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本文基于肾上腺素、去甲肾上腺素和多巴胺对鲁米诺-铁氰化钾化学发光体系的增敏作用,建立了一种高效液相色谱分离-化学发光检测体系同时检测三种物质;研究了试剂浓度、酸碱条件、流动相成分等参数对分析结果的影响。在优化发光条件下,以邻苯二甲酸氢钾-甲醇溶液(92:8)为色谱流动相,用C18柱分离检测肾上腺素、去甲肾上腺素和多巴胺样品,肾上腺素线性范围为1×10-8~5×10-6g/mL,检测限4.0×10-9g/mL;去甲肾上腺素线性范围是 5.0×10-9~1.0×10-6g/mL,检测限1.0×10-9g/mL;多巴胺线性范围为5.0×10-9~1.0×10-6g/mL,检测限8.0×10-10g/mL。本方法快速、简便而准确,且已成功用于血清中三种物质的分析。 相似文献
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发现了盐酸氯丙嗪在K3Fe(CN)6-钙黄绿素化学发光反应体系中的后化学发光反应,优化了反应条件,建立了一种利用后化学发光反应测定盐酸氯丙嗪的流动注射化学发光分析法.方法的检出限为3×10-8/mL,相对标准偏差为2.0%(2.0×10-6 g/mL盐酸氯丙嗪,n=11),线性范围为1.0×10-7~1.0×10-5 g/mL.此法已用于盐酸氯丙嗪片剂中盐酸氯丙嗪含量的测定,结果与药典方法测定值一致. 相似文献
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流动注射-化学发光法测定盐酸地尔硫卓 总被引:1,自引:0,他引:1
发现了盐酸地尔硫卓在过硫酸钾-鲁米诺化学发光反应体系中的后化学发光反应.据此发现建立了利用后化学发光反应测定盐酸地尔硫卓的流动注射化学发光新方法.方法的线性范围为3.0×10-6~1.0×10-4 g/mL,检出限为3×10-7 g/mL,对6.0×10-5 g/mL的盐酸地尔硫卓标准溶液进行11次平行测定的相对标准偏差为1.6%.方法已用于盐酸地尔硫卓片剂中盐酸地尔硫卓含量的测定. 相似文献
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《化学研究与应用》2016,(11)
本文建立了以铁氰化钾-Fe(Ⅲ)体系测定盐酸异丙肾上腺素的方法。研究表明,在pH 3.0,盐酸异丙肾上腺素可使Fe(Ⅲ)还原为Fe(Ⅱ),生成的Fe(Ⅱ)可以与K_3[Fe(CN)_6]反应生成可溶性普鲁士蓝(KFe~(Ⅲ)[Fe~(Ⅱ)(CN)_6)。盐酸异丙肾上腺素的浓度在0.03~5.00μg·m L~(-1)范围内与吸光度呈现良好线性关系,线性回归方程A=0.017+0.57779C(μg·m L~(-1)),相关系数R=0.9997,检出限为0.025μg·m L~(-1),相对标准偏差R.S.D.=1.05%(n=11),间接测定盐酸异丙肾上腺素的摩尔吸光系数ε=1.4×105L·mol~(-1)·cm~(-1)。本方法成功用于药物制剂和生物样品中盐酸异丙肾上腺素含量的测定,结果满意。 相似文献
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研究了高锰酸钾-Ⅰ--甲醛体系化学发光,从而建立了一种测定微量Ⅰ-的新方法.讨论了各种反应物浓度、酸度、干扰离子等因素对测定结果的影响.Ⅰ-浓度在1.0×10-6~4.0×10-5g/mL范围内与化学发光强度有较好的线性关系.对1.0×10-5g/mL的Ⅰ-进行了11次平行测定,相对标准偏差为2.8%,方法的检出限为2.4×10-8g/mL.结果令人满意. 相似文献
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IR and Raman spectra of [Mo2O2S2(S2)2]2- were reported. The resonance Raman spectra and the depolarization ratios in CH3CN solution were measured. By using the data of crystal structure, the simplified normal coordinate calculation of the stretching vibrations for anion [Mo2O2S2(S2)2]2- was performed. The results obtained are useful to assign the vibrational bands of some Mo-Fe-S clusters. 相似文献
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I. A. Topol A. S. Chesnyi V. M. Kovba N. F. Stepanov 《Theoretical chemistry accounts》1982,61(4):369-377
The SCF-X
-SW method in an overlapping atomic spheres approximation has been used to calculate the electronic structure, ionization potentials, energies and oscillator strengths of the allowed optical transitions and also some of the one-electron properties of the MoO2Cl2 molecule. The electronic absorption spectra of vapours over molybdenum and tungsten dioxodibromides have been measured. Interpretation of the experimental electronic absorption spectra of the MoO2Cl2, MoO2Br2 and WO2Br2 molecules is discussed. 相似文献
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4-Hydroxy-2H-chromen-2-one and 4-hydroxy-2H-chromene-2-thione reacted with allyl bromide, 1,1,3-trichloroprop-1-ene, and 1,3-dichlorobut-2-ene to give the corresponding ethers, which were oxidized to (2-oxo-2H-chromen-4-yloxy)acetic acid with potassium permanganate, and various derivatives of that acid were obtained. 3-(3,3-Dichloroprop-2-enyl)-7-hydroxy-4-methyl-2H-chromen-2-one and 3-(3,3-dichloroprop-2-enyl)-7-hydroxy-4-methyl-2H-chromene-2-thione were synthesized, and some their transformations were studied. 相似文献
