曲利本蓝-氨基糖苷类抗生素的显色反应及其分析应用

曲利本蓝 (TB)与硫酸卡那霉素 (KANA)和硫酸妥布霉素 (TOB)等氨基糖苷类抗生素在pH 2 .0～ 7.0的条件下反应生成蓝色离子缔合物。其最大显色波长位于 680nm(TOB)和 686nm(KANA) ,线性范围分别是 0～ 1 1 .0 μg mL(TOB)和0～ 1 3.0 μg mL(KANA) ,摩尔吸光系数 (ε)分别为 5 .32× 1 0 3(TOB)和 3.64× 1 0 3(KANA)L·mol-1·cm-1;最大褪色波长位于 5 88nm(TOB)和 5 90nm(KANA) ,线性范围均为 0～ 1 1 .0 μg mL ,摩尔吸光系数 (ε)分别为 1 .84× 1 0 4 (TOB)和 1 .1 1× 1 0 4(KANA)L·mol-1·cm-1。当用双波长叠加法时 ,ε值分别为 2 .37× 1 0 4 (TOB)和1 47× 1 0 4 (KANA)L·mol-1·cm-1。探讨了适宜的反应条件及主要的分析化学性质。该方法用于市售药物中氨基糖苷类抗生素的测定。     

曲利本红分光光度法测定氨基糖苷类抗生素

在pH2.8~7.0的条件下,曲利本红(TR)与硫酸妥布霉素(TOB)、硫酸庆大霉素(GEN)和硫酸新霉素(NEO)等氨基糖苷类抗生素反应生成红色离子缔合物,最大显色波长位于392nm(NEO、GEN)和570nm(TOB),不同体系的线性范围从0~14.0mg.L-1至0~16.0mg.L-1,摩尔吸光系数(ε)在7.65×103~1.40×104L.mol-1.cm-1之间;最大褪色波长位于502nm(NEO)和498nm(GEN、TOB),线性范围从0~13.0mg.L-1至0~16.0mg.L-1,摩尔吸光系数(ε)在4.02×103~9.32×103L.mol-1.cm-1之间。当用双波长叠加法测定时,ε值在1.46×104~2.67×104L.mol-1.cm-1之间。探讨了适宜的反应条件及主要的分析化学性质。该法用于市售药物中氨基糖苷类抗生素含量的测定,结果满意。     

依文思蓝-氨基糖苷类抗生素的显色反应及其分析应用

在pH 2 .0～ 7.0的条件下 ,依文思蓝 (EB)与硫酸新霉素 (NEO)、硫酸卡那霉素 (KANA)、硫酸庆大霉素(GEN)和硫酸妥布霉素 (TOB)等氨基糖苷类抗生素反应生成蓝色离子缔合物 ,最大显色波长位于 672～ 676nm ;不同体系的线性范围从 0～ 9.0至 0～ 1 2 .0mg L ;摩尔吸光系数 (ε)在 1 .75× 1 0 4 ～ 3 .3 0× 1 0 4 L·mol- 1 ·cm- 1之间 ;最大褪色波长位于 61 6～ 62 0nm的区间。用褪色光度法测定时 ,线性范围从 0～ 6.0mg L至 0～ 1 4.0mg L;摩尔吸光系数 (ε)从 1 .2 2× 1 0 4 至 4.63× 1 0 4 L·mol- 1 ·cm- 1 。当用双波长叠加法时 ,ε值在 (2 .97～ 7.93 )× 1 0 4 L·mol- 1 ·cm- 1 之间。探讨了适宜的反应条件及主要的分析化学性质。该方法用于市售药物及尿液中氨基糖苷类抗生素含量的测定 ,结果满意     

铕-伊文思蓝分光光度法测定新霉素及妥布霉素

在酸性条件下,铕(Ⅲ) 伊文思蓝(EB)与硫酸新霉素(NEO)或硫酸妥布霉素(TOB)反应生成三元蓝色离子缔合物。最大吸收波长位于668nm(NEO)和670nm(TOB);线性范围分别为0～15.5μg·mL-1(NEO)和0～15.0μg·mL-1(TOB);摩尔吸收光系数(ε)为1.19×105(NEO)和9.05×104(TOB)L·mol-1·cm-1;最大负吸收波长位于608nm,线性范围分别为0～16.5μg·mL-1(NEO)和0～16.0μg·mL-1(TOB),摩尔吸收光系数(ε)为1.54×105(NEO)和1.08×105(TOB)L·mol-1·cm-1。当用双波长叠加时,ε值为2.73×105(NEO)和2.00×105(TOB)L·mol-1·cm-1。该法已用于市售药物及尿液中新霉素和妥布霉素含量的测定,分析结果满意。     

