石墨炉原子吸收光谱法规定全血铅的方法研究

目的:建立一种新的血铅测定方法。方法:选择测定最佳条件,采用5%的4—甲基氢氧化铵做为一种新的稀释剂,用石墨炉原子吸收法测定全血铅。结果:本法的检出限为11pg,相对标准偏差为2.5%～4,4%,回收率为94%～99%。标准曲线在。0～100μg/L范围内线关系良好。结论:本法简便、快速、灵敏,准确度高,精密度好,适用好大量的日常样品检测,结果满意。     

AA800石墨炉原子吸收光谱仪检测全血铅

目的用PE AA800石墨炉原子吸收光谱仪测定全血铅,并探讨相关实验条件。方法取全血样本0.4 mL,用普析MG2型血铅稀释液进行溶血稀释后,直接用PE AA800石墨炉原子吸收光谱仪进行测定,并分析其检测性能。结果该方法回收率93.2%~107.4%,变异系数CV1.39%~2.60%,相对标准差(RSD)1.15%~2.35%,共存离子对检测结果的干扰小;用于分析720例儿童和162例成年人静脉血标本,结果满意。结论该方法操作简便、快速、准确,为一种理想的血铅测定方法。     

丝网印刷电极法测定血铅的方法学评价

目的比较丝网印刷电极(SPE)法和石墨炉原子吸收光谱(GFAAS)法在血铅检测中的应用,评价SPE法的实用性和可靠性。方法采用SPE法检测卫生部临床检验中心室间质控样本和全血样本,进行方法学评价,并与GFAAS法进行比较。结果 SPE法检测血铅低、中、高3个水平样本的相对标准偏差(RSD)分别为14.80%、4.03%、2.11%,平均回收率为103.7%。SPE法测定全血样本的结果与GFAAS法比较差异无统计学意义(P0.05),线性回归分析相关系数(r2)为0.964,2种方法呈高度相关。Bland-Altman分析显示2种方法具有一致性。以GFAAS法为金标准,SPE法假阳性率为4.4%,假阴性率为0.0%。结论 SPE法稳定性强、操作简便,与GFAAS法呈高度相关,适用于临床大批量样本的快速检验。     

原子吸收光谱法测定碳酸氢钠中铜含量的不确定度评估

目的：探讨标准曲线法在石墨炉原子吸收光谱中测定碳酸氢钠中铜含量的不确定度。方法：利用标准曲线的相关系数,建立数学模型,找出影响不确定度的因素,并对其分量进行评估。结果：碳酸氢钠中铜的含量为0.000010578%±0.000000090%,p=95%。结论：该方法可用于标准曲线法在石墨炉原子吸收光谱中测定铜含量的不确定度分析。     

石墨炉原子吸收光谱法规定全血铅的方法研究

目的：建立一种新的血铅测定方法。方法：选择测定最佳条件，采用5％的4-甲基氢氧化铵做为一种新的稀释剂，用石墨炉原子吸收法测定全血铅。结果：本法的检出限为11pg，相对标准偏差为2．5％～4．4％，回收率为94％～99％。标准曲线在0～100μg／L范围内线关系良好。结论：本法简便、快速、灵敏，准确度高，精密度好，适用好大量的日常样品检测，结果满意。     

纳米银抗菌凝胶中银含量检测方法的探讨

摘要 目的 建立一种简便、快速的纳米银抗菌凝胶前处理方法，并对银含量的检测方法进行对比研究。方法 分别采用超声波溶解和硝酸消解的方式对抗菌凝胶进行处理，优化前处理方法，并对检测银含量的石墨炉原子吸收法（GFAAS）和电感耦合等离子体质谱法（ICP-MS）进行比较分析。结果 抗菌凝胶用超声波溶解效果好，简单、快速，可代替传统硝酸消解。通过方法学验证和方法比对试验，GFAAS法可代替ICP-MS法检测抗菌凝胶中银含量。结论 纳米银抗菌凝胶用超声波溶解处理、GFAAS法检测银含量，具有准确、便捷、经济等优点，可为相关国家标准的修订提供参考。     

