流动注射—氢化物—石墨炉原子吸收光谱法应用研究

本文采用自制的氢化物－石墨炉自动进样器及流动注射仪，直接测定了一些环境试样中的痕量锗，并研究了测定条件，该方法灵敏度高，线性范围宽，操作简单，速度快，耗样量少。特征质量：５．７ｐｇ／０．００４４Ａ；检出限：１．３ｐｇ，测定速度：３０个样／ｈ；回收率：９９．５％－１０４％。     

饮料食品中Ge－132和Ge~（4＋）含量测定研究

本文报告了在０．０１ｍｏｌ／ＬＣＴＡＢ体系中，以Ｆ－为掩蔽剂、苯芴酮显色、用分光光度法测定饮料食品中Ｇｅ－１３２含量，最低检测限０．０５４μｇ／ｍＬ；线性范围０．５４～２７．１４μｇ／ｍＬ；回收率９６．３％～１０１．５％，并确定了Ｇｅ－１３２摩尔吸收系数（ε）３．３９×１０４。用本法测定了康寿茶、矿泉水和博士奶中Ｇｅ－１３２含量，灵敏度高、重现性和准确度好。用盐酸化本体系，研究了二氧化锗（Ｇｅ~（４＋））的含量测定，其最低检测限０．０２１μｇ／ｍＬ；线性范围１．０～２１．０μｇ／ｍｌ；回收率９５．８％～１０２．８％，Ｇｅ－１３２不干扰。饮料食品中同时存在Ｇｅ－１３２和Ｇｅ（４＋）时，本体系可分别测定两者含量。     

新—阶导数双峰光谱法解析及应用──测定NO_3~－和NO_2~－

本文通过对ＮＯ３－和ＮＯ２－的一阶导数光谱研究，提出利用它们各自导致光谱峰值的两种解析方法测定相互干扰的两组份含量，由于利用尽可能最大信息量和导数谱的特有功能，使测定ＮＯ３－和ＮＯ２－灵敏度分别为０．００５μｇ／ｍＬ、０．００９μｇ／ｍＬ（峰高－截矩比ｆ校正系数法）及０．００４μｇ／ｍｌ、０．００６μｇ／ｍＬ（双峰ｋ系组合导致法），线性范围皆为０～１．０μｇ／ｍＬ方法用于水样分析，结果令人满意。     

病人血样中痕量锗,锶的石墨炉原子吸收光谱法测定

本文运用石墨炉ＡＡＳ法加基体改进技术，测定了５０岁以上病人血清及环境水样中锗和锶的含量。用０．０１ｍｏｌ／ＬＨＮＯ３－０．１％ＴｒｉｔｏｎＸ－１００稀释血清，测定精度可与火焰法媲美。锗，锶的特征量分别为２８ｐｇ和１８ｐｇ；线性范围为０－２５０ｎｇ／ｍＬ和－３５．０ｎｇ／ｍＬ；相对标准偏差（ｎ＝１０）４．１０％和２．４９％；回收率分别为９２．２％－９９．０％和９２．０％１０２％。方法快速准确，结果满     

石墨炉原子吸收光谱法测定人血及人发中的锗

研究了人体血液及人发中锗的测试方法，其中人发样品在密封罐中消化分解，血液用Ｔｒｉｏｎ Ｘ－１００以１：８稀释，以硝酸钯和硝酸铵混合溶液作为基体改进剂，用石墨炉原子吸收光谱法进行测定，在很大程度上提高了方法的灵敏度和抗干扰能力。方法特征值为２０ｐｇ，标准检出限为０．４５μｇ／Ｌ。样品加标回收率，血液１００．９％￣１０３．２％，发样９３．７％￣９７．２％，ＲＳＤ＝５．１％。     

