六种常用滋补中药铅、汞、镉含量的测定

为了解山楂、山药、百合、枸杞子、麦冬、莲子六种常用滋补中药有害重金属含量,用石墨炉原子分光光度法测定了六种中药的铅和镉含量,用冷原子吸收分光光度法测定了六种中药的汞含量。结果表明,六种中药有害重金属含量由高到低顺序为:铅、镉、汞,六种中药汞含量均不超过0.02 mg/kg,镉含量最高0.32 mg/kg,最低0.08 mg/kg,铅含量在0.53~2.43 mg/kg之间。     

潮州市西湖沉积物中金属元素的污染特性研究

用原子吸收分光光度法研究了潮州市西湖沉积物中的铜、锌、铅、镉、锰、镍、镁、钙等金属元素的含量及分布规律。结果表明,铜、铅、锌、镉和镍是主要的重金属污染物,沉积物中5种重金属的平均含量为:铜584.7 mg/kg,铅149.1 mg/kg,锌360.9 mg/kg,镉1.2 mg/kg,镍76.7 mg/kg,均高于我国土壤背景值。     

ICP-AES法测定焊锡中铅、镉及其不确定度的评价

在加热条件用浓硝酸消解样品,同时伴随有少量白色沉淀,冷却后再加入1~3滴纯盐酸使产生的白色沉淀完全消解,用ICP-AES法对样品中铅、镉进行了测定,建立了数学模型对其不确定度进行了评定。结果表明,样品中铅和镉的含量分别为Pb 258 mg/kg和Cd 27.1 mg/kg,扩展不确定度分别为Pb 15.5 mg/kg和Cd 1.54 mg/kg(k=2)。     

水母雪莲中不同器官五种元素含量测定

用火焰原子吸收光谱法\石墨炉原子吸收光谱法以及分光光度法对水母雪莲花不同器官中K,Mg,Pb,Cd和P元素进行了测定分析。在水母雪莲的花中,钾的含量最高,可达26045.22mg/kg。在水母雪莲瘦果中磷的含量最高达6944.444 mg/kg。水母雪莲苞片中镁的含量最高为7066.51 mg/kg。重金属元素铅在叶中最高,其次为根中和苞片中,茎、花萼及瘦果中含量都很少。而重金属元素镉在苞片和花中含量较高,在其他各器官中含量较低。     

火焰原子吸收分光光度法测大沂河水体的重金属含量

采用火焰原子吸收分光光度法测定了山东省曲阜市大沂河水体的重金属铜、铅、镉、锌含量。结果表明,大沂河水体中铜、铅、镉、锌的最高含量分别为0.018,0.230,0.176,0.490mg/L,其中铅和镉的含量超过国家Ⅴ类水标准。     

阻抑动力学光度法同时测定痕量铅和镉

基于氨水溶液介质中,痕量镉和铅阻抑过氧化氢氧化偶氮胂Ⅰ褪色的作用,建立了动力学光度法同时测定痕量铅和镉的新方法。方法测定铅、镉的线性范围分别为0.005~0.50μg/mL和0.002~0.80μg/mL。用于实际样品中铅、镉同时测定。     

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。     

二乙胺荒酸钠–四氯化碳萃取连续光源原子吸收法测定磷酸一二钙中的痕量铅、镉

建立连续光源原子吸收分光光度法同时测定磷酸一二钙(MDCP)中铅、镉的方法。MDCP经盐酸消解后,以氢氧化钠溶液调节p H为11,加入KCN作为掩蔽剂,用二乙氨荒酸钠–四氯化碳络合铅、镉离子,再经CCl_4进一步萃取浓缩,采用连续光源原子吸收分光光度法测定铅、镉的含量。该方法铅、镉的检出限为1,0.5 mg/kg;用于不同批次MDCP产品测定,铅、镉测定结果的相对标准偏差分别为3.58%,6.91%(n=11);铅、镉的加标回收率分别为88.9%~104.7%,91.0%~106.4%。该法可用于MDCP中痕量铅、镉的同时测定。     

液相色谱-质谱/质谱法检测人参和土壤中多菌灵的残留动态

建立了液相色谱-质谱/质谱法测定50%多菌灵可湿性粉剂在人参和土壤中的消解动态和残留量。多菌灵在0.01~0.5μg/mL质量浓度范围内呈良好线性,相关系数为0.9985,在0.01~0.2 mg/kg加标水平下,多菌灵在人参和土壤中的回收率为82.74%~91.88%,相对标准偏差(RSD)为2.85%~6.28%,最低检出浓度为0.005mg/kg。两年两地残留实验结果表明,拌土施药剂量52 500g a.i./hm2下,人参和土壤中多菌灵半衰期分别为11.6~13.7d和10.4~13.0d,最终残留量分别在0.0075~0.0332mg/kg和0.0068~0.0428mg/kg之间。建议我国对人参中多菌灵的最大残留限量(MRL)值为0.5mg/kg,最高施药剂量52 500g a.i./hm2,安全施药间隔期28d。     

