塞曼石墨炉AAS法直接测定硝酸银中的杂质

本文介绍了利用塞曼石墨炉原子吸收法直接测定硝酸银中的杂质锰、镍、铜、铁和铬。方法简单、快速、检出限低、回收率好。     

Aflatoxin Analysis by Reverse Phase HPLC Using Post-Column Derivatization for Enhancement of Fluorescence

Abstract

The application of a technique for the determination of aflatoxins by reverse phase HPLC and fluorescence detection incorporating post-column derivatization with iodine, is described. The procedure proved to be extremely sensitive and reproducible. Chromatograms of extracts from maize, peanut butter, sorghum malt and duckling mash are presented illustrating the value of the procedure for confirming the presence of aflatoxins B₁ and G₁.     

三种蒙药中微量元素含量与疗效相关性分析

用原子吸收分光光度计测定了蒙药扎木萨－4,阿拉坦－5,阿那日－5中多种微量元素及常量元素的含量。结果表明,这三种健胃消食蒙药中Mg、Fe、Mn、Zn均较高,呈一定相关性,而有害元素Pb、Cd很少,探讨了三种蒙药中微量元素与其疗效的关系。     

Sample introduction assisted by compressed air in flame furnace AAS: a simple and sensitive method for the determination of traces of toxic elements

The power of detection of flame AAS for the toxic elements Cd, Hg, Pb and Tl can be improved by 1–2 orders of magnitude by using flame furnace AAS. In flame-furnace AAS, liquid samples are introduced directly into a nickel tube located in the flame, in the simplest case through a ceramic thermospray capillary. Transportation of the samples is achieved by using compressed air only. Comparatively low detection limits are achieved by both beam injection flame furnace (BIFF-AAS) and thermospray flame furnace AAS (TS-FF-AAS). For TS-FF-AAS, a pressure of less than 20 kPa (<80 in. water) is required. The TS-FF-AAS technique is very simple, robust and cheap. The detection limits were 0.2–0.4 g L^–1 (Cd), 40–100 g L^–1 (Hg), 5–9 g L^–1 (Pb) and 4–14 g L^–1 (Tl), respectively, depending on the method, flow rate and sample volume used. Pb and Cd were found at concentrations of 0.1–2 and 0.005–0.3 g g^–1, respectively, in samples of various spices.Dedicated to the memory of Wilhelm Fresenius.     

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。     

微波消解石墨炉原子吸收光谱法测定钛白粉中铅

采用微波消解系统消解钛白粉样品，研究了各种酸的用量与不同消解程序对消解效果的影响，选择了微波消解的最佳工作条件。用平台石墨炉原子吸收光谱法测定样品中的铅，与常压酸消解法的结果作比较，结果基本一致。     

大承气颗粒剂中微量元素的溶出量分析

采用原子吸收光谱法测定了大承气颗粒剂中铅、砷、镉、 铬、铜和锌的含量及其在人工胃液和人工肠液中的溶出量。结果表明，大承气颗粒剂中微量重金属元素在人工胃液中的溶出量明显高于人工肠液中，其中铜、 锌的溶出百分率较其它元素高。     

快速原子吸收法测定蔬菜样品中微量铜

本文描述了蔬菜悬浮液直接进样非火焰原子吸收法测定微量钢的方法,讨论了样品的粉碎、匀浆及进样技术,研究了原子化温度程序等实验条件,并通过对各种蔬菜中微量铜测定的结果与常规法结果比较,确立了方法的可行性。     

Determination of mercury in soils and sediments by graphite furnace atomic absorption spectrometry with slurry sampling

A graphite furnace atomic absorption spectrometric procedure for the determination of mercury is presented, in which the samples are suspended in a solution containing hydrofluoric and nitric acids. Silver nitrate (4% m/v) and potassium permanganate (3%) are incorporated, in the order specified, and aliquots are directly introduced into the graphite furnace. A fast heating programme with no conventional pyrolysis step is used. The detection limit for mercury in a 125 mg ml⁻¹ suspension is 0.1 μg g⁻¹. Calibration is performed by using aqueous standards. The reliability of the procedure is proved by analysing certified reference materials.     

原子吸收法测定矿石中钴的不确定度评定

利用原子吸收光谱法评定了矿石中钴测定的不确定度,为质量控制提供有效、可靠的测量数据。结果表明,测量结果的不确定度由钴的质量浓度C0、称样质量m0、试液定容体积V等引入的不确定度分量组成,而主要分量是钴的质量浓度。     

石墨炉原子吸收法测定补钙剂和补锌剂中痕量镉

探讨了用塞曼效应石墨炉原子吸收法测定补钙剂和补锌剂中痕量镉,研究了石墨炉升温程序及基体改进剂对测定的影响。测定结果表明,采用塞曼效应扣背景的方法,以5μL1.0g／L硝酸钯作为基体改进剂,能够提高镉对温度的稳定性和分析的灵敏度,用标准曲线法测定镉,回收率的平均值高达96％o     

Preliminary Study of a Potential Post-Column Photodegradation Reaction Scheme for the Detection of Organophosphorus Compounds

Abstract

The photodegradation of organophosphorus compounds has been studied using triethylphosphate as a model compound, A 150 W xenon lamp was used in conjunction with ammonium peroxydisulfate to achieve high yields of orthophosphate in a 100-second irradiation time. The effects of the pH of the reaction medium and the initial concentrations of a peroxydisulfate and triethylphosphate on the extent of reaction were determined. A survey of potential interferences was performed, Copper (II) ion was found to catalyze the reaction, The effect of varying the Cu (II) concentration and the pH dependence of the catalyzed reaction were determined, Organic solvents were found to interfere with the photo degradation, but the reaction shows good potential for incorporation into a post-column detection system for the liquid chromatographic determination of organophosphorus compounds where totally aqueous mobile phases can be used.     