新体系Co－H_2O_2－OCPF催化褪色光度法测定痕量钴的研究

本文研究了在碱性介质中，钴（Ⅱ）对过氧化氢氧化邻氯苯基荧光酮（ＯＣＰＦ）褪色反应，建立了催化光度法测定痕量钴的新方法。其检出限为８．２ｐｇ／ｍＬ，在０～３．５ｎｇ／ｍＬ范围内，钴（Ⅱ）与ｌｏｇ（Ａ＿０／Ａ）有良好线性关系。该指示反应灵敏度高选择性好，应用于维生素Ｂ＿（１２）和污水中钴的测定获得满意结果。     

流动注射停流—分光光度法同时测定痕量铝和铁

在弱酸性溶液中，基于铝、铁与铬天青Ｓ、溴化十六烷基吡啶形成蓝色三元络合物，采用两次标准加入法，建立了流动注射停流技术同时测定铝、铁的新方法。测定频率９０次／ｈ。铝、铁的线性范围分别为０－０．４ｍｇ／Ｌ，和０－０．８ｍｇ／Ｌ。应用于水及食品中痕量铝、铁的测定，结果满意。     

血清中铬、锰的GFAAS测定及其临床研究

本实验运用ＧＦＡＡＳ法采用热解涂层平台管，测定了血液病患儿、新生儿脐血以及老年组患者血清中铬和锰。用０．０１ｍｏｌ／ＬＨＮＯ３（含０．１％ＴｒｉｔｏｎＸ－１００）以１＋４（Ｖ＋Ｖ）稀释血清，测定的精密度可与火焰法媲美。铬锰检出限（ｐｇ／ｍＬ）分别为１３．８和６．９，回收率分别为９６．３％～１０３．３％和９７．０％～１０４．０％。以最佳实验条件测定了病患儿、新生儿及老年患者血清并以标准牛血清作方法检验，结果满意。     

钯作基体改进剂FIA－HG－GFAAS法测定锗及其机理研究

采用钯，钯－镁作基体改进剂，ＦＩＡ－ＨＧ－ＧＦＡＡＳ法成功地测定了锗。灵敏度、精密度和分析速度都得到很大的提高。峰值吸收的特征质量８．０ｐｇ，检出限１０．９ｐｇ，相对标准偏差０．３４％，同时探讨了基体改进剂钯的稳定作用机理及锗在石墨管中的原子化机理。     

钯作基体改进剂FIA—HG—GFAAS法测定锗及其机理研究

采用钯，钯－镁作基体改进剂，ＦＩＡ－ＨＧ－ＧＦＡＡＳ法成功地测定了锗。灵敏度，精密度和分析速度都得到很大的提高，峰值吸收的特征质量８．０ｐｇ，检出限１０．９ｐｇ，相对标准偏差０．３４％，同时探讨了基体改进剂钯的稳定作用机理及锗在石墨管中的原子化机理。     

Simultaneous Determination of Aluminum,Cadmium and Lead in Whole Blood by Simultaneous Atomic Absorption Spectrometry with Oxygen Charring

A method for the simultaneous determination of aluminum (Al), cadmium (Cd) and lead (Pb) in whole blood has been developed by using simultaneous atomic absorption spectrometry (SIMAAS) with oxygen charring. The optimized conditions for the simultaneous determination of Al, Cd and Pb were obtained in the presence of palladium (Pd) as the chemical modifier, using 600 °C and 2400 °C as the pyrolysis and the atomization temperature, respectively. The whole blood samples were diluted 1+5 (v/v) directly with 0.1% (v/v) Triton X‐100. Oxygen was employed to eliminate the interference of carbonaceous residues in the charring step before pyrolysis. The calibration curves were carried out with aqueous standard solutions and the linear ranges were 0–40 ng mL⁻¹, 0–4 ng mL⁻¹ and 0–40 ng mL⁻¹ for Al, Cd and Pb, respectively. The detection limits were 0.96 ng mL⁻¹ (19.2 pg) for Al, 0.03 ng mL⁻¹ (0.6 pg) for Cd and 0.60 ng mL⁻¹ (12.0 pg) for Pb. The spiked recoveries of Al, Cd and Pb in whole blood were 98.0%, 100.0% and 101.7%, respectively. The accuracy of the proposed method was evaluated with the analysis of a whole blood certified reference material (Seronorm, level 2). The found concentrations were in agreement with the recommended values. The proposed method has been successfully applied to the simultaneous determination of Al, Cd and Pb in whole blood of healthy volunteers before and after eating barbecued foods.     