微波消解-ICP-MS测定电镀污泥中的重金属

采用微波消解系统对某电镀污泥进行消解,利用ICP-MS对污泥中的重金属进行测定。称取制备后样品,置于消解罐中充分反应后,赶酸、定容后利用电感耦合等离子体质谱法进行测定。电镀污泥中的铬为18845.2mg/kg、镉为10.3mg/kg、镍为5200.0mg/kg、铅为189.7mg/kg、铜为3271.7mg/kg、锌为49632.6mg/kg。测定结果表明所检测项目工作曲线线性关系好,相关系数r均大于0.999。铬加标回收率在91.6～97.7%之间、镉加标回收率在92.0～97.0%之间、镍加标回收率在95.1～98.0%之间、铅加标回收率在94.3～95.2%之间、铜加标回收率在97.1～102%之间、锌加标回收率在96.3～98.7%之间,均满足相关测定要求。计算的潜在生态危害系数、潜在生态危害指数结果表明,电镀污泥中的铬、镉、铅、铜、锌为轻微生态危害,镍为强生态危害;潜在生态危害指数RI计算值为216.69,属于中等生态危害。     

豆腐生产过程中微量元素硒分布特性研究

为确定以不同硒含量的大豆为原料生产豆腐过程中硒分布特性,用石墨炉原子吸收分光光度法对该过程中各种产物的硒含量进行了分析研究。结果表明,以硒含量分别为0.692、2.561、2.801 mg/kg的大豆为原料生产得到的豆腐、黄浆水、豆渣的硒含量分别为:0.089、0.250、0.138 mg/kg,0.462、0.760、0.507 mg/kg和0.532、0.764、0.524 mg/kg。豆腐生产过程中,以低硒大豆为原料生产豆腐,硒总回收率为75.59%;采用富硒大豆为原料生产,硒的回收率分别达到87.37%、87.20%;生产过程中豆腐、黄浆水和豆渣中硒含量占总回收硒的比率分别为39.01%～49.97%、23.92%～29.89%、26.11%～30.92%。     

洛阳市郊区叶菜中重金属含量抽样分析及评价

为了研究洛阳市郊区蔬菜中重金属污染状况,采用火焰原子吸收法对郊区李楼乡和孙旗屯乡抽取的叶菜样品中重金属Cu、Zn、Pb、Cd含量进行了测定。结果表明,8个蔬菜样品中Cu含量在0.393 9～0.970 7 mg/kg之间,Zn含量在1.395 0～10.080 0 mg/kg之间,均未超过国家蔬菜卫生限量标准;Pb含量在0.100 0～0.248 6 mg/kg之间,其中有3个样品Pb含量超出国家蔬菜卫生限量标准;Cd含量有5个样品未检出,其余3个样品也不超国标。经用单因子和综合因子污染指数评价,洛阳市郊区叶菜类蔬菜重金属污染大部分已处于警戒级到轻度污染,因此,应加强蔬菜中重金属污染的预防与治理工作。     

Determination of mineral balances in sheep offered feed with added cadmium and zinc

The optimum conditions for microwave digestion of herbage and faeces to determine mineral concentrations were obtained by varying sample mass, reagent and heating programme, and it was confirmed that the resulting element concentrations were the same as for certified reference material. The effects of feeding cadmium to sheep at a level that is typical of polluted regions (1 mg/kg) for ten days were investigated, as well as the possible amelioration of cadmium effects by adding 30 mg/kg Zn to the diet. Cadmium in the feed increased the cadmium balance and produced several mineral disturbances, in particular a reduction in sodium balance which is typical of renal tubular disorders. Including zinc in the diet as well as cadmium reduced the cadmium balance to a level similar to that of sheep that did not receive cadmium or zinc, which suggests that the zinc status is critical in determining whether cadmium in feed increases the cadmium balance in sheep.     

Determination of mineral balances in sheep offered feed with added cadmium and zinc

The optimum conditions for microwave digestion of herbage and faeces to determine mineral concentrations were obtained by varying sample mass, reagent and heating programme, and it was confirmed that the resulting element concentrations were the same as for certified reference material. The effects of feeding cadmium to sheep at a level that is typical of polluted regions (1 mg/kg) for ten days were investigated, as well as the possible amelioration of cadmium effects by adding 30 mg/kg Zn to the diet. Cadmium in the feed increased the cadmium balance and produced several mineral disturbances, in particular a reduction in sodium balance which is typical of renal tubular disorders. Including zinc in the diet as well as cadmium reduced the cadmium balance to a level similar to that of sheep that did not receive cadmium or zinc, which suggests that the zinc status is critical in determining whether cadmium in feed increases the cadmium balance in sheep. Received: 1 August 1997 / Revised: 8 December 1997 / Accepted: 10 December 1997     

Effect of irradiation on anti-nutrients (total phenolics, tannins and phytate) in Brazilian beans