双硫腙-离子液体萃取-原子吸收光谱法测定复杂体系样品中锌

将离子液体1-丁基-3-甲基咪唑六氟磷酸盐和双硫腙螯合剂用于复杂体系样品中锌的萃取。用原子吸收光谱法测定复杂体系样品中的锌含量。选择测定波长为516nm。锌的质量浓度在0.1~2.0mg·L-1范围内与其吸光度呈线性关系,检出限(3s/k)为0.69μg·L-1。方法应用于硫酸锌口服液样品中锌的测定,测定结果与药典法测定值相符。用标准加入法对方法的回收率进行试验,测得回收率在98.5%~101%之间,测定值的相对标准偏差(n=5)在1.9%~2.8%之间。     

Dry ashing,sources of error,and performance evaluation in AAS

Three different stages of the analytical chain will be discussed. Firstly, the merits and demerits of the traditional dry ashing, a well established technique that is sometimes viewed with unwarranted sceptisism. Secondly, control of ashing temperature, background correction systems and autosampler volumes in AAS-determinations will be discussed. Thirdly, the role of intercalibrations and the use of reference materials will be discussed in terms of their limitations in providing information on analytical performance. Two ways to obtain more complete information on a laboratory's performance will be described.     

1990～1999年湛江市婴幼儿发中Zn、Fe、Ca含量的调查分析

报道了１９９０ ～１９９９ 年湛江市０ ～３ 岁婴幼儿发中Ｚｎ 、Ｆｅ 、Ｃａ 含量的调查分析。结果显示： ①Ｚｎ 、Ｆｅ 、Ｃａ 含量十年的总平均值分别为６９－６２ ×１０ － ６ 、３７－１１ ×１０ － ６ 、５１１－６８ ×１０ － ６ ; 三种元素含量均在１９９０ 年最低, Ｚｎ 、Ｆｅ 含量于１９９３ 年明显升高, Ｃａ 含量于１９９４ 年明显升高, 以后几年趋于平衡; ②０ ～０－５ 岁组的三种元素含量均明显高于其他年龄组（ Ｐ＜ ０－０１ ） , 在其他年龄组中Ｚｎ 、Ｃａ 含量有性别差异（ Ｐ＜ ０－０１ ） 。     

石墨炉原子吸收法直接测定全血中镉和铅

直接测定人体血镉和血铅较为困难。本文介绍用铂作基体改进剂以提高镉、铅的灰化温度,在灰化阶段除去产生高背景吸收的蛋白,而不发生镉、铅的挥发损失。实现了不需消化样品、络合提取等复杂的化学前处理,用石墨炉原子吸收法和校正曲线直接测定。同时应用衬钽技术,大大延长了石墨管的使用寿命。     

微波消解–石墨炉原子吸收光谱法测定84消毒剂中的痕量铅

建立了84消毒剂中痕量铅的微波消解–石墨炉原子吸收光谱测定方法。84消毒液以硝酸为消解试剂,用微波消解法进行消解。用2%磷酸二氢铵为基体改进剂,在优化后的仪器工作条件下测定。铅的质量浓度在0~80.0ng/mL范围内与吸光度呈良好的线性关系,线性相关系数r=0.999 3,方法检出限为0.005 4 mg/kg,平均回收率为94.66%,测定结果的相对标准偏差为1.87%(n=6)。该方法灵敏度与准确度高,可用于84消毒剂中痕量铅的检测。     

微波消解-石墨炉原子吸收光谱法测定鱼肉和河蚌中的重金属

建立微波消解样品,石墨炉原子吸收光谱法测定鱼肉和河蚌中重金属Pb,Cd,Cr,Cu,Ni含量的方法。优化了石墨炉原子吸收光谱法测定条件,在最佳实验条件下,选用磷酸二氢铵作为Pb,Cd,Cr,Cu的基体改进剂,抗坏血酸作为Ni的基体改进剂。Pb,Cd,Cr,Cu,Ni的检出限分别为0.05,0.01,0.05,0.05,0.07μg/g,实际样品测定结果的相对标准偏差为6.3%~14.5%(n=6),加标回收率为84.5%~113.0%。测定了牡蛎标准参考样,测定值在标准值可接受范围内。该方法检出限低、准确度高,适用于鱼类、河蚌样品中重金属含量的分析。     

Fluorescamine Post-Column Derivatization for the HPLC Determination of Cephalosporins in Plasma and Urine

Abstract

A post-column fluorescamine derivatization procedure is proposed for the determination of cephalosporins having an α-primary amino group in their side chain (cefaclor, cephalexin, cephradine, cefroxadine, cefaloglycine and cefadroxil). The linearity, repeatability and detection limits of fluorescence emission and UV absorption detection are compared under the same chromatographic conditions. Fluorescence detection is about two times more sensitive than UV absorption detection. Application to the determination of these cephalosporins in plasma and urine shows an improved selectivity by comparison with UV detection.     

酸枣根与酸枣仁中部分微量元素的比较研究

用乙炔火焰原子吸收分光光度法对酸枣根、酸枣仁中的八种微量元素进行了比较测定,对进一步研究其药理机制、综合利用酸枣资源提供了参考数据。