改良石墨炉原子吸收法直接测定血液中的铅

目的 建立一种改良石墨炉原子吸收法直接测定血液中铅的方法 .方法 以氯化钯、硝酸铵和Trionx-100作为基体改进剂,血液样品经稀释后直接用石墨炉原子吸收法测定.结果 氯化钯、硝酸铵和Trionx-100基体改进剂的使用,可将灰化温度提高到1 000℃,降低血液成分对测定结果 的影响.线性范围为0～80μg/L,相关系数在0.9980以上,相对偏差为55%～12.2%,回收率为90.1%～106.2%,方法 的检出限为1.1 μg/L.结论 此方法 具有准确可靠、简便快速、样品不需要消化、污染小等优点,可适用于血铅的测定.     

生物样品中铜的石墨炉原子吸收检测及其在肝豆状核变性诊断中的应用

目的建立诊断肝豆状核变性患者的生物样品中微量铜的石墨炉原子吸收检测方法。方法尿液和血清样品经1％HNOsub3/sub 稀释后,采用石墨炉原子吸收光谱标准曲线法直接测定。结果线性范围0~200 g/L,相关系数0.9997,方法检出限为1.4 g/L,回收率96.7％～99.2％,相对标准偏差1.0%~1.7％,经冻干人尿标样（GBW 09102）对照测定,其结果在允许范围内,相对误差为-1.2％。结论采用GFAAS法测定生物样品中铜,方法可靠、准确、灵敏,能适用于肝豆状核变性诊断中生物样品微量铜检测的要求。     

氯化钯作改进剂石墨炉原子吸收法测定尿中铅

目的 建立比重校正-氯化钯作改进剂石墨炉原子吸收法直接测定尿中铅的分析方法.方法 尿样不进行消化处理,采用比重校正-氯化钯作改进剂石墨炉原子吸收法直接测定尿中铅的含量.结果 尿样用氯化钯等体积稀释,方法的线性范围为0~60 μg/L,回收率97.3%~106.1%,精密度为2.1%~6.4%.结论 此法快速、简单、回收率高,适用大规模样品的测定.     

多种微量元素的微量进样AAS法测定

目的利用国产新型仪器,进行铜、锌、钙、镁、铁五种微量元素的检测.方法采用微量进样原子吸收分析技术.结果用微量血进行人体五种微量元素的检测,该法的铜、锌、钙、镁、铁微量元素的批内CV分别为:2.38%、2.35%、3.66%、2.99%和2.79%,回收率为:99.90～100.72、98.91～103.67、95.06～102.28、96.70～102.72、99.42～105.16.手指血与静脉全血测定结果基本一致,经统计学处理,差异无显著性(P＞0.05),结果与国内外文献报道相近.男性与女性间有十分显著的差异(P＜0.001).结论利用微量法进行微量元素的检测简单快速、灵敏精确、经济实用,易于广大患者接受,值得推广.     

Determination of trace elements and calcium in bone of the human iliac crest by atomic absorption spectrometry

A rapid and reliable analytical method for the determination of trace elements in human bone by atomic absorption spectrometry is reported. Calcium was determined to estimate the homogeneity of samples. Human bone from the iliac crest was obtained at autopsy of adult subjects. Before analysis samples were decomposed by microwave digestion and acid digestion in a Parr bomb. Zinc, rubidium, strontium, calcium and iron were determined by flame atomic absorption spectrometry (FAAS) and aluminium, copper and lead by electrothermal atomic absorption spectrometry (ETAAS) at optimum measurement conditions. The results for the two digestion procedures agreed for zinc, rubidium and calcium within +/-5%, for copper within +/-7% and for strontium, iron, aluminium and lead within +/-10%. The repeatability of measurement (R.S.D.) for determination of calcium and trace elements after microwave digestion and acid digestion in a Parr bomb was tested in one representative autopsy bone sample by six parallel determinations. It was found to be better than +/-5% either for microwave digested samples or samples digested in a Parr bomb, for all elements determined by FAAS and ETAAS techniques. The accuracy of the applied digestion procedures was checked by analysis of trace elements in NIST SRM 1486 Bone Meal reference material. Good agreement of the results with certified values was obtained for both digestion procedures. The microwave procedure developed for digestion of small amounts of sample was applied in trace elements analysis of bone biopsy samples from dialysis patients.     