石墨炉原子吸收法测定钒的研究

本文比较了在标准石墨管,热解涂层和全热解石墨管中钒的吸收信号形状。用全热解石墨管和EDTA铵盐作基体改进剂,直接测定水系沉积物中痕量钒。方法的特征量为61pg/0.0044A。     

DBM—MSA光度法测定化妆品中铅

为建立一个新的测定化妆品中铅的分光光度法,在0．24mol／L的磷酸介质中,铅与DBM—MSA{3-[（2-磺酸基苯）偶氮]-6-[2,6-二溴-4-甲基苯）偶氮]-4,5-二羟基-2,7-萘二磺酸}反应形成1：2的蓝色配合物,在波长630nm处比色测定。结果表明,铅量在0—1μg／mL范围内符合比耳定律;样品测定的相对标准偏差为1．24％～4．59％,标准加入回收率为95．0％～107．0％,化妆品中共存物质不干扰测定,方法简便,选择性好,结果满意。     

The determination of lead in blood by atomic fluorescence flame spectrometry

The use of atomic flame fluorescence for the direct determination of lead in diluted blood is described. The method is sensitive enough to determine the lead concentration in 20× diluted blood accurately and with a precision of better than 4% at a lead concentration level of 0.20 μg ml^-1. A special design of hollow cathode lamp is used, with an argon-hydrogen-oxygen flame. Sodium interference is compensated by addition to standards, and light scatter effects are eliminated by a simple filter. Linear response to lead concentration is obtained in the range 0–40 μg ml^-1.     

石墨探针—原子吸收光谱法测定人发中痕量铟的研究

探针原子化技术是一种实现等温原子化,改善灵敏度的行之有效的方法。本文采用此方法对痕量钿进行了一系列条件试验,峰面积与钿浓度在0～50ng·ml~(-1)范围内呈线性关系,其特征量4.8pg,检出限21.5pg,相对标准偏差5.7％,并成功地测定了成人发中铟的含量,范围在12～159pg·g~(-1),回收率96.4％～103.2％。该方法灵敏度高,操作简单、快速,结果满意。     

Application of tertiary amines for arsenic and selenium signal enhancement and polyatomic interference reduction in ICP-MS analysis of biological samples

Water soluble tertiary amines enhance signals and decrease polyatomic chloride interferences in the direct inductively coupled plasma – mass spectrometric (ICP-MS) determination of As and Se in biological samples. Preliminary experiments with amine concentrations and nebulizer flow rates produced element and interference signal intensity changes. Arsenic and Se ICP-MS determination parameters have been optimized by a simplex procedure with amines in an argon plasma or without amines but with addition of N₂ to the Ar. Variables include RF (radio frequency) power, nebulizer gas flow rate, intermediate gas flow rate, and amine concentration or nitrogen gas flow rate. Detection limit, minimization of polyatomic ion intensities, and reproducibility have been evaluated as reponse factors. The signal enhancement and element-to-molecular interference ratios differ to some extent with analyte intensity optimum operating conditions. The detection limits with addition of nitrogen (16 pg mL^–1 for As and 180 pg mL^–1 for Se) or of amines (8 pg mL^–1 for As and 120 pg mL^–1 for Se) and the extent of chloride interference minimization were compared. Amines addition was more beneficial. Biological standard reference materials and food and fecal samples were analyzed following different sample dissolution procedures.     

