分光光度法研究氨基酸与四氯苯醌形成的荷移配合物

本文用分光光度法研究了5种氨基酸与四氯苯醌形成的荷移配合物.通过对影响配合物形成因素的研究,确立了以四氯苯醌形成荷移配合物的方法测定氨基酸的最佳反应条件,测定了反应平衡常数.讨论了配合物的组成.     

5-[(偶氮苯基)偶氮]-8-氨基喹啉的合成、性质及其应用的研究

本文报道了新试剂5-[(偶氮苯基)偶氯]-8氨基喹啉的合成方法。研究了该试剂的理化性质,分析性能及其与钯显色反应的条件。从而拟定了直接分光光度法测定微量钯的新方法,结果满意。     

氧氟沙星的荷移分光光度法测定

研究了氧氟沙星与７，７，８，８－四氰基对二次甲基苯醌（ＴＣＮＱ）的荷移反应，确定了反应的最佳条件，在甲醇－丙醇（３：２）介质中，二者于３０℃水浴中恒温３０ｍｉｎ即可形成１：１络合物，在测定波长７４３ｎｍ处络合物的表观摩尔吸光系数为３．５８×１０＾４Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，氧氟沙星浓度在０～１５ｍｇ／Ｌ范围内符合比尔定律，方法的相对标准差小于３％。     

Spectrophotometric Assay of Certain Aminoglycosoide Antibiotic Using Chloranil

Abstract

Chloranil (2,3,5,6-teterachloro-p-benzoquinone) reacts with certain aminoglycosoide antibiotics in borate buffer at pH 9.0 to give charge-transfer complexes. The complexes possese an absorption maxmum at about 350 nm with molar absorptivities of 3.78 × 10⁵, 4.69 × 10⁵, 5.0 × 10⁵ and 7.08 × 10⁵ for kanamycin, neomycin B, amikacin and tobramycin reepectively, These high intensity of the chargetransfor band and confirmity to beer's law enabled assay of these antibiotics with appreciable sensitivity and good precision.

Aminoglycosoide antibiotics have a broad spectrum of activity against both gram-negative and gram-positive bacteria.

The official compendia^1,2 recommend the microbiological assay for their evalution. The high experimental errors in microbiological estimation heae been reported³. Numerous spectrophotometric, fluorometric and chromatographic techniques for their quantitation have been thoroughly reviewed^4,5.

Substituted quinones such as 2,5 dichloroquinone⁶, 7,7,8,8-tetracyanoqulnone dimethane⁷, flouranil⁸ are used as TT- acceptors with various electron donors to form charge-transfer(CT) complexes and radical ions^9,10. Some aromatic amines^11,12 and aminoacids have been determined with chloranil^13–15.

The present work describes the utility of chloranil for the spectrophotometric determination of kanamycin sulphate, amikacin sulphate tobramycin aulphate, and neorycin B sulphate (framycetine sulphate) either in bulk or in their reepective doaage forms.     

5—（4—乙酰胺基苯偶氮）—8—氨基喹啉荧光光度法测定微量铜（Ⅱ）

用本实验室首次合成的5-(4-乙酶胺基苯偶氮)-8-氨基喹啉(AAPAQ)荧光光度法测定微量铜(Ⅱ)。在Tween-80存在下,试剂与铜(Ⅱ)在pH9.8～10.8的硼砂缓冲溶液中形成淡黄色络合物。在λ_(em)/λ_(ex)=414nm/334nm处产生强荧光。此体系对铜(Ⅱ)的测定的线性范围是4～36ng/ml,检测下限为1ng/ml。此外,本文还探讨了H_2O_2对体系的增敏机理。     

5-(4-Carboxylphenylazo)-8-aminoquinoline as an analytical reagent for the spectrophotometric determination of gold

The synthesis and analytical application of 5-(4-carboxylphenylazo)-8-aminoquinoline (CPAQ) are described. A simple, rapid, selective, and sensitive spectrophotometric method for the determination of microgram amounts of gold is developed, based on the colour reaction between the metal ion and CPAQ in the presence of cetyltrimethyl ammonium bromide. Gold (III) reacts with the reagent in the ratio 1 3 (metal to ligand) in alkaline solution to form a blue-green complex with an absorption maximum at 608 nm. Beer's law is obeyed over the concentration range 0–1.8 g · ml^–1 (ppm) of gold. The molar absorptivity and Sandell's sensitivity of the method are 9.11 × 10⁴ l · mole^–1 · cm^–1 and 0.00216 g · cm^–2, respectively. The interference of various ions has been studied and conditions were developed for the determination of gold in an ore and anode slimes.     

