Spectrofluorimetric Determination

Spectrofluorimetric method was reported by Chalmers and Wadds (1970) for the estimation of opium alkaloids in micro amounts where morphine, codeine, papaverine and narcotine mixtures are determined spectrofluorime-trically in 2.5 h with 7% relative errors. Morphine and codeine are determined by a differential method involving fluorescence measurements in 0.1 N sulfuric acid and 0.1 N sodium hydroxide solutions, after the papaverine and narcotine were extracted into chloroform from the sample solution in 0.1 N sulfuric acid. Then papaverine and narcotine are determined after extraction at pH 9. Trichloroacetic acid is used for simultaneous enhance- 

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SPECTROFLUORIMETRIC DETERMINATION OF OXYTETRACYCLINE AND CITRATE ION USING TERNARY COMPLEX WITH EUROPIUM(III)... 

Refaat et al. [24] used a spectrophotometric method for the determination of primaquine, and 16 other tertiary amine drugs, in bulk or in pharmaceuticals. The method involved the condensation of malonic acid with acetic anhydride in the presence of a tertiary amine in an aliphatic or a heterocyclic system. The condensation product is highly fluorescent and allows the spectrofluorimetric determination of the drug in the ng/mL ranges (Xcx = 415 nm and >.em = 455 nm). 

Velapoldi, R.A., White, P.A., May, W.E., Eberhardt, K.R. (1983) Spectrofluorimetric determination of polycyclic aromatic hydrocarbons in aqueous effluents from generator columns. Anal. Chem. 55, 1896-1901. 

The neomycin molecule does not exhibit fluorescence but following suitable de-rivatisation two spectrofluorimetric determinations have been described. Maeda et al l reported the complexation of simple hexosamines with pyridoxal and zinc ions to result in a fluorescent derivative. Applying this procedure to neomycin, Simpsonl32 demonstrated a linear response over the concentration range 0-50 yg/ml of neomycin sulphate. 

Spectrofluorimetric Determination of Al3+ Using 3-hydroxy-2-(4-methoxy phenyl)-4H-chromen-4-one as Analytical Reagent. 

Ion exchanger colorimetry has been used as a sensitive and rapid method for vanadium analysis by immobilization of 2[2-(3-5-dibromopyri-dyl)azo]-5-dimethylaminobenzoic acid onto an ion exchanger resin AG 1X2 [75]. Solid phase fluorimetry can be useful for the analysis of very dilute solutions in water analysis or trace metal determination thus a chelating 8-(benzene-sulfonamido)quinoline, immobilized on Amberlite XAD2 support, has been used for the spectrofluorimetric determination of Zn(II) and Cd(II) [76]. 

The reaction is stopped by the addition of 1 ml ice-cold 10% trichloroacetic acid and the tubes are kept in ice water for 15 min. They are then centrifuged for 5 min at 14,000 rpm (16,1OOxg) in a bench-top centrifuge. One milliliter of supernatant is aspirated with a 1-ml syringe and filtered into brown HPLC autosampler tubes. Twenty-microliter aliquots of standards and samples are injected into the HPLC system. Spectrofluorimetric determination may be used instead of HPLC. 

Recently, Street and Schenk (13) reported a spectrofluo-rimetric analysis of salicylamide in the presence of acetylsalicylic acid and salicylic acid as impurities by direct and indirect methods. Salicylic acid is determined in the range of 10-Tm concentration after separation from salicylamide. The instrumental conditions for the spectrofluorimetric determination of salicylamide, acetylsalicylic acid and salicylic acid is shown in Table 1. 

Terenina, N. B. (1984). Results of spectrofluorimetric determination of biogenic amines (serotonin, dopamine) in cestodes. Helminthologia, 21 275-80. 

Liu ZH, Wang QL, Mao LY et al (2000) Highly sensitive spectrofluorimetric determination of ascorbic acid based on its enhancement effect on a enzyme-catalyzed reaction. Anal Chim Acta 413 167-173... 

Ruiz-Medina, A., Fernandez-de Cordova, M. L., and Molina-Diaz, A. Flow injection-solid phase spectrofluorimetric determination of pyridoxine in presence group B vitamins. Presenilis J. Anal. Chem. 363(3) 265-269, 1999. 

Bautista, J. A. G., Mateo, J. V. G., and Calatayud, J. M. Spectrofluorimetric determination of iproniazid and isoniazid in an FIA system provided with a solid-phase reactor. Anal. Lett. 31(7) 1209-1218,1998. 

T. Sakai, N. Ohno, Y.S. Chug, H. Nishikawa, Spectrofluorimetric determination of berberine in oriental pharmaceutical preparations by flow-injection analysis coupled with liquid-liquid extraction, Anal. Chim. Acta 308 (1995) 329. 

