七种中成药中有毒重金属元素的测定

目的建立原子吸收分光光度法测定灯盏花素注射液、丹参注射液、清开灵注射液、胃康灵胶囊、冠心丹参胶囊、康尔心胶囊和桂龙咳喘宁胶囊中砷、汞、铅、镉的残留量。方法湿法消解样品,运用氢化物发生原子吸收分光光度法测定砷、汞和铅的含量,用空气-乙炔火焰原子吸收分光光度法测定镉的含量。结果在丹参注射液和康尔心胶囊中,砷的回收率分别为89.01%~116.41%和93.60%~103.17%,汞的回收率分别为80.70%~113.83%和86.12%~115.88%,铅的回收率分别为96.27%~109.48%和99.97%~110.61%,镉的回收率分别为93.00%~114.40%和96.50%~102.93%。结论7种中成药中砷、汞、铅、镉的残留量均不超标。     

石墨炉原子吸收分光光度法测定葛根芩连片中铅、镉、铜、锰的含量

目的:建立石墨炉原子吸收分光光度法测定葛根芩连片中铅、镉、铜、锰的含量.方法:采用硝酸和高氯酸(2:1,v/v)消解样品,用石墨炉原子吸收分光光度法测定铅、镉、铜、锰的含量.结果:各元素的方法回收率在98.4%～99.0%之间,RSD在1.0%～1.2%之间.结论:该方法准确、可靠,适用于葛根芩连片中铅、镉、铜、锰的含量测定.     

原子吸收光谱法测定小活络丸中重金属的含量

目的:测定34家企业生产的小活络丸中铅、镉、砷、汞、铜的含量。方法:采用微波消解样品,石墨炉原子吸收分光光度法测定铅、镉、砷的含量;氢化物原子吸收分光光度法测定汞的含量;空气-乙炔火焰原子吸收分光光度法测定铜的含量。结果:34家企业生产的小活络丸中,铅、镉、砷、汞均有不同程度的超出规定限度。结论:该方法简单、准确,可用于小活络丸中重金属的含量测定。     

原子吸收分光光度法测定香丹注射液中铅和镉的含量

目的建立原子吸收分光光度法测定香丹注射液中铅、镉的含量。方法高温法消解样品,石墨炉法测定铅、镉的含量。结果铅、镉分别在0.0025～0.004μg·ml-1和0.0004～0.004μg·ml-1范围内线性关系良好;r分别为0.9990、0.9988;平均回收率分别为102.2%、98.74%,RSD分别为5.95%、5.75%。结论该方法准确、灵敏,可用于测定香丹注射液中铅、镉的含量。     

不同产地野菊花中微量元素含量的测定

目的:建立测定不同产地野菊花中微量元素含量的方法。方法:采用石墨炉原子吸收分光光度法(GFAAS)测定药材中铅(Pb)、镉(Cd)、砷(As)的含量;采用原子冷吸收分光光度法(HGAAS)测定药材中汞(Hg)的含量;采用火焰原子吸收分光光度法(FAAS)测定药材中铜(Cu)、铁(Fe)、锰(Mn)、钙(Ca)、锰(Mg)、锌(Zn)的含量。结果:Pb、Cd、As、Hg、Cu、Fe、Mn、Ca、Mg、Zn检测质量浓度线性范围分别为0~50(r=0.999 9)、0~10(r=0.999 2)、0~50(r=0.999 0)、0~20(r=0.999 5)、0~5(r=0.999 3)、0~15(r=0.999 8)、0~2(r=0.999 9)、0~50(r=1.000 0)、0~20(r=0.999 9)、0~2μg/L(r=0.999 8);精密度、稳定性、重复性试验的RSD<3%;加样回收率分别为94.25%~97.43%(RSD=1.07%)、94.97%~99.46%(RSD=1.68%)、96.25%~99.46%(RSD=1.09%)、96.61%~99.91%(RSD=1.26%)、94.11%~98.41%(RSD=1.68%)、93.11%~99.59%(RSD=2.73%)、93.11%~99.48%(RSD=2.63%)、93.01%~99.85%(RSD=2.49%)、95.13%~99.75%(RSD=1.58%)、94.08%~97.37%(RSD=1.18%),n均为6。结论:该方法操作简便、稳定、重复性好,可用于不同产地野菊花中微量元素含量的测定。     