4, 5-二溴苯基荧光酮光度法测定微量钯

研究了在十二烷基磺酸钠存在下,Pd(Ⅱ)与4,5 二溴苯基荧光酮的显色反应.试验表明,在pH6 3醋酸 醋酸钠缓冲溶液中,Pd(Ⅱ)与试剂形成1∶4的暗黄色配合物,配合物的最大吸收峰位于376nm波长处,表观摩尔吸光系数ε为1 06×105L/(mol·cm).Pd(Ⅱ)含量在0～12μg/10mL范围内符合比尔定律.所拟方法用于钯催化剂和钯矿样中微量钯的测定,结果满意.     

8-羟基喹哪啶固相萃取光度法测定水样中的铁

研究了8-羟基喹哪啶与铁的显色反应，在pH为8．0的氯化氨-氨水缓冲介质中，在十六烷基三甲基溴化铵(CTMAB)存在下，8-羟基喹哪啶与铁反应生成3：1稳定的蓝紫色络合物，该络合物可被Waters Sep-Park-C18固相萃取小柱萃取，用乙醇洗脱后用光度法测定，络合物λmax=600nm。在此波长下其它金属离子的络合物无光吸收，对铁选择性很好，铁含量在0-5mg/L内符合比尔定律，方法用于水样中痕量铁的测定，结果令人满意。     

利用电荷迁移反应测定头孢羟氨苄

提出一种基于电荷迁移反应简便可靠地测定头孢羟氨苄的分光光度法。在甲醇－乙醇介质中，头孢羟氨苄与氯冉酸于５０℃反应１５ｍｉｎ能够形成稳定的１：１络合物，其λｍａｘ＝５２８ｎｍ，线性范围为２０￣４００ｍｇ／Ｌ。用拟定的方法测定原粉和胶囊，结果与药典法一致。对浓度１００ｍｇ／Ｌ的药物１０次测定相对标准偏差为１．４％，样品的标准加入回收率为９９．０％￣１００．８％。     

Spectrophotometric Study on Some Amino Acid Drugs with Chloranil and its Analytical Application

Aminobutyric acid, carbocisteine and levodopa are attributed to amino acid derivative agents, which are widely used as drugs for resuming brain cells, grume regulator and curing parkinsonism, respectively. Several methods have been reported for quantitati…     

表面活性剂增敏荷移反应紫外分光光度法测定三聚氰胺

在pH =7.55的Tris-HC1缓冲溶液中,以十六烷基三甲基溴化铵( CTMAB)为增敏剂,三聚氰胺与四氯对苯醌之间发生荷移反应,研究了其反应产物的紫外光谱性质,据此建立了荷移反应紫外分光光度法测定三聚氰胺的方法.三聚氰胺的线性范围为8.61×10-8 ～2.60×10 -6mol/L,r=0.9995,检出限为2...     

2,4-二硝基酚分光光度法测定氯氮卓

在水溶液中 ,氯氮卓与 2 ,4 二硝基酚发生荷移反应 ,生成稳定的 1∶1的配合物 .最大吸收波长为 44 4nm ,表观摩尔吸光系数为ε =1.48× 10 3L/ (mol·cm) ,线性范围 3～ 96 μg/mL ,回收率为 99.95 %～ 99.97% ,相对标准偏差为 0 .5 5 %     

荷移反应-紫外分光光度法测定尿酸

本文采用紫外分光光度法研究了尿酸与四氰乙烯之间的荷移反应。尿酸与四氰乙烯可以形成淡绿色的荷移配合物,其配合比为1∶2。在测定波长395 nm处,该配合物的表观摩尔吸光系数ε=6.24×104L.mol-1.cm-1,方法线性范围为5.7×10-7~5.7×10-6mol.L-1。应用本法测定了人体代谢物中尿酸的含量,回收率为96.4%~110.5%,相对标准偏差(RSD)为1.98%(n=7)。     

7-(对甲酰基苯偶氮)-8-羟基喹啉-5-磺酸的合成及其双波长分光光度法测定镓

7－（对甲酰基苯偶氮）－8－羟基喹啉－5－磺酸是一新显色剂。该试剂在微碱性介质中（pH＝7．5）与镓形成黄色络合物。络合物λmax＝392nm，摩尔吸光系数ε392＝2．24×104L·mol-1·cm-1。同时在500nm呈现负峰，用双峰观波长法测定镓ε392～500＝6．89×104L·mol-1·cm－1，灵敏度是单波长法的三倍多．线性范围0～2．0×10－5mol／L。用拟定的方法测定了掺硅的GaAS材料及岩石中的镓，加入回收率为106％～110％；方法的相对标准偏差小于1．6％。     