Spectral characteristics and selection of surfactant. Increase in the fluorescence intensity of the carbaryl solution was observed using SDS as surfactant at excitation and emission wavelengths of 281 nm and 349 nm respectively (Fig. 1). As can be seen from Fig. 1, Triton X-100 and dodecyl pyridinium chloride (DPC) decreased the fluorescence. This phenomenon clearly indicates that cationic surfactant (DPC) and neutral surfactant (Triton X-100) have negative effects on the fluorescence intensity for carbaryl while anionic surfactant (SDS) enhances the fluorescence intensity of carbaryl. This surfactant-enhanced phenomenon by SDS was used for the spectrofluorimetric determination of carbaryl. 

Parameter optimization. For maximum fluorescence various parameters, e.g. alcohol, pH and SDS concentration were optimized for the spectrofluorimetric determination of carbaryl. By addition of ethanol an increase in fluorescence was observed. Further it was found that increasing the ethanol percentage up to 20 % increased fluorescence. Beyond 20 % ethanol a decrease in fluorescence was found. Therefore, 20 % ethanol was used in further experiments. Phosphate buffer pH 7 was found to be the optimum buffer. The optimum concentration for SDS was found to be 1.0 xiO 4 mol/L. Above this concentration of SDS, a decrease in response was observed. 

Sakai, T., Piao, S., Teshima, N. et al. (2004) Flow injection system with in-line Winkler s procedure using 16-way valve and spectrofluorimetric determination of dissolved oxygen in environmental waters. Talanta, 63 (4), 893-898. 

Croubels, S. Van Peteghem, C. Baeyens, W. Sensitive spectrofluorimetric determination of tetracycline residues in bovine milk. Analyst, 1994, 119, 2713-2716... 

Fluorescence Spectroscopy. - A method for the spectrofluorimetric determination of six organophosphorus pesticides has been established. The fluorescence of the solutions was measured at excitation wavelength, 380 nm and emission wavelength, 488 nm. The optimum pH for measurement is 9.3 - 9.6 and transition metal ions interfere but can be removed by complexation. Detection limits varied between 10and 10 g/ml, depending on the substance. There are... 

P. Linares, M. D. Luque de Castro, and M. Valcarcel, Spectrofluorimetric Determination of Silicon by Flow Injection Analysis. Anal. Chim. Acta, 111 (1985) 263. 

M. Aihara, M. Arai, and T. Taketatsu, Flow Injection Spectrofluorimetric Determination of Europium(III) Based on Solubilizing Its Ternary Complex with Thenoyltrifluoroacetone and Trioctylphosphine Oxide in Micellar Solution. Analyst, 111 (1986) 641. 

M. H. Memon and P. J. Worsfold, The Use of Microemulsions in Flow Injection Analysis. Spectrofluorimetric Determination of Primary Amines. Anal. Chim. Acta, 183 (1986) 179. 

K19. Kennedy, J. F., The spectrofluorimetric determination of carbohydrates, glycoproteins and some amino acids. Automat. Anal. Chem., Technicon Symp., 1971 pp. 532-541 (1974). 

Fernandez P, Perez Conde C, Gutierrez A, et al. 1992b. Selective spectrofluorimetric determination of zinc in biological samples by flow injection analysis (FIA). Fresenius Journal Analytical Chemistry 342(7) 597- 600. 

Vasimalai, John, S. A. (2011). Ultrasensitive and selective spectrofluorimetric determination of Hg(II) using a dimercaptothiadiazole fluorophore. J. Luminesc., 131, pp. 2636-2641, ISSN 0022-2313... 

In literature (Cha et al., 1998), salicylic add has been used as a fluorescence reagent for the spectrofluorimetric determination of iron(III) in batch conditions. Experimentally it was found to be a very sensitive emission reagent for the spectrofluorimetric determination of iron(III) in the absence of iron (II). A very strong emission p>eak of salicylic acid in aqueous solution, which decreased linearly with the addition of iron(III), occurred at 409 nm with excitation at 299 nm. Also, salicylic acid is a commerdally available reagent and it does not have a risk of serious toxidty when compared to the reagents used previously. 

Asan A., Andac M. and Isildak I. (2010) Flow injection spectrofluorimetric determination of iron(III) in water using salicylic acid. Chemical Papers, 64(4) 424-428. 

Aghamohammadi, M., Hashemi, J., Kram, G.A. Alizadeh, N. (2007) Enhanced synchronous spectrofluorimetric determination of aflatoxin B1 in pistachio samples using multivariate analysis. Anal. Chim. Acta 582, 288-294. 

El-Kemary, M.A. El-Mehasseb, I.M. Global and distribution analysis of fluorescence decays and spectrofluorimetric determination of stoichiometry and association constant of... 

This chapter focuses on the spectrofluorimetric determination of vitamin Bi (thiamin). 

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