不同消解方法测定保健食品桑苣胶囊中铅、镉的对比研究

目的建立保健食品桑苣胶囊中铅、镉的含量测定方法。方法样品采用微波消解法与湿法消解,以原子吸收分光光度法对桑苣胶囊中铅、镉的含量进行对比研究,比较不同消解方法的精密度、重复性及回收率等。结果微波消解与湿法消解测定桑苣胶囊中铅、镉的平均回收率分别为99.97%、100.46%,99.21%、98.73%。结论采用微波消解法进行样品前处理更简便、更快捷,更适用于桑苣胶囊中铅和镉的含量测定。     

鱼腥草注射液中铅镉砷汞铜残留量的测定

目的建立测定鱼腥草注射液中铅镉砷汞铜残留量的方法。方法采用石墨炉原子吸收分光光度法测定铅、镐含量;火焰原子吸收分光光度法测定铜含量;氢化物发生-原子荧光法测定砷汞含量。结果铅、镐、砷、汞、铜的回收率分别为98．01％、90．17％、88．91％、86．68％、84．83％。结论该方法操作简便、快速,可用于鱼腥草注射液中铅镉砷汞铜残留量的测定。     

益母草注射液中铅、镉、砷、汞、铜残留量的测定

目的：建立测定益母草注射液中铅、镉、砷、汞、铜残留量的方法。方法：采用石墨炉原子吸收分光光度法测定铅、镉含量；氢化物发生-原子荧光法测定砷、汞含量；火焰原子吸收分光光度法测定铜含量。结果：铅、镉、砷、汞、铜的回收率（n=6）分别为116．4％，91．36％，108．5％，96．93％，81．17％。结论：该方法操作简便、快速，可用于中药注射液中铅、镉、砷、汞、铜残留量的测定。     

原子吸收分光光度法测定磺胺嘧啶银乳膏的含量

目的建立原子吸收分光光度法测定磺胺嘧啶银乳膏含量的方法。方法应用原子吸收分光光度法进行测定,采用标准曲线法计算样品含量。结果样品平均回收率为100.11%,RSD为0.42%。结论该方法准确、精密度高,可作为该药的质量控制方法。     

复叶耳蕨根中微量元素锌铁铜锰含量测定

目的　测定复叶耳蕨根中微量元素Zn、Fe、Cu、Mn的含量。 方法　利用微波消解法处理样品,火焰原子吸收分光光度法测定。 结果　复叶耳蕨根中Zn、Fe、Cu 、Mn含量分别为 44.09,630.91,17.08,67.45 µg·g^-1,试验各元素的加标回收率为95.4%~107.5%,RSD为0.1%~1.1%。结论　复叶耳蕨根中含有丰富的Zn、Fe、Cu、Mn,该方法准确度和精密度均符合要求,可用于实际样品的测定。     

火焰原子吸收光谱法测定化妆品中铅的不确定度评定

目的建立并运用火焰原子吸收光谱法测定化妆品中铅的不确定度评定方法。方法根据《测量不确定度评定与表示》,并参考《化学分析中不确定度的评估指南》,对火焰原子吸收光谱法测定化妆品中的铅进行测量不确定度的分析与评定。结果合成标准不确定度为0.46mg·kg^-1,扩展不确定度为0.92mg·kg^-1。结论运用该不确定度评定方法对测定过程中的关键环节进行重点质量控制,严格按照操作规范,尽可能减少稀释过程影响,可有效降低引入的不确定度,保证测定结果准确。     

Optimization of magnetic ionic based dispersive liquid-liquid microextraction of cadmium in water and food samples using experimental design prior to flame atomic absorption spectrophotometry

A magnetic ionic based dispersive liquid liquid microextraction (MIL-DLLME) procedure was optimized for the analysis and extraction of cadmium in water and food samples by flame atomic absorption spectrophotometry (FAAS). Contribution of experimental variables were optimized through central composite design combined with response surface analysis. Under optimized conditions, the limit of detection was found 0.6 ng mL^?1 with the relative standard deviation of 1.7%. Dynamic range was obtained in the concentration range of 2–700 ng mL^?1 with correlation coefficient of 0.9983. Relative recoveries were ranged from 94% to 99% with enrichment factor of 172. The validation of the optimized method was successfully confirmed by reference material analysis. The optimized method allows the analysis of cadmium in water and food samples with good reliability of the determination. Compared with the conventional procedures, the method enabled a fast, green and simple determination of cadmium in the real sample with minimal solvent consumption and a higher extraction capability.     

