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22.
Meng Wang Weiyue Feng Junwen Shi Fang Zhang Bing Wang Motao Zhu BaiLi Yuliang Zhao Zhifang Chai 《Talanta》2007,71(5):2034-2039
A mild, efficient and convenient extraction method of using 2-mercaptoethanol contained extractant solution combined with an incubator shaker for determination of mercury species in biological samples by HPLC–ICP-MS has been developed. The effects of the concentration of 2-mercaptoethanol, the composition of the extractant solution and the shaking time on the efficiency of mercury extraction were evaluated. The optimization experiments indicated that the quantitative extraction of mercury species from biological samples could be achieved by using 0.1% (v/v) HCl, 0.1% (v/v) 2-mercapoethanol and 0.15% (m/v) KCl extractant solution in an incubator shaker for shaking overnight (about 12 h) at room temperature. The established method was validated by analysis of various biological certified reference materials, including NRCC DOLT-3 (dogfish liver), IAEA 436 (tuna fish), IAEA MA-B-3/TM (garfish filet), IAEA MA-M-2/TM (mussel tissue), GBW 08193 (bovine liver) and GBW 08572 (prawn). The analytical results of the reference materials were in good agreement with the certified or reference values of both methyl and total mercury, indicating that no distinguishable transformation between mercury species had occurred during the extraction and determination procedures. The limit of detection (LOD) for methyl (CH3Hg+) and inorganic mercury (Hg2+) by the method are both as 0.2 μg L−1. The relative standard deviation (R.S.D.s) for CH3Hg+ and Hg2+ are 3.0% and 5.8%, respectively. The advantages of the developed extraction method are that (1) it is easy to operate in HPLC–ICP-MS for mercury species determination since the extracted solution can be directly injected into the HPLC column without pH adjustment and (2) the memory effect of mercury in the ICP-MS measurement system can be reduced. 相似文献
23.
六极杆碰撞反应池-等离子体质谱测定生物样品中痕量铬和钒 总被引:1,自引:0,他引:1
采用带六极杆碰撞反应池的电感耦合等离子体质谱直接测定了生物样品中痕量铬和钒。在碰撞反应池中引入He/NH3(93∶7)混合气,有效地消除了分子离子(ArC 、NCl 、Cl O 、Cl OH 等)对超痕量铬、钒测定的干扰,降低了方法的检出限。比较了干法灰化和湿法消解两种样品处理方法,两种消解方式获得的结果基本一致。方法的检出限(3σ):钒为0.005 0μg.g-1,铬为0.001 8μg.g-1。相对标准偏差:钒为3.25%~14.08%;铬为4.20%~8.24%。经国家一级生物标准物质验证,测定值与标准值吻合。 相似文献
24.
建立了生物材料中克伦特罗 (clenbuterol)的气相色谱 -质谱测定方法 ;大白鼠喂食克伦特罗获得阳性生物材料 ,生物材料中克伦特罗经0.01mol/L盐酸溶液提取 ,乙醚脱脂净化 ,乙酸乙酯提取后蒸发至干 ,用乙醇溶解后加样到氧化铝柱上 ,用0.01mol/L盐酸溶液洗脱 ,蒸发至干后 ,用BSTFA(双三甲基硅烷基三氟乙酰胺 ) +1 % (φ)TMCS(三甲基氯硅烷 )衍生 ,采用GC -MS进行测定 ,外标法定量 ;试验表明 ,生物材料中添加0.056×10 -6~0.54×10 -6(w)含量水平的克伦特罗 ,方法回收率在89 %~107 % ,相对标准偏差为7.3 %~16 % ,线性相关系数r为0.998,克伦特罗的检出限为2.0×10-9(w)。 相似文献
25.
A novel method for the determination of trace amounts of Al(III) based on resonance Rayleigh scattering (RRS) has been developed. In the presence of some surfactants, Al(III) can react with morin and form an Al(III)-morin-surfactant complex, which results in the enhancement of RRS intensity and the appearance of the corresponding RRS spectral characteristics. Their maximum scatter peaks are at 476 nm for the cetyltrimethylammonium bromide (CTAB) system, 489 nm for the cetylpyridinium chloride (CPC) system, 474 nm for the Triton X-100 system, and 473 nm for the Tween-20 system. The enhanced RRS intensity is directly proportional to the concentration of Al(III). The detection limits are in the range of (0.50-1.2)×10−7 mol l−1 depending on the surfactant. The characteristics of RRS spectra of the complexes, the optimum conditions of these reactions and the influencing factors have been investigated. The method has high selectivity, and was successfully applied to the determination of Al(III) in natural and biological samples. Furthermore, according to different complexation capacity of Al(III)-morin-CTAB system under two pH conditions, speciation analysis of Al(III) in natural waters was explored. The labile monomeric Al fraction (mainly inorganic Al, Ali) is determined at acidic pH and the total monomeric Al fraction (Ala) is determined at alkaline pH. The results are in agreement with those obtained by Driscoll’s 8-hydroxyquinoline extraction-ion exchange method. 相似文献
26.
