High-performance liquid chromatography with fast-scanning fluorescence detection and multivariate curve resolution for the efficient determination of galantamine and its main metabolites in serum

Based on green analytical chemistry principles, an efficient approach was applied for the simultaneous determination of galantamine, a widely used cholinesterase inhibitor for the treatment of Alzheimer's disease, and its major metabolites in serum samples. After a simple serum deproteinization step, second-order data were rapidly obtained (less than 6 min) with a chromatographic system operating in the isocratic regime using ammonium acetate/acetonitrile (94:6) as mobile phase. Detection was made with a fast-scanning spectrofluorimeter, which allowed the efficient collection of data to obtain matrices of fluorescence intensity as a function of retention time and emission wavelength. Successful resolution was achieved in the presence of matrix interferences in serum samples using multivariate curve resolution-alternating least-squares (MCR-ALS). The developed approach allows the quantification of the analytes at levels found in treated patients, without the need of applying either preconcentration or extraction steps. Limits of detection in the range between 8 and 11 ng mL⁻¹, relative prediction errors from 7 to 12% and coefficients of variation from 4 to 7% were achieved.     

荧光光谱法间接测定叶绿素的含量

叶绿素中的镁可被氢离子置换而形成去镁叶绿素。本文首次提出用荧光光谱法测定叶绿素中的镁而间接测定叶绿素的方法。在氨性溶液中,以7-碘-8-羟基喹啉-5-磺酸(铁试剂)作荧光试剂,省去了叶绿素标准物质。     

环糊精锌(Ⅱ)荧光试剂在水分析中的应用研究

合成高水溶性的锌()荧光试剂-修饰环糊精的N-(8-对氨基苯磺酰)胺基喹啉(HQAS-1-CD)。该试剂在水溶液中与Zn2+形成2:1配合物而使荧光增强,并且碱金属或碱土金属离子几乎不干扰Zn2+的荧光。利用此配位反应建立了一个荧光测定痕量锌的新方法,测定锌的线性范围为0—13μg/L,检出限0.57μg/L,方法成功的应用于矿泉水中痕量锌的测定。     

Simple and Sensitive Spectrofluorimetric Method for the Determination of Oseltamivir Phosphate in Capsules Through Derivatization with Fluorescamine

A new, simple and sensitive spectrofluorimetric method has been developed for the determination of oseltamivir phosphate (OSP) in capsules. The method is based on the reaction between oseltamivir and fluorescamine in borate buffer solution of pH 8.50 to give highly fluorescent derivatives that are measured at 483 nm using an excitation wavelength of 381. The different experimental parameters effecting the development and stability of the reaction product were carefully studied and optimized. The fluorescence intensity concentration plot is rectilinear over the range 50–450 ng mL⁻¹ with a lower detection limit (LOD) of 1.219 ng mL⁻¹ and limit of quantitation (LOQ) of 4.064 ng mL⁻¹. Selectivity was validated by subjecting stock solution of OSP to acidic, basic, oxidative, and thermal degradation. No interference was observed from excipients present in formulations. The developed method was successfully applied to determination of the drug in capsules. The mean % recovery (n = 6) was 100.08. The results obtained were in good agreement with those obtained using a reported spectrophotometric method.     

过氧化氢-巯嘌呤氧化还原反应的研究及荧光分析应用

研究了过氧化氢氧化巯嘌呤的反应条件及产物的荧光特性 ,提出了高灵敏荧光光度法测定巯嘌呤含量的新方法。在碱性介质和沸水浴加热条件下 ,过氧化氢能将巯嘌呤定量转化为 6-嘌呤磺酸钠 ,其体系的荧光强度与巯嘌呤浓度在6.0× 1 0 -8～ 1 .0× 1 0 -5mol/L范围内呈线性关系 ,检出限为 2 .4× 1 0 -8mol/L。该法已用于片剂中的巯嘌呤含量的测定。     

水杨醛缩5,7-二溴-8-氨基喹啉荧光光度法 测定粮食中的痕量锌

合成了新型息夫碱类试剂水杨醛5,7－二溴－8－氨基喹啉,建立了该试剂荧光光度法测定痕量锌（Ⅱ）的新体系,在pH5-6范围内,50％（V／V）乙醇的溶液中,试剂与锌（Ⅱ）的络事比为2：1,λem=400nm/475nm,线笥范围为0－288μg/L,检出限为1.4μg/L,考察了共存离子的影响,已应用于粮食中痕量锌的测定。     

荧光光谱法研究6—巯基嘌呤的氧化反应及其分析应用

系统地研究了高锰酸钾对６－巯基嘌呤的氧化作用,提出了高灵敏测定６－巯基嘌呤的荧光光度分析新方法。在碱性介质中,氧化产物的荧光强度较６－巯基嘌呤处身的荧光强度提高了１０倍,且稳定性好。本体系的激发波长为２８６ｎｍ,发射波长为３９７ｎｍ,荧光强度与６－巯基嘌呤的浓度在０．００６４～３．０μｇ／ｍＬ范围内呈线性关系,检测限为０．００３２μｇ／ｍＬ。应用该法于片剂中６－巯基嘌呤含量的测定,与标准方法对照,     

Flow injection analysis for the determination of thiabendazole and fuberidazole in water by spectrofluorimetry

Flow-injection analysis (FIA) is proposed for determining thiabendazole (TBZ) and fuberidazole (FBZ) by Spectrofluorimetry. A pH 2 aqueous solution was found to be the optimal solvent for the rapid, precise and sensitive fluorescence analysis of both fungicides. Linear dynamic graphs were established over a concentration range of two orders of magnitude. Limits of detection were 0.7ng/ml for TBZ and 0.1 ng/ml for FBZ. Relative standard deviations were 0.5 and 0.8% for TBZ and FBZ, respectively. The method was applied to the determination of both compounds in spiked river and tap water samples, with satisfactory recoveries.On leave from the Department of Analytical Chemistry and Food Technology, University of Castilla-La Mancha, E-13071-Ciudad Real, Spain     

Flow injection renewable drops spectrofluorimetry for sequential determinations of Vitamins B1, B2 and B6

A novel optical chemical sensor based on the dynamic liquid drops combined with flow injection-solid phase has been developed for continuous and sequential determinations of the mixture of Vitamin B₁, Vitamin B₂ and Vitamin B₆. The design and characteristics of the sensor system are described. The dynamically growing and falling drops serve as windowless optical cells. The adsorption, desorption and quantitative determinations of VB₁, VB₂ and VB₆ were carried out based on selective adsorption of Sephadex CMC-25 and different fluorescence characteristics of VB₂, VB₆ in the basic solutions. The optimum analytical conditions for compound Vitamin B assay have been established. Under these conditions, linear calibration curves were obtained over the range of 0.01-8.00, 0.01-10.00 and 0.01-3.00 μg/ml for VB_1, VB₂ and VB₆ with the limits of determination of 0.008, 0.005 and 0.006 μg/ml, respectively. This method has been applied in the determination of synthetic mixture of VB_1, VB₂, VB₆ and Vitamin B compound tablets with satisfactory results. The technique, which has been described, provides a simple, effective and sensitive method to assay the biological samples.     

P－矩阵荧光法同时测定苯酚和十二烷基苯磺酸钠

在研究了苯酚（Ｐｈ－ＯＨ）和十二烷基苯磺酸钠（ＳＤＢＳ）荧光性质的基础上，以Ｐ－矩阵计算混合体系中苯酚和十二烷基苯磺酸钠．方法灵敏度高，选择性好，简便快速，应用于环境水样测定结果令人满意．