2,6-二碘-4-硝基偶氮胂分光光度法测定微量铋

研究了显色剂 2 (2 胂酸基苯偶氮 ) 7 (2 ,6 二碘 4 硝基苯偶氮 ) 1,8 二羟基 3,6 萘二磺酸与铋的显色反应。在 0 .6mol LHClO4 介质中 ,试剂与铋生成的深色络合物 ,最大吸收波长 6 33nm ,摩尔吸光系数为1 2 0× 10 5L·mol- 1 ·cm- 1 ,灵敏度高 ,常见的金属离子允许量大 ,选择性好。Bi 0～ 0 .8mg L范围内符合比耳定律 ,以NaCl褪色试样空白为参比 ,分光光度法测定纯铜及铜合金中的微量铋 ,方法简便 ,结果可靠     

4,5—二溴苯基荧光酮光度法测定钇

研究４，５－二溴苯基荧光酮灵敏光度法测定钇。在ｐＨ５．５缓冲溶液中钇与ＤＢＰＥ形成橙红色络合物，最大吸收波长位于５５０ｎｍ，表观摩吸光系ε值１．５３×１０＾５Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，钇量在每２５ｍＬ０－８μｈ范围内服从比耳定律，测定极限６．８μｇ／Ｌ，对于钇０．２４ｍｇ／Ｌ测定的相对标准偏差为２．６％，络合物的摩尔组成为Ｙ：ＤＢＰＦ＝１：３。方法用于镁合金和地质标样中钇的测定，结果满意。     

A new Cu(II)-5-(4-sulphophenylazo)-8-aminoquinoline complex used for copper determination in presence of gold and silver in water and mineral samples

In this work, a characterization of reagent chromophere 5-(4-sulphophenylazo)-8-aminoquinoline [SPA] by IR and ¹H RMN was carried out and a pK_a value of 3.55 ± 0.03 was found as well. An 1:2 stoichiometry for the Cu(II)-SPA complex was determined at pH 9 by Job and molar ratio methods. A value of 1.4 × 10¹⁴ for the stability constant was also found. Based on the formation of this complex a new method for the copper determination in presence of gold and silver was developed by derivative spectrophotometry using a previous preconcentration on solid phase. In this method, the analytical measures were executed directly in the solid phase containing the complex. The Cu(II) reacts with the reagent chromophere SPA previously retained in the anionic exchange DEAE Sephadex A25. In this determination, the first derivative at 605 nm was used. The quantification range was between (3.2 ± 0.3 × 10⁻¹) × 10⁻⁸ and (94.4 ± 0.9) × 10⁻⁸ mol L⁻¹ (3.2 ± 0.3 × 10⁻¹) × 10⁻⁸ , and (94.4 ± 0.9) × 10⁻⁸ mol L⁻¹. The repeatability expressed as RSD was between 1.1 and 2.0%. The method was applied successfully for the copper determination in mineral residuals and natural water samples. The results were consistent with those provided by ICP-mass spectrometry.     

The Simultaneous Spectrophotometric Determination of Osmium and Ruthenium

Abstract

A spectrophotometric procedure is described for the simultaneous determination of osmium and ruthenium in the form of bromo complexes. It was found that a blue ruthenium-thiourea complex could be formed in 6.7 M HBr solutions while the osmium could be maintained as the hexabromoosmate complex. Absorption maxima were at 620 μ for the ruthenium complex and at 446 μ for the osmium complex. Molar absorptivities for the ruthenium complex were 2.47 × 10³ at 620 μ and 763 at 446 μ. For the osmium complex molar absorptivities were 328 at 620 μ and 6.81 × 10³ at 446 μ. The method is useable over the range of 5 to 30 ppm with an absolute error of = 1 ppm over the range. Other platinum metals interfere.     

新试剂5-(4-氯苯基偶氮)-8-苯磺酰氨基喹啉光度法测定微量铜

在 p H 8.5的 Na2 B4 O7- HCl介质及有氯化十六烷基吡啶 ( CPC)存在时 ,室温下铜 ( )与 5 - ( 4 -氯苯基偶氮 ) - 8-苯基磺酰氨基喹啉 ( CPBSQ)迅速反应 ,生成络合比为 1∶ 3的有色络合物。研究了反应的最佳条件 ,建立了一个测定 Cu( )的光度分析新方法。Cu( )的浓度在 0～ 1 4.0 μg/2 5 m L 范围内符合比耳定律 ,其摩尔吸光系数为 8.1 2× 1 0 4 L· mol- 1· cm- 1。方法用于面粉、茶叶及奶粉中铜的测定 ,其相对标准偏差为 0 .5 8%～ 1 .2 % ,标准加入回收率为 95 .5 %～ 1 0 4 .5 %。