硅基甲硫醇R^1R^2CH3SiCH2SH与O,O-二烷基二硫代磷酸酯(RO)2P(S)SH及甲醛可顺利地发生类Mannich缩合反应,利用此反应和硅基甲硫醇与O,O-二乙基-S(2-溴乙基)二硫代磷酸酯的取代反应合成了37种新的含硅二硫代到酯化合物(RO)2P(S)S(CH2)nSCH2SiCH3R^1R^2(n=1,2),在初筛浓度下,该类化合物具有一定的杀虫,杀螨活性。 相似文献
27.
Magno Aparecido G. Trindade Glaucia Maria da Silva Valdir Souza Ferreira 《Microchemical Journal》2005,81(2):209-216
This work presents an electroanalytical methodology developed for square-wave voltammetry based in the electrochemical reduction in hanging mercury drop electrode (HMDE), which is simple, fast, reliable and sensitive for determination of moxifloxacin (MOXI) in tablets and spiked urine human samples. The support electrolyte that provided a more defined and intense peak current for MOXI determination was the phosphate buffer 0.04 mol l− 1 pH 8.0. In the best-optimized conditions the drug presented an only peak of reduction at − 1.38 V vs. Ag/AgCl, using an Eacc. of − 0.30 V. An LOD of 0.44 and 3.20 ng ml− 1 and an LOQ of 1.46 and 10.60 ng ml− 1 were found for the pure standard of moxifloxacin and in the presence of matrix, respectively. A good recovery was obtained for assay spiked urine samples and a good quantification of MOXI was achieved in a commercial formulation. The methodology proposed was more sensitive than the spectrofluorimetric and spectrophotometric method with precision and accuracy equivalent. 相似文献
28.
Summary A fully integrated chromatographic system was developed for the determination of leukotrienes in biological samples using
photodiode-array detection (PDAD), which eliminates time consuming manual sample handling steps. A special solid phase extraction,
(SPE) methodology for leucotriene metabolite stability was developed which increased the recoveries and eliminates the contamination
risk of biological samples. The inherent instability (autooxidation) of many of the leukotriene mediators, and the adsorption
effects onto exposed surfaces in vials and in the chromatographic system were found to be very important parameters to control
in order to circumvent high loss of sample analytes. By binding the cell supernatants to the functionalities of the SPE support
stabilised these mediators. Cell culture samples were eluted through a disposable C18 SPE column. The SPE columns were allowed to thaw and deposited in an automated sample handling unit (ASPEC XL). Desorption
of the analytes was followed by a second on-line SPE step, to eliminate remaining interfering matrix compounds. Typical recoveries
when stored at −70°C were in-between 55–97% except for (LTE4) which was found to be around 40% after 72 days of storage. Seven reversed-phase packings were studied. Selectivity factors,
as well as the separation efficiencies, were found to differ for the various C18 bonded silica stationary phases. This integrated on-line column liquid chromatographic system was applied to the determination
of leukotriene B4, leukotriene C4, leukotriene D4, leukotriene and E4 in human cell extracts using prostaglandin B2 as the internal standard. More than 1500 biological samples were analysed. Some validation data are presented for unattended
operations. 相似文献
29.
用(RCp)2MCl2和(RCp)TiCl3(R=H,Me;M=Ti,Zr)分别与具有生物活性的2-甲氧基-5-氟尿嘧啶、2-甲硫基-5-氟尿嘧啶在甲苯溶剂中110℃下反应,合成了20个未见报道的(RCp)·M(Opm)2Cl、(RCp)2M(OPm)Cl和(RCp)M(OPm)Cl2(OPm=2-甲氧基-5-氟尿嘧啶基,2-甲硫基-5-氟尿嘧啶基)型钛锆配合物,这些配合物均经元素分析、1HNMR、IR光谱鉴定.初步动物试验表明,配合物1、4、11、14对小白鼠移植性艾氏腹水场的抑制作用居首,而配合物2、3、5、6、12、13、15、16次之,其它锆配合物几乎没有抑制作用。 相似文献
30.
A review of sample preparation methods for organic acids in biological fluids, in particular serum and urine, is presented. It covers techniques on organic acid determination without sample preparation, release of organic acids from binding locations, removal of proteins by protein precipitation and ultrafiltration, isolation of the organic acids by liquid-liquid and liquid-solid extraction, purification of the extract, derivatization and pre-fractionation. The various alternative sample preparation steps are compared and critically discussed. Examples of applications including profile analysis of organic acids by gas chromatography (GC), determination of particular organic acids by GC or liquid chromatography and determination of fatty acids as a distinct chemical class of acids demonstrate that the kind of sample preparation chosen depends strongly on the analytical aims. 相似文献