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When bromoform (CHBr3) is photolyzed at 266 or 303 nm in the presence of O2 and NO, the formation of secondary Br atoms is observed. By following the rate of growth of this secondary Br atom signal as a function of conditions, rate constants have been determined for the reactions CHBr2 + O2, CHBr2 + NO (both pressure-dependent), and CHBr2O2 + NO (k(2a) = (1.74 +/- 0.16) x 10(-11) cm3 molecule(-1) s(-1) at 23 degrees C). By measuring the amplitude of the secondary Br signal compared to the primary Br formed in the initial photolysis, it is established that the CHBr2O radical spontaneously decomposes to form CHBrO + Br at least 90%, and probably 100%, of the time, in agreement with previous work and with recent ab initio calculations. A survey of four other polybrominated methanes, CH2Br2, CHClBr2, CF2Br2, and CBr4, shows that they all generate secondary Br atoms when photolyzed at 266 nm in the presence of O2 and NO, suggesting that their reaction sequences are similar to that of bromoform. 相似文献
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The mechanism of reaction CI2+2HBr=2HCI+Br2 has been carefully investigated with density functional theory (DFT) at B3LYP/6-311G** level. A series of three-centred and four-centred transition states have been obtained. The activation energy (138.96 and 147.24 kJ/mol, respectively) of two bimolecular elementary reactions CI2+HBr→HCI+BrCI and BrCI+HBr→HCI+Br2 is smaller than the dissociation energy of CI2, HBr and BrCI, indicating that it is favorable for the title reaction occurring in the bimolecular form. The reaction has been applied to the chemical engineering process of recycling Br2 from HBr. Gaseous CI2 directly reacts with HBr gas, which produces gaseous mixtures containing Br2, and liquid Br2 and HCI are obtained by cooling the mixtures and further separated by absorption with CCI4. The recovery percentage of Br2 is more than 96%, and the CI2 remaining in liquid Br2 is less than 3.0%. The paper provides a good example of solving the difficult problem in chemical engineering with basic theory. 相似文献
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Stéphanie Ricol Etienne Vernaz Philippe Barboux 《Journal of Sol-Gel Science and Technology》1997,8(1-3):229-233
Gels have been synthesized in the SiO2-Na2O-ZrO2 system and calcined at various temperatures up to 700°C. They have been studied by infrared absorption spectroscopy. The position of the asymmetric stretching frequency of the SiO4 unit is used as a tracer of the homogeneity. It is shown that sodium increases the solubility of zirconium in the silica matrix as already observed in fused glasses. 相似文献
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Computations predict that H2O will shift rapidly between the carbons of \documentclass{article}\pagestyle{empty}\begin{document}$ \mathop {\rm C}\limits^{\rm .} {\rm H}_2 {\rm CH}_2 \mathop {\rm O}\limits^ + {\rm H}_2 $\end{document} over most of the energy range between the threshold for formation of the ion and the onset of its decomposition. This prediction is important to understanding the relationships and contrasts between the chemistries of free radicals and carbonium ions. We present experimental evidence that the theoretical predictions are correct. 相似文献