微波消解-电感耦合等离子体质谱测定大气颗粒物中痕量稀土元素

研究了电感耦合等离子体质谱（ICP-MS）测定大气颗粒物中痕量稀土元素（REEs）的分析方法。在微波条件下,采用HNO3 ＋ H2O2（3 ＋ 1）混合介质能快速而有效地分解颗粒物样品。详细讨论了测定稀土元素的质谱干扰。通过分析不同粒径颗粒物中稀土元素的含量,初步探讨了大气颗粒物中稀土元素的分布规律。结果表明：颗粒物试样的粒径越小,稀土元素的含量越高。分析方法的检出限为0．7～2．8pg／mL,用于大气颗粒物国际标样（SRM 1648）中稀土元素分析,结果与推荐值有良好的一致性。     

High throughput screening of sub-ppb levels of basic drugs in equine plasma by liquid chromatography-tandem mass spectrometry

This paper describes a high throughput LC-MS-MS method for the screening of 75 basic drugs in equine plasma at sub-ppb levels. The test scope covers diversified classes of drugs including some alpha- and beta-blockers, alpha- and beta-agonists, antihypotensives, antihypertensives, analgesics, antiarrhythmics, antidepressants, antidiabetics, antipsychotics, antiulcers, anxiolytics, bronchodilators, CNS stimulants, decongestants, sedatives, tranquilizers and vasodilators. A plasma sample was first deproteinated by addition of trichloroacetic acid. Basic drugs were then extracted by solid-phase extraction (SPE) using a Bond Elut Certify cartridge, and analysed by LC-MS-MS in positive electrospray ionization (+ESI) and multiple reaction monitoring (MRM) mode. Liquid chromatography was performed using a short C(8) column (3.3 cm L x 2.1mm ID with 3 microm particles) to provide fast analysis time. The overall instrument turnaround time was 8 min, inclusive of post-run and equilibration time. No interference from the matrices at the expected retention times of the targeted masses was observed. Over 60% of the drugs studied gave limits of detection (LoD) at or below 25 pg/mL, with some LoDs reaching down to 0.5 pg/mL. The inter-day precision for the relative retention times ranged from 0.01 to 0.54%, and that for the relative peak area ratios (relative to the internal standard) ranged from 4 to 37%. The results indicated that the method has acceptable precision to be used on a day-to-day basis for qualitative identification.     

Determination of total gaseous lead in the atmosphere by honeycomb denuder/electrothermal atomic absorption spectrometry.

A technique is described for the determination of total gaseous lead in the atmosphere by honeycomb denuder collection, followed by an electrothermal atomic absorption spectrometry (ETAAS) measurement. The collection efficiency of the honeycomb denuder in which a solution containing 2% HNO3/2% glycerine/1% ammonium dihydrogenphosphate was coated for trapping the gaseous lead in the atmosphere was 98.8%. The linear absorbance response was obtained for a concentration range of 0-1.39 microg m(-3) of lead in the atmosphere. A precision of 4.8% RSD (peak-height absorbance, n = 11) for an aqueous solution of 1 ng of lead standard, characteristic masses (CM) of 23 pg and detection limit (3sigma) of 54 pg for an aqueous solution of 0.01 ng lead standard was achieved with 100 microg ammonium dihydrogenphosphate as a chemical modifier. The average recovery of lead in three standard samples prepared by the independent digestion of NIST SRM 1648 (Urban Particulate Matter) using our analytical system was 97.8%. The total content of the gaseous lead in the atmosphere of our laboratories was 0.35-0.38 microg m(-3).     

顺序注射氢化物发生-原子荧光光谱法同时测定中草药中的铅和锡

建立了一种顺序注射氢化物发生一原子荧光光谱法同时测定中草药中的铅和锡含量的方法,同时讨论了共存离子的干扰情况。结果表明,在最佳实验条件下,铅和锡的检出限分别为0．0253μg／L和0．0425μg／L,加标回收率为95．5％～103．1％,相对标准偏差小于5．2％,被测试样中共存的离子对铅和锡的测定没有干扰。该法操作方便、快速,用于中草药试样中铅和锡的同时测定,具有很好的可行性和实用性。