硫酸卡那霉素-固绿体系的共振瑞利散射光谱及其分析应用

提出了共振瑞利散射法(RRS)测定硫酸卡那霉素(KANA)的方法。在p H为4.56~6.09的B-R缓冲溶液中,固绿与KANA结合生成离子缔合物,使溶液共振瑞利散射(RRS)增强,其最大散射峰位于709 nm,另在463 nm、370 nm有两个较弱的散射峰。KANA的浓度在0.08~1.6 mg·L~(-1)范围内,与RRS强度有良好的线性关系,对KANA的检出限(3σ)达0.024 mg·L~(-1)。研究了适宜的反应条件和影响因素,表明该方法灵敏、稳定。用于硫酸卡那霉素注射液的测定,回收率为96.5%~103.0%。     

滂胺天蓝-氨基糖苷类抗生素的显色反应及其分析应用

在 pH2.0～7.0的条件下 ,滂胺天蓝(PSB)与硫酸卡那霉素(KANA)、硫酸庆大霉素(GEN)和硫酸新霉素(NEO)等氨基糖苷类抗生素反应生成蓝色离子缔合物 ,最大显色波长位于686～690nm ,线性范围分别为0～14.0、0～12.5、0～14.0mg/L ,摩尔吸光系数(ε)分别为1.53×104、1.12×104、1.47×104L/(mol·cm) ;最大褪色波长位于620～622nm ,线性范围分别为0～14.0、0～12.0、0～14.0mg/L ,摩尔吸光系数(ε)分别为1.41×104、1.43×104、2.42×104L/(mol·cm) ;当用双波长叠加法测定时 ,ε值分别为2.94×104、2.55×104、3.89×104L/(mol·cm) ;探讨了适宜的反应条件 ;该法用于市售药物中氨基糖苷类抗生素含量的测定 ,结果令人满意     

达旦黄与氨基糖苷类抗生素相互作用的共振瑞利散射光谱研究及其应用

在弱酸性介质中,达旦黄(TY)和氨基糖苷类抗生素(AGs)本身的共振瑞利散射(RRS)均很微弱。但两者相互作用形成离子缔合物时,溶液的RRS显著增强,并产生了新的RRS光谱。不同AGs的反应产物具有相似的光谱特征,其RRS峰位于278和469 nm;与此同时,它的倍频散射(FDS)也明显增强,并且最大FDS峰位于392 nm处,但二级散射(SOS)变化不明显。RRS较FDS具有较高的灵敏度,而且在一定范围内,AGs的浓度与散射强度(ΔIRRS)成正比。对于不同抗生素的检出限在17.2~23.3μg.L-1之间,用于氨基糖苷类注射液和血清样品中AGs的测定,测得结果的RSD(n=5)值均小于3.5%,回收率在96.3%~97.2%之间。     

水溶苯胺蓝褪色光度法测定庆大霉素及妥布霉素的研究

在酸性条件下,水溶苯胺蓝(ABWS)与硫酸庆大霉素(GEN)或硫酸妥布霉素(TOB)反应,生成离子缔合物,使水溶苯胺蓝溶液褪色,其最大褪色波长分别位于606nm(GEN)和608nm(TOB);在0～1.2×10-5mol·L-1(GEN)和0～1.5×10-5mol·L-1(TOB)的浓度范围内遵从比耳定律;表观摩尔吸光系数(ε)分别为2.21×104L·mol-1·cm-1(GEN)和3.10×104(TOB)L·mol-1·cm-1。本法已用于市售药物及人体尿液中庆大霉素及妥布霉素含量的测定,结果满意。     