石墨炉原子吸收分光光度法测定冰片中微量铅镉铜

目的:建立石墨炉原子吸收分光光度法测定冰片中微量铅、镉、铜的分析方法.方法:检查波长铅为283.3 nm,镉为228.8nm,铜为324.7 nm;灯电流为10.0 mA;狭缝宽度为0.4 nm.结果:铅在0.0～40.0 ng/mL、镉在0.0～1.0 ng/mL、铜在0～10 ng/mL范围内有较好的线性关系,平均加样回收率分别为98.3％,98.0％,97.3％.结论:石墨炉原子吸收分光光度法测定冰片中微量铅、镉、铜,方法准确、简单、灵敏,被测溶液稳定性好.     

复方电解质眼内冲洗液中氯化钙及硫酸镁的含量测定

目的：建立快速准确地检验复方电解质眼内冲洗液中氯化钙及硫酸镁含量的新方法。方法：采用火焰原子吸收分光光度法富燃火焰测定复方电解质眼内冲洗液中氯化钙的含量、计量火焰测定硫酸镁的含量。结果：氯化钙回收率为98．18％～100．64％,RSD=0．76％（n=9）,方法检出限为0．5μg·ml^-1;硫酸镁回收率为99．11％～100．76％,RSD=0．56％（n=9）,方法检出限为0．002μg·ml^-1。结论：本方法操作简便精密度好,结果准确可靠。     

石墨炉原子吸收分光光度法测定维生素C原料中微量铅、镉含量

目的 建立石墨炉原子吸收分光光度法测定维生素C原料中微量铅、镉的分析方法.方法 检测波长铅为283.3 nm、镉为228.8 nm,灯电流为2.0 mA,狭缝宽度为0.4 nm.结果 铅质量浓度在0.0~10.0 ng/mL、镉质量浓度在0.0~0.5 ng/mL范围内与吸光度呈较好的线性关系,平均加样回收率分别为98.6%和97.8%,RSD分别为1.1%和1.5%(n=9).结论 石墨炉原子吸收分光光度法测定维生素C原料中微量铅、镉,方法准确、简单、灵敏,被测溶液稳定性好.     

维生素B2注射液中镉、砷和铅的电感耦合等离子体质谱法测定

建立了电感耦合等离子体质谱法测定维生素B2注射液中的镉、砷和铅.维生素B2注射液经过微波消解,使用铟、锗、铋作为内标元素进行校正,以杨树叶为质控标准物,镉和铅在1～100 ng/ml、砷在1～150 ng/ml浓度范围内线性关系良好,回收率为92.4％～101.7％,RSD小于4.1％.     

Optimisation of parameters for determination of rubidium in spent CAPD fluids by flame and electrothermal atomic absorption spectrometry

An analytical procedure is reported for the determination of rubidium in spent continuous ambulatory peritoneal dialysis (CAPD) fluids by flame and electrothermal atomic absorption spectrometry (FAAS, ETAAS). Samples of spent CAPD fluids were collected as 5 ml aliquots in polyethylene tubes and stored in a freezer at -20 degrees C. Before analysis, samples were equilibrated to room temperature and analysed within 8 h. A total of 2 mg ml(-1) of caesium was added to each sample and standard solution to overcome interferences from ionisation. An air-acetylene flame was applied in FAAS determinations. Analysis was performed against aqueous standards. The calibration graph was linear from 30.0 up to 5000 microg l(-1) Rb, while the limit of detection (3 s) was found to be 20.0 microg l(-1) rubidium. Good repeatability of measurement (RSD 1%) was obtained. Parameters were also optimised for determination of rubidium in spent CAPD fluids by ETAAS. Ten-fold diluted samples (3.5% nitric acid) were analysed applying standard addition calibration. The calibration graph was linear from 2.0 up to 30.0 microg l(-1) rubidium, while the limit of detection (3 s) was found to be 1.0 microg l(-1) rubidium (sample volume 10 microl). Good repeatability of measurement (RSD 5%) was obtained. The results of direct determination by FAAS and ETAAS were compared to those obtained after acid digestion of samples in Parr bombs. The accuracy of the procedure for direct determination was checked by spiking samples. In 73% of samples analysed, the differences between the results obtained by the two techniques, either for direct determinations of samples or for samples digested in a Parr bomb did not exceed +/-10%.     