The Brazilian bean varieties Phaseolus vulgaris L. var. Carioca and Vigna unguiculata (L.) Walp var. Macaçar were irradiated with doses of 0.5, 1.0, 2.5, 5.0 and 10 kGy and subsequently stored at ambient temperature for 6 months. The anti-nutrients phenolic compounds, tannins and phytate were determined to be 0.48 mg g⁻¹ dry basis, 1.8 mg g⁻¹ dry basis and 13.5 μmol g⁻¹ dry basis in the raw non-irradiated Carioca beans and 0.30 mg g⁻¹ dry basis, 0.42 mg g⁻¹ dry basis and 7.5 μmol g⁻¹ dry basis in the raw non-irradiated Macaçar beans. After soaking and cooking a higher content of phenolic compounds and a lower phytate content was observed in both bean varieties. Tannin content was not affected by soaking and cooking of Carioca beans, but higher after soaking and cooking of Macaçar beans. Using radiation doses relevant for food did not effect the content of the anti-nutrients under investigation in both bean varieties.     

Determination of cadmium, lead, and thallium in materials of the environmental specimen bank using mass spectrometric isotope dilution analysis (MS-IDA)

Summary An analytical procedure for the simultaneous determination of cadmium, lead, and thallium in the mg/kg- and g/kg-range in biological materials and sewage sludge by mass spectrometric isotope dilution analysis (MS-IDA) is described.Cadmium, lead, and thallium were separated by electrolytical deposition after low temperature ashing (LTA) of the samples in oxygen plasma and dissolution of the ashes in HNO₃ or HNO₃/HF. Measurement of the isotopic ratio was carried out with a thermal ionization mass spectrometer using the silica gel technique. Cadmium contents ranging from 1.03 to 4.60 mg/kg with relative standard deviations from 0.3 to 1.3%, lead contents ranging from 75 g/kg to 25 mg/kg with relative standard deviations from 0.6 to 3.5%, and thallium contents ranging from 2.9 to 247.7 g/kg with relative standard deviations from 0.1 to 1.7% were determined in the materials of the environmental specimen bank analyzed.

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Bestimmung von Cadmium, Blei und Thallium in Materialien der Umweltprobenbank mit der massenspektrometrischen Isotopenverdünnungsanalyse

Zusammenfassung Ein Analysenverfahren zur simultanen Bestimmung von Cadmium, Blei und Thallium im mg/kg- und g/kg-Bereich in biologischen Materialien und Klärschlamm mit der massenspektrometrischen Isotopenverdünnungsanalyse (MS-IDA) wird beschrieben.Nach Niedertemperaturveraschung (LTA) der Proben im Sauerstoffplasma und Lösen der Aschen in HNO₃ oder HNO₃/HF-Gemisch werden Cadmium, Blei und Thallium durch elektrolytische Abscheidung abgetrennt. Die Isotopenverhältnismessung erfolgt mit der Silicageltechnik in einem Thermionen-Massenspektrometer. In den analysierten Probenbankmaterialien werden Cadmiumgehalte im Bereich von 1,03 bis 4,60 mg/kg mit relativen Standardabweichungen von 0,3 bis 1,3%, Bleigehalte im Bereich von 75 g/kg bis 25 mg/kg mit relativen Standardabweichungen von 0,6 bis 3,5 % und Thalliumgehalte im Bereich von 2,9 bis 247,7 g/kg mit relativen Standardabweichungen von 0,1 bis 1,7% bestimmt.

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Dedicated to Prof. Dr. W. Fresenius on the occasion of his 70th birthday     

石墨炉原子吸收光谱法测定苦黄注射液及其中药材中的铅和镉

应用石墨炉原子吸收光谱（GF-AAS）法测定了苦黄注射液及其生中药材中铅及镉量。试样用浓硝酸及过氧化氢消解。对仪器的工作条件,包括波长、光谱带宽、灰化温度及原子化温度,作了试验和优化。选用柠檬酸作为基体改进剂,对大黄、茵陈、柴胡、苦参及“苦黄”注射液等试样中的铅及镉量作了测定,分析结果的相对标准偏差均小于4．4％。按标准加入法作了回收率试验,测得值在96%～110％之间。     

Indirect complexometric determination of cadmium(II) using 1,10-phenanthroline as selective masking agent

An indirect complexometric method is described for the determination of cadmium(II), 1,10-phenanthroline being used as masking agent. Cadmium(II) in a given sample solution is initially complexed with an excess of EDTA and the surplus EDTA is titrated with lead nitrate solution at pH 5.0–6.0 (hexamine), using xylenol orange as indicator. An excess of 1,10-phenanthroline is then added and the EDTA released from the Cd-EDTA complex is titrated with standard lead nitrate solution. Results are obtained for 1.5–57 mg of Cd with relative errors 0.90% and standard deviations 0.06 mg. Cu(II), Co(II), Hg(II), Ni(II), Zn(II), Pd(II), Tl(III), Au(III) and Sn(IV) interfere, but can be easily masked. The method is applied for the determination of cadmium in synthetic alloy solutions.