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Spectrofluorimetric determination of oxamniquine in dosage forms and spiked human plasma through derivatization with 1-dimethylaminonaphthalene-5-sulphonyl chloride.

El-Enany N, Belal F, Rizk M - J Fluoresc (2007)

Bottom Line: The proposed method was successfully applied to the analysis of commercial capsules.The results obtained were in good agreement with those obtained using the official spectrophotometric method.A proposal of the reaction pathway was presented.

View Article: PubMed Central - PubMed

Affiliation: Department of Analytical Chemistry, Faculty of Pharmacy, University of Mansoura, Mansoura, Egypt. nelenany1@yahoo.com

ABSTRACT
A sensitive, simple and selective spectrofluorimetric method was developed for the determination of oxamniquine (OXM) in pharmaceutical formulations and biological fluids. The method is based on the reaction between the drug and 1-dimethylaminonaphthalene-5-sulphonyl chloride (dansyl chloride) in presence of 0.5 M sodium carbonate (pH 10) to yield a highly fluorescent derivative that is measured at 445 nm after excitation at 335 nm. The different experimental parameters affecting the development and stability of the reaction product were carefully studied and optimized. The fluorescence concentration plot was rectilinear over the range of 0.02-0.2 microg ml(-1) with a lower detection limit (LOD) of 0.007 microg ml(-1) and limit of quantitation (LOQ) of 0.02 microg ml(-1). The proposed method was successfully applied to the analysis of commercial capsules. The results obtained were in good agreement with those obtained using the official spectrophotometric method. Furthermore, the method was applied for the determination of oxamniquine in spiked human plasma, the mean % recovery (n = 4) is 97.77 +/- 1.19. A proposal of the reaction pathway was presented.

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Proposed reaction pathway between dansyl chloride and oxamniquine
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Sch1: Proposed reaction pathway between dansyl chloride and oxamniquine

Mentions: The stoichiometry of the reaction was studied adopting the limiting logarithmic method [29]. The fluorescence intensity of the reaction product was alternatively measured in the presence of excess of either dansyl chloride or OXM. A plot of log fluorescence versus log [dansyl chloride] and log [OXM] gave straight lines, the values of the slopes are 0.901 and 0.984 respectively (Fig. 6). Hence, it is concluded that, the molar reactivity of the reaction is 0.901/0.984, i.e. the reaction proceeds in the ratio of 1:1. Based on the observed molar reactivity of the reaction, and depending on the presence of secondary amino group and by analogy to similar reports dealing with the reaction of dansyl chloride with compounds containing secondary amino group, the reaction pathway proposed in Scheme 1 is presented.Fig. 6


Spectrofluorimetric determination of oxamniquine in dosage forms and spiked human plasma through derivatization with 1-dimethylaminonaphthalene-5-sulphonyl chloride.

El-Enany N, Belal F, Rizk M - J Fluoresc (2007)

Proposed reaction pathway between dansyl chloride and oxamniquine
© Copyright Policy
Related In: Results  -  Collection

Show All Figures
getmorefigures.php?uid=PMC2266787&req=5

Sch1: Proposed reaction pathway between dansyl chloride and oxamniquine
Mentions: The stoichiometry of the reaction was studied adopting the limiting logarithmic method [29]. The fluorescence intensity of the reaction product was alternatively measured in the presence of excess of either dansyl chloride or OXM. A plot of log fluorescence versus log [dansyl chloride] and log [OXM] gave straight lines, the values of the slopes are 0.901 and 0.984 respectively (Fig. 6). Hence, it is concluded that, the molar reactivity of the reaction is 0.901/0.984, i.e. the reaction proceeds in the ratio of 1:1. Based on the observed molar reactivity of the reaction, and depending on the presence of secondary amino group and by analogy to similar reports dealing with the reaction of dansyl chloride with compounds containing secondary amino group, the reaction pathway proposed in Scheme 1 is presented.Fig. 6

Bottom Line: The proposed method was successfully applied to the analysis of commercial capsules.The results obtained were in good agreement with those obtained using the official spectrophotometric method.A proposal of the reaction pathway was presented.

View Article: PubMed Central - PubMed

Affiliation: Department of Analytical Chemistry, Faculty of Pharmacy, University of Mansoura, Mansoura, Egypt. nelenany1@yahoo.com

ABSTRACT
A sensitive, simple and selective spectrofluorimetric method was developed for the determination of oxamniquine (OXM) in pharmaceutical formulations and biological fluids. The method is based on the reaction between the drug and 1-dimethylaminonaphthalene-5-sulphonyl chloride (dansyl chloride) in presence of 0.5 M sodium carbonate (pH 10) to yield a highly fluorescent derivative that is measured at 445 nm after excitation at 335 nm. The different experimental parameters affecting the development and stability of the reaction product were carefully studied and optimized. The fluorescence concentration plot was rectilinear over the range of 0.02-0.2 microg ml(-1) with a lower detection limit (LOD) of 0.007 microg ml(-1) and limit of quantitation (LOQ) of 0.02 microg ml(-1). The proposed method was successfully applied to the analysis of commercial capsules. The results obtained were in good agreement with those obtained using the official spectrophotometric method. Furthermore, the method was applied for the determination of oxamniquine in spiked human plasma, the mean % recovery (n = 4) is 97.77 +/- 1.19. A proposal of the reaction pathway was presented.

Show MeSH