Lead,Cadmium and Nickel Contents of Some Medicinal Agents

Thirty nine brands of pharmaceutical dosage forms (28 tablets, 4 syrups, 6 suspensions and one chewing gum) that are available in United Arab Emirates pharmaceutical markets were investigated for the presence of three heavy metals; lead, cadmium and nickel. Amongst the samples, 13 products were manufactured locally in United Arab Emirates and 26 products were imported from around the world. The samples were prepared by acid digestion procedure and the resultant solutions were analyzed for heavy metals by using a validated graphite furnace atomic absorption spectrometric method. Calibration curves were achieved using different concentration of lead, nickel and cadmium ranged from 0.001 to 0.05 μg/ml. The mean recoveries of metals from the samples were 86.4 to 97%. The %relative standard deviation for the intraassay and interday precision for the metals were <5%. Amongst the 39 samples of pharmaceutical dosage form all exhibited a positive response for lead, cadmium and nickel except three products whose Ni levels were below quantification level. The products contained variable amounts of heavy metals as of 0.0017 to 11.88 μg lead; 0.0011 to 0.5559 μg cadmium and 0.0011 to 2.6428 μg nickel, respectively. Based on maximum recommended daily dose (g) of these products, maximum daily ingested mass of lead was 0.0034 to 11.88 μg/d, 0.0013 to 0.56 μg/d for cadmium and 0.0011 to 2.64 μg/d for nickel, respectively. The results were compared with those of oral permitted daily exposure levels of United State Pharmacopeial National Formulary 2013. All the products were safe to consume and contained lower level of lead, cadmium and nickel than Oral Permitted Daily Exposure levels, except three products which showed higher level of lead than oral permitted daily exposure levels. Hence the raw materials used in manufacturing of these medicinal agents might be responsible for the presence of higher level of lead.     

人参等10种中药材及饮片中重金属及有害元素测定

目的：采用微波消解-电感耦合等离子体质谱（ICP-MS）法测定人参、白茅根、白头翁、苍术、大黄、骨碎补、苦参、龙胆、红参、肉苁蓉10种中药材及饮片中重金属及有害元素的含量。方法：采用微波消解法对样品进行前处理,电感耦合等离子体质谱（ICP-MS）法对500批中药材及饮片中铅、镉、砷、汞、铜5种重金属及有害元素进行含量测定,并对样品中镍、铬、钡3种金属元素含量进行考察,应用SPSS19.0软件对数据结果进行统计学分析。结果：同一品种8种元素测定值与来源（野外采集、基地种植与市售饮片）及产地无明显相关性。500批样本测定结果显示：铅、镉、砷、汞、铜元素总超标率分别为6.60%、25.20%、1.00%、0.00%、0.40%;元素残留量与药材品种存在一定的相关性,镉元素在白头翁、苍术、骨碎补、龙胆药材中容易蓄积,而铅元素易在白头翁药材中蓄积残留,导致残留量较高。大黄、白头翁、龙胆中钡元素、镍元素、铬元素含量均明显高于其他品种。汞均未超出0.2 mg·kg^-1;除5批样本外,砷均未超出2 mg·kg^-1;除2批样本外,铜均未超出20 mg·kg^-1,表明上述10种中药材及饮片中砷、汞、铜元素残留方面的安全隐患较低。结论：有必要对中药材及饮片中部分重金属元素的含量加以监管,以保证中药的品质和临床用药安全。该方法准确、简便、灵敏,可为中药材及饮片中重金属及有害元素的检测与控制提供参考。     

Trace element determination of Argentine wines using ETAAS and USN-ICP-OES.

The objective of this work was to develop a method to determine the metal content in wine samples from the province of Mendoza in Argentina. Ten samples of white wine and 10 samples of red wine available in the supermarket were analyzed for the metals aluminium, cadmium, calcium, chromium, copper, iron, nickel, lead and zinc by electrothermal atomic spectrometry (ETAAS) and ultrasonic nebulization was coupled to inductively coupled plasma optical emission spectrometry (USN-ICP-OES). The aluminium, cadmium, calcium, copper, iron, lead, zinc, chromium concentrations were between 17.0-18.0 microg l(-1), 1.0-4.7microg l(-1), 10.0-15.0 mg l(-1), 23.0-28.0 microg l(-1), 480-790 microg l(-1), 50-90 microg l(-1), 24-130 microg l(-1), and <0.2-6.25 microg l(-1), respectively. The levels compare well with those reported for similar wines from some other parts of the world. A significant aspect in this paper is the samples mineralization step, which allowed the direct determination of the metals. Concerning to the Cd determination, a refluxing digestion system was used for the pretreatment of the samples.