Simultaneous Determination of Ceftazidime in Three Different Pharmaceutical Preparations Combined with Either Tazobactam, Tobramycin or Sulbactam by HPTLC-Spectrodensitometric Method.

A new, simple hight performance thin layer chromatography (HPTLC)-Spectrodensitometric strategy was created and approved for the synchronous estimation of four antibacterial specialists: ceftazidime (CEF), tazobactam (TAZ), tobramycin (TOB) and sulbactam (SUL). The four compounds were separated on TLC aluminum plates covered with silica gel 60 F254, using chloroform-acetonitrile-methanol-ammonia (4:1:0.5:0.15, v/v/v/v) as a mobile phase at 254 nm. Linear correlation was obeyed over the concentration ranges of 12.0-72.0, 2.0-12.0, 3.0-18.0 and 10.0-50.0 µg mL-1 for CEF, TAZ, TOB and SUL, respectively. The proposed approach is efficient, repeatable and convenient as a flexible method for the quality control of diverse combinations of these pharmaceuticals in various pharmaceutical preparations, with high percent recoveries that are highly consistent with labeled data. When the findings of the proposed technique were compared to those of the comparison methods, there were no critical contrasts in terms of precision and accuracy.

A novel spectrofluorimetric method for determination of lomefloxacin adopting on zinc(II) chelation strategy: Application in human plasma.

A new sensitive and instantaneous spectrofluorimetric method for efficient determination of lomefloxacin (LMX) in its pure, dosage form and human plasma was designed. The developed method depends on formation of a metal-chelation compound of LMX as a ligand with zinc(II) in a buffer of acetate (pH 5.5). The following parameters; type of metal, concentration of metal, pH, type of buffer and diluting solvent were optimized. After carefully investigation; 0.2 mM zinc, 2.0 ml acetate buffer (pH 5.5) and water as diluting solvent were set as optimum reaction conditions. Under these conditions, a large increase in the intensity of the fluorescence of LMX was attained at 450 after excitation at 284 nm. The limits of detection and quantification were 5.8 and 1.9 ng ml-1 , respectively, with linearity range of 10.0 to 500.0 ng ml-1 . The binding mode of LMX and zinc(II) ion (Zn2+ ) was found to be 2:1, respectively, and confirmed by Job's plot method. Furthermore, it extended to the analysis of LMX in the spiked plasma of humans with percentage recovery (98.70 ± 0.97 to 100.30 ± 1.69%, n = 3).

Benzofurazan -based fluorophore for the spectrofluorimetric determination of 6-Aminocaproic acid: Application to spiked human plasma and urine.

6-Aminocaproic acid is one of the most widely used antihemorrhagic and antifibrinolytic agent, therefore, it is essential to create a novel, sensitive, low cost and straightforward spectrofluorimetric method for its determination. The nucleophilic substitution interaction between the primary amine of 6-aminocaproic acid with 4-chloro-7-nitro benzofurazan (NBD-Cl) generated a yellow product. The reaction proceeded in borate buffer (pH 9) and its fluorescence has been measured at 525 nm after excitation at 472 nm. All of the parameters that have impact on the performance of the developed method were investigated and optimized. The range of linearity was 0.1-0.7 µg/mL while, the quantitation limit was down to 0.101 µg/mL and limit of detection was 0.033 µg/mL. This approach was effectively employed to evaluate the content of 6-aminocaproic acid in laboratory prepared dosage form with average percentage recovery of 100.19 ± 0.72% without any interference from basic excipients. Moreover, the proposed method was extended to determine 6-aminocaproic acid in spiked human plasma and urine.

Sensitivity improvement for spectrofluorimetric determination of commonly used antifungal drug 'nystatin': application for oral suspension.

In this paper, two simple, rapid and highly sensitive spectrofluorimetric methods were developed and validated for nystatin determination in its pure form and pharmaceutical dosage form (oral suspension). The first method was based on measuring the nystatin native fluorescence after dilution with isopropyl alcohol at 407 nm (excitation 303 nm). The fluoresence intensity was linearly dependant on the nystatin concentration within the specified range 50-500 ng ml-1 . The second was based on micellar enhancement of nystatin fluorescence using sodium dodecyl sulphate (SDS). In the presence of 2% w/v SDS, an ~1.9-fold enhancement could be achieved in the relative fluorescence intensity of nystatin. The linear range for the second method was 20-100 ng ml-1 . The limits of quantification and detection were found to be 43.23 ng ml-1 and 14.27 ng ml-1 (Method I), 6.08 ng ml-1 and 2.0 ng ml-1 (Method II). According to percentage recoveries and relative standard deviations (RSDs) obtained, the proposed methods were precise (RSDