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41.
42.
Summary Nickel dithiocarbamate complexes derived from some sympathomimetic drugs are examined on silica Radial-Pak columns using binary solvents containing a small percentage of an organic polar modifier. Both the type and concentration of this modifier was found to influence the separation of the ternary from the parent binary complexes. When the two ligands in a ternary complex are racemic to each other, separation of the ternary complex is only possible when certain structural requirements of the molecule are fulfilled. Ternary complexes which contain structurally similar, but nonracemic ligands, are shown to be readily separated from binary complexes. When two such complexes differ only in that one of the ligands in one is enantiomeric to a ligand in the second complex, then it can be shown that the ternary complex with the (+) enantiomer ligand elutes faster from the silica column than the one with the (–) enantiomer ligand. An example of the use of ternary complexes for the identification of optical and structurally related impurities in pharmaceutical products is also given. 相似文献
43.
A new procedure for determining nitrogenated bases by forming ion pairs with Fe(SCN)63– is studied. The method consists of extracting the ion pair formed by a nitrogenated base and the inorganic complex Fe(SCN)63– into an organic phase, and measuring the iron in the organic phase by AAS at 248.3 nm. The optimal experimental conditions for determining amylocaine, avacan, bromhexine, diphenhydramine and papaverine are studied. The organic phase used is 1,2-dichloroethane. The standard deviation of the method varies between 10–1 and 10–2. The interferences produced by various substances are studied. 相似文献
44.
This paper reports the development of a method based on capillary electrophoresis with laser-induced fluorescence detection for the simultaneous determination of thiouracil (TU) and phenylthiouracil (PhTU) with high sensitivity (nanomolar range, i.e., attomoles detected). After derivatization with 5-iodoacetamidofluorescein, the analytes were separated by capillary zone electrophoresis using 20 mM phosphate buffer (pH 10.0) and quantified by fluorescence detection. The linearity range, precision, recovery, and detection limits were determined, and the method was shown to be applicable for the determination of TU and PhTU in spiked feed samples and urine. 相似文献
45.
气相色谱法测定蔬菜中有机磷农药的残留量 总被引:8,自引:1,他引:8
采用DB-1型毛细管柱及氮磷检测器,建立了同时测定蔬菜中有机磷农药甲胺磷、氧化乐果、甲拌磷、甲基对硫磷残留量的气相色谱法,测定4种有机磷农药残留量的线性范围均为0.02-4.00mg/L,相关系数为0.9955~0.9980,检出限为0.0012~0.0020mg/L,加标回收率为89.3%-92.2%,相对标准偏差为2.2%~3.2%。 相似文献
46.
47.
An automated sample pretreatment of human blood plasma for liquid chromatographic determination of three antidepressant drugs, dibenzepine; a tricyclic antidepressant (TCA), reboxetine; a selective noradrenaline reuptake inhibitor (SNRI) and fluvoxamine; a selective serotonin reuptake inhibitor (SSRI), based on supported liquid membrane (SLM) for unsurpassed sample clean-up and analyte enrichment, has been developed. The chromatograms after enrichment of plasma blank and aqueous blank are virtually indistinguishable. The entire analytical procedure revealed good linearity and low detection limits of 5, 15 and 20 ng mL–1 for dibenzepine, reboxetine and fluvoxamine, respectively. No carry-over effects were noted. The repeatability of extraction at three concentrations in the range 40–150 ng mL–1 for the three drugs was between ca. 3% and 7% as relative standard deviation. The reproducibility relative standard deviation during three different days (replacing the membrane each day) was not significantly higher. 相似文献
48.
49.
土壤中绿黄隆残留量分析方法的研究 总被引:2,自引:0,他引:2
本文确立了土壤中绿黄隆残留量的间接气相色谱分析方法,用0.15mol/L NaHCO3提取土样,二氯甲烷洗涤初步纯化后,在水浴上加热水解,再用二氯甲烷萃取,弗罗里硅土柱净化,最后用气相色谱-电子捕获检测器检测水解产物邻氯苯磺酰胺。土壤中添加回收率78.5%-90.8%,检测极限0.3ng/g。 相似文献
50.
The mass resolution of a time-of-flight (TOF) mass spectrometer is directly proportional to its total flight pathlength. Multi-turn or multi-passage ion optical geometries are necessary to obtain fight distances of sufficient length within reasonable size limitations. We have investigated ion optics for a multi-turn TOF mass spectrometer with electrostatic sectors. The concept of 'perfect' focusing conditions is introduced. Furthermore, a new type of multi-turn TOF mass spectrometer, the MULTUM Linear plus, was developed. It consists of four cylindrical electric sectors and 28 electric quadrupole lenses. It has a vacuum chamber 60 x 70 x 20 cm in size. Mass resolution is demonstrated to increase according to the number of ion cycles. A mass resolution of 350 000 (m/z = 28, FWHM) was achieved after 501.5 cycles. The MULTUM Linear plus analyzer is not simple, however; 28 electric quadrupole lenses are used. In order to reduce the number of ion optical parts, an improved multi-turn TOF mass spectrometer, the MULTUM II, consisting of only four toroidal electric sectors, was also developed. The possibility of tandem mass spectrometric applications using multi-turn TOF mass spectrometers is also discussed. 相似文献