镧-曲利本红光度法测定新霉素及庆大霉素

在pH3.0～6.5的条件下,镧(Ⅲ) 曲利本红(TR)与硫酸新霉素(NEO)或硫酸庆大霉素(GEN)反应生成三元红色离子缔合物,其最大吸收波长位于388nm,摩尔吸收光系数(ε)为4.86×104、2.10×104L·mol-1·cm-1;最大负吸收波长位于432nm(NEO)和428nm(GEN),摩尔吸收光系数(ε)为1.38×104、1.19×104L·mol-1·cm-1。当用双波长叠加时,ε值为6.24×104(NEO)、3.28×104(GEN)L·mol-1·cm-1。探讨了适宜的反应条件和主要分析化学性质。该法用于市售药物中新霉素、庆大霉素含量的测定,结果满意。     

甲基蓝与庆大霉素、妥布霉素的褪色反应及其应用

在酸性条件下,硫酸庆大霉素(GEN)、硫酸妥布霉素(TOB)与甲基蓝(MB)反应,生成离子缔合物,使甲基蓝褪色,其最大褪色波长位于606nm(GEN)和610nm(TOB),表观摩尔吸光系数(ε)为1.80×104(GEN)和2.93×104(TOB)L·mol-1·cm-1;庆大霉素、妥布霉素浓度在0～1 2×10-5mol·L-1范围内遵从比耳定律。该法用于市售药物及人体尿液中庆大霉素及妥布霉素含量的测定,结果满意。     

Resonance Rayleigh scattering measurement of aminoglycoside antibiotics with Evans Blue.

In a weak acid medium, some aminoglycoside antibiotics, such as kanamycin (KANA), gentamicin (GEN), tobramycin (TOB) and neomycin (NEO), or acid bisazo dye Evans Blue (EB) can only produce very weak resonance Rayleigh scattering (RRS) signals. However, when two agents react with each other to form ion-association complexes, the RRS intensity can be greatly enhanced and a new RRS spectrum with a significant enhancement of the RRS intensity in the wavelength range from 350 nm to 600 nm can be observed. The maximum scattering peak is at 570 nm. There is a linear relationship between the RRS intensity and the antibiotic concentration in the range of 0.01-6.0 microg mL(-1) at 570 nm. This RRS method for the determination of aminoglycoside antibiotics at trace-amount levels has been developed. The detection limits (3sigma) of the four antibiotics, whose order of sensitivity from high to low ranks as KANA > NEO > TOB > GEN, are 5.2-6.9 ng mL(-1). This method has good selectivity and has been successfully applied to the quick determination of antibiotics not only for injections and ear drops, but for clinic serum samples as well. In addition, the reaction mechanism by using a quantum chemistry method and the influencing factors of the RRS spectra and the enhancement reasons of RRS have been discussed.     

Resonance Rayleigh scattering spectra for studying the interaction of aminoglycoside antibiotics with pontamine sky blue and their analytical applications

In a weakly acid medium, some aminoglycoside antibiotics, such as kanamycin (KANA), gentamicin (GEN), tobramycin (TOB), and neomycin (NEO), or acid bisazo dye pontamine sky blue (PSB) can only produce very weak resonance Rayleigh scattering (RRS) signals. However, when the two agents react with each other to form the ion association complexes, the RRS intensity can be enhanced greatly and a new RRS spectrum and a significant enhancement of the RRS intensity in the wavelength range 350-600 nm can be observed. The maximum scattering peak is at 580 nm. There is a linear relationship between the RRS intensity and the antibiotic concentration in the range 0.01-6.0 microg mL(-1) at 580 nm. This RRS method has therefore been developed for the determination of trace levels of aminoglycoside antibiotics. The detection limits (3 sigma) of the four antibiotics, whose order of sensitivity is KANA>NEO>TOB>GEN, are 5.8-6.9 ng mL(-1). This method has a good selectivity and has been successfully applied to the quick determination of antibiotics not only for injections and ear drops, but clinic serum samples as well. In addition, quantum chemistry-based analysis of the reaction mechanism, the factors influencing the RRS spectra, and the reasons for the enhancement of RRS are discussed.     