Determination of zinc in blood serum by electrothermal atomic absorption spectrometry with matrix modification

Zinc determination in serum microsamples can be treated by graphite furnace atomic absorption spectrometry. To reduce the contamination risks and to obtain results as right as possible, the serum has been twenty fold diluted instead of 100-fold diluted (rate frequently obtained). In these conditions, the use as diluent of a 1% Triton X 100 solution or of a 33.7 mmol/l magnesium nitrate did not allow to obtain exact results. Yet, with an 37.8 mmol/l ammonium phosphate solution, the results given by the direct calibration on an aqueous calibration curve were in good accordance with those found with a recommended flame atomic absorption spectrometry method. The within-run RSD of our method was 2.6%.     

Manganese content of the cellular components of blood

We measured the manganese content of whole blood, plasma, platelets, mononucleated cells, polymorphonucleated cells, and erythrocytes. Platelets and blood cells were separated from whole blood by use of discontinuous gradients of colloidal polyvinylpyrrolidone-coated silica (Percoll), and their manganese content was measured by Zeeman graphite furnace atomic absorption spectrophotometry, after digestion with nitric acid and hydrogen peroxide. Erythrocytes account for about 66% of the manganese in whole blood, whereas the "buffy coat"--platelets and leukocytes--accounts for about 30%. The "buffy coat" components turn over more rapidly than do erythrocytes, so their manganese content may better indicate the body's manganese status.     

重庆市部分地区成人血铅水平及其影响因素的分析

目的 了解重庆市部分地区18～70岁公民血铅水平及其影响因素.方法 采用石墨炉原子吸收光谱仪检测静脉血铅值,对影响血铅水平的因素进行分析.结果 1 486例健康体检公民血铅平均值为(77.26±27.35)μg/L,铅中毒检出率为12.4%,成人男女性血铅水平差异无统计学意义(t=1.67,P＞0.05),男女性铅中毒的检出率差异无统计学意义(P＞0.05).成人血铅水平主要与环境因素、卫生、饮食习惯、职业、居住环境、吸烟及化妆等有关.结论 重庆市部分地区成年居民血铅平均水平及铅中毒检出率较高,长期如此将严重影响人们的生活质量和水平,如何预防和及早治疗铅中毒,应引起社会的广泛重视.     

Determination of silver in biological samples using graphite furnace atomic absorption spectrometry based on Zeeman effect background correction and matrix modification

A method for the determination of silver in human body fluids and biological material is described. The silver in an acid digest of biological samples and diluted body fluids is quantified using Zeeman graphite furnace atomic absorption spectrometry (ZGFAAS). The effects of NH4H2PO4 as matrix modifier and standard addition are discussed. Atomization from the graphite tube wall and from the pyrolytical tube with platform is also discussed and the peak height and the peak area are compared. The best results were achieved by using matrix modification, stabilized temperature platform furnace, integrated absorbance and standard addition technique. The calibration was linear up to 15 micrograms X L-1; the between-run precision was 5.9% at 40 micrograms X kg-1 of silver.     

