvement in the LOD of As (3.9 microg l(-1)) was realized. For the 35 red and white wine samples studied, the highest metal contents were observed for Cu ranging from 20 to 640 microg l(-1) (average: 148 microg l(-1)), followed by Pb from 6 to 90 microg l(-1) (average: 32.3 microg l(-1)), and Cd from 0.05 to 16.5 microg l(-1) (average: 1.06 microg l(-1)), whereas the As content was below the LOD. This wide fluctuation in the trace metal content could be associated with the origin of wines from various regions (i.e., different trace metal level and/or quality of soil, and/or anthropogenic impact), and with diverse materials (e.g., additives and containers) involved in the wine production processes. The Cu content of wine samples was significantly correlated with Pb, whereas its weak anti-correlation was found with Cd. Interestingly, the level of Pb was anti-correlated with the year of production of the wines. This is likely due to the gradual decrease in the Pb content of soils of vineyards by time, which certainly causes less Pb-uptake of the grape plant, thus a decrease in the Pb content of wines as well.     

青黛中微量元素含量测定分析

用原子吸收分光光度法测定了青黛中的7种微量元素。结果表明,青黛中含有丰富的人体必需的微量元素和极微量的有害元素镉和铅。     

Anodic stripping voltammetric determination of lead and cadmium in soil extracts

Two single-step extraction procedures validated by BCR, extraction with 0.43 mol dm⁻³ acetic acid and 0.05 mol dm⁻³ EDTA, are used for assessing bioavailable species of Pb and Cd in soils. After an extensive study of interferences of humic substances and using standard additions procedures, the extractable contents of Pb and Cd have been determined by DPASV directly in soil extracts with a good reproducibility (RSD varied from 1.0 to 7.9 %). Pb(II) and Cd(II) were released from complex in EDTA extracts by pH adjustment to 1 with 1 mol dm⁻³ HCl. The results were compared with those obtained with atomic absorption spectrometry and indicated reasonable agreement of both methods. Exchangeable forms represented 0.2 to 3.3 % and 13.0 to 63.6 % of total content of Pb and Cd in soils, respectively. EDTA extraction released from soils 7.9 to 29.9 % and 33.5 to 59.6 % of total content of Pb and Cd, respectively.     

海水中铜锌铅镉的萃取-反萃取法同时提取-原子吸收光谱法测定

采用萃取-反萃取法同时提取出海水中Cu、Zn、Pb、Cd,Cu、Pb、Cd石墨炉法测定,Zn用火焰法测定.对样品的前处理方法和最佳仪器条件进行了研究,并通过加标实验验证了方法的可靠性.结果表明:萃取-反萃取法能完全满足海水中Cu、Zn、Pb、Cd的前处理要求,可节省一半前处理时间,有溶液稳定、环保、节省试剂等优点.     

原子吸收光谱法测定宁夏几种中草药中微量元素含量

采用原子光谱法测定了宁夏几种野生中草药苦豆子、败酱草、老瓜头全草及根、茎、叶中Ca、Mg、Fe、Mn、Zn、Cu、Pb、Cd 8种元素的含量。结果表明,几种野生中草药Ca、Mg、Fe、Mn、Zn、Cu含量较为丰富,Pb含量低,Cd未检出,分析结果对几种中草药的辨证使用及其生长环境的研究具有一定的实际意义。     

十种元素在癌瘤组织中的分布

通过２５种（１５８例）正常人组织和２９种（１６８例）癌瘤组织中Ａｓ，Ｓｅ、Ｐｂ，Ｃｄ，Ｃｏ，Ｚｎ，Ｃｕ、Ｈｇ、Ｆｅ和Ｍｇ等十种元素量分析，发现癌瘤组织中Ｃｄ、Ｐｂ，Ａｓ三种元素高于正常组织，而Ｓｅ和Ｚｎ两种元素与致癌元素的比值进行显著性测验，结果癌组明显高于正常组。