Resonance Rayleigh scattering and resonance non-linear scattering method for the determination of aminoglycoside antibiotics with water solubility CdS quantum dots as probe

In pH 6.6 Britton–Robinson buffer medium, the CdS quantum dots capped by thioglycolic acid could react with aminoglycoside (AGs) antibiotics such as neomycin sulfate (NEO) and streptomycin sulfate (STP) to form the large aggregates by virtue of electrostatic attraction and the hydrophobic force, which resulted in a great enhancement of resonance Rayleigh scattering (RRS) and resonance non-linear scattering such as second-order scattering (SOS) and frequency doubling scattering (FDS). The maximum scattering peak was located at 310 nm for RRS, 568 nm for SOS and 390 nm for FDS, respectively. The enhancements of scattering intensity (ΔI) were directly proportional to the concentration of AGs in a certain ranges. A new method for the determination of trace NEO and STP using CdS quantum dots probe was developed. The detection limits (3σ) were 1.7 ng mL⁻¹ (NEO) and 4.4 ng mL⁻¹ (STP) by RRS method, were 5.2 ng mL⁻¹ (NEO) and 20.9 ng mL⁻¹ (STP) by SOS method and were 4.4 ng mL⁻¹ (NEO) and 25.7 ng mL⁻¹ (STP) by FDS method, respectively. The sensitivity of RRS method was the highest. The optimum conditions and influence factors were investigated. In addition, the reaction mechanism was discussed.     

Study on the interaction of aminoglycoside antibiotics with Titan Yellow by spectrophotometric method and their analytical applications

In a weak acidic medium, the reaction of some aminoglycoside antibiotics (AGs) such as kanamycin sulfate (KANA), gentamycin sulfate (GEN), and tobramycin sulfate (TOB) with acid thiazolyl bisazo dye Titan Yellow (TY) can result in the fading of TY. The maximum fading wavelength was located at 409 nm. The molar absorptivities (ɛ/×10⁴ 1 mol⁻¹ cm⁻¹) were 2.0, 1.5 and 2.5 for KANA, GEN and TOB, respectively. The spectral characteristics, effect factors, optimum conditions of the reaction and the influence of foreign substances were also investigated. The procedure is easy and fast. This method has high sensitivity and can be applied to the determination of commercial aminoglycoside antibiotics and serum samples with satisfactory results. __________ Translated from Journal of southwest China Normal University, 2005, 30(2) (in Chinese)     

同多钨酸-阿米卡星相互作用的共振瑞利散射光谱及其分析应用

在pH 0.65~1.10的HCl-NaAc缓冲溶液中,当同多钨酸(IPT)与阿米卡星(AMK)形成离子缔合物,能引起共振瑞利散射 (RRS)显著增强,并产生新的RRS光谱,其最大散射峰位于340 nm,AMK浓度在0.001~0.08 µg•mL-1范围内与散射增强程度呈线性关系,据此建立测定AMK的RRS新方法。方法具有较高的灵敏度,检出限(3σ)为0.4 ng•mL-1。考察了体系的RRS和吸收光谱特征,优化了适宜的反应条件,试验了常见共存物质的影响,表明方法具有良好的选择性。方法用于人血清中AMK的测定,结果满意。文中对离子缔合反应机理和RRS增强的原因进行了讨论。     

铁氰化钾高灵敏共振瑞利散射法测定青霉素类抗生素

在稀HCl介质中,K3[Fe(CN)6]与阿莫西林(AMO)、氨苄西林(AMP)、氯唑西林钠(CLO)、羧苄西林钠(CAR)和青霉素钠(BEN)等抗生素药物在加热条件下反应生成结合产物,会导致溶液的共振瑞利散射(RRS)强度急剧增强,并产生新的RRS光谱,5种反应产物的最大散射峰均位于330 nm附近。在一定的浓度范围内,不同的反应体系散射强度(∆I)与药物浓度成正比,反应具有很高的灵敏度,K3[Fe(CN)6]对5种药物的检出限分别在4.61至5.62 ng·mL-1之间。本文研究了RRS的光谱特征和适当的反应条件,并讨论了反应机理和散射增强的原因,还考察了共存物质的影响,表明方法具有较好的选择性,可用于胶囊、片剂和人血清及尿液中青霉素类药物的测定。     