Trace analysis of lead in blood, aluminium and manganese in serum and chromium in urine by graphite furnace atomic absorption spectrometry

A graphite furnace atomizer with automatic sampler is used to measure low levels of trace metals in biological samples by atomic absorption spectrometry. With blood and serum, the sample treatment consists of diluting (1:1) with aqueous Triton X-100 solution, centrifuging in the case of blood, and dispensing the liquid directly into a pyrolytic coated graphite tube. Sample volumes for blood and serum range from 5 to 10 microL. Stabilized urine (25 microL) is analyzed directly. The possibility of contamination is minimized by this simple procedure. The methods described minimize sample handling and involve reagents which are virtually free of contamination of the analytes. Background correction is necessary except for the determination of aluminium in serum, and precisions range from 0.7% to 4.3% RSD. The standard additions technique is used to establish the calibration and the required volume of sample and aqueous addition is automatically dispensed directly into the graphite tube.     

An ultrasensitive method for the measurement of human leukocyte calcium: lymphocytes.

Studies of the transport and distribution of calcium in leukocytes have been severely hampered by the inability to measure accurately and reproducibly the concentration of calcium in small numbers of cells. We have applied a recent development in analytical chemistry, the graphite furnace atomic absorption spectrophotometer, to this problem. The calcium content of human blood lymphocytes was determined by both graphite furnace and conventional flame atomic absorption spectrophotometry. The linearity, sensitivity and detection limits of the two techniques were compared. For measurement of calcium, the graphite furnace sensitivity was 55 times higher in aqueous samples and 60 times higher in cell samples than the flame technique. The detection limit of the graphite furnace was 800 times lower in aqueous samples and 1500 times lower in cell samples. The enhanced sensitivity of this technique allowed us to prepare samples with 20 times fewer blood cells. We have employed this graphite furnace technique to measure lymphocyte calcium content and its relationship to the calcium concentration and proportion of serum in the suspending medium. In the absence of serum, the lymphocyte calcium content approximately doubled as the medium calcium concentration was increased from 1 mumol/l to 0.5 mmol/l. At medium calcium concentrations of 0.5 mmol/l and above, the lymphocyte calcium content was 1.0 mmol/l cells. In medium adjusted to 2 mmol/l calcium, the lymphocyte calcium content approximately doubled as the medium serum concentration was increased from 0 to 2%. At medium serum concentrations of 2% and above, lymphocyte calcium content was 2 mmol/l cells. The exchangeable cell calcium, measured with 45Ca in the same samples, did not increase as serum was added to the medium.     

过氧化氢银离子消毒液中银离子稳定性检测方法研究

目的建立过氧化氢银离子复方消毒液中银含量的检测方法,从而快速、准确评价消毒剂中银离子的稳定性。方法采用塞曼背景校正石墨炉原子吸收法,在波长328.1 nm、灯电流7.0 mA和狭缝宽1.3 nm条件下,对某消毒液中银离子含量进行分析和评价。结果检测线性范围2.5～60 ng/ml,相关系数为0.9997,检出限0.10ng/ml,相对标准偏差2.13%,平均回收率为104%～116%。结论该方法测定消毒剂中银离子具有快速、准确、灵敏等优势,能满足这类消毒剂中银离子稳定性的评价。     

Direct calibration for determining aluminum in bone and soft tissues by graphite furnace atomic absorption spectrometry

We describe a direct-calibration method for determining aluminum in bone and soft tissues by graphite furnace atomic absorption spectrometry. Aluminum in bone was determined in uncoated tubes, whereas the analytical performance in soft tissue analysis was markedly improved by using pyrolytically coated tubes with a L'vov platform and added calcium. The analytical imprecision (CV) was less than or equal to 5.4% for aluminium concentrations between 12 and 98 micrograms/L, and analytical recoveries of added analyte varied between 94.5% and 103.0%. Detection limits (2 SD of determinations of the zero standard) were 7 and 6 pg for bone and soft tissues, respectively. Characteristic masses (amounts of Al yielding an absorbance signal of 0.0044 A) were 9 and 8 pg, respectively.