Study on the resonance Rayleigh scattering spectra and resonance non-linear spectra of congo red-amikacin system and its analytical application

The interaction between congo red (CR) and amikacin (AMK) was studied by resonance Rayleigh scattering (RRS), frequency doubling scattering (FDS) and second-order scattering (SOS) combining with absorption spectrum. In a weak acidic medium, CR combined with AMK to form an ion association complex with the composition ratio of 1∶1 by electrostatic interaction, hydrophobicity and charge transferring effect. As a result, the new spectra of RRS, FDS, and SOS appeared and their intensities were enhanced greatly. The maximum wavelengths of RRS, FDS and SOS were located at 563 nm, 475 nm and 940 nm, and the scattering intensities were proportional to the concentration of AMK. These three methods have very high sensitivities, and the detection limits were 4.0 ng·mL?1 for RRS, 3.6 ng·mL?1 for FDS and 1.9 ng·mL?1 for SOS, respectively. At the same time, the methods have better selectivity. A new method for the determination of trace amounts of AMK with congo red by resonance scattering technique has been developed. The recovery for the determination of AMK in blood serum and urine sample was between 95.5% and 105.5%. In this study, the properties, such as enthalpy of formation, charge distribution and mean polarizability, were calculated by AM1 quantum chemistry method. In addition, the reaction mechanism and the reasons for the enhancement of scattering spectra were discussed.     

Resonance Rayleigh scattering spectrum for the chelate of lanthanum(III) with sodium tanshinon IIA silate and its analytical application

In a pH 3.6–5.0 HAc-NaAc buffer solution, when sodium tanshinon IIA silate (STSIIA) reacts with La(III) to form a chelate, the resonance Rayleigh scattering (RRS) intensity can be enhanced greatly and a new RRS spectrum will appear. The maximum RRS peak is located at 306 nm and the RRS intensity is proportional to the concentration of STSIIA in a certain range. The method is very sensitive and the detection limit for STSIIA (3σ/K) is 82.12 ng·mL⁻¹. The optimum reaction conditions and the effect of coexisting substances have been investigated. A new, simple and fast method for the determination of STSIIA based on RRS method is developed. It can be applied to the determination of STSIIA in the synthesis samples and Nuoxinkang injection. Combined with infrared absorption and NMR spectra, the structure of the chelate and the reasons of RRS enhancement are also discussed.     

十二烷基苯磺酸钠-硫酸耐而蓝体系的共振瑞利散射光谱及其分析应用

提出了共振瑞利散射法(RRS)测定十二烷基苯磺酸钠(SDBS)的新方法。在pH为1.98～3.29的B-R缓冲溶液中,硫酸耐而蓝与SDBS结合生成离子缔合物,使溶液共振瑞利散射(RRS)增强,其最大散射峰位于760 nm,另在533 nm、400 nm有两个较弱的散射峰。SDBS的浓度在0.04～1.6 mg/L范围内,与RRS强度有良好的线性关系,对SDBS的检出限(3σ)达0.018 mg/L。研究了适宜的反应条件和影响因素,表明该方法灵敏、稳定。用于环境水样中阴离子表面活性剂含量的测定,回收率为95.9%～106.7%。     

Resonance Rayleigh-scattering method for the determination of sildenafil citrate in a pharmaceutical formulation using Evans blue.

A highly sensitive resonance Rayleigh-scattering (RRS) method for the determination of sildenafil citrate has been developed, based on the fact that sildenafil (Sild) reacted with Evans Blue (EB) to form an ion-association complex in pH 1.1 - 4.6 aqueous solution. This resulted in a significant enhancement of the RRS intensity, and a new spectrum appeared. The wavelength of the maximum RRS was at 365 nm, and other scattering peaks were at 400, 442, 470 and 534 nm, respectively. The intensity of RRS was directly proportional to the concentration of Sild in the range 0 - 11.5 microg ml(-1), and the detection limit for Sild (3 sigma) was 30.3 ng ml(-1). The composition of the ion-association complex was Sild:EB = 1:1, as established by Job's method. The method had good selectivity and could be applied to the determination of Sild in the aqueous phase without using organic solvent extraction. The method was simple and rapid. In addition, the reaction mechanism and the reason for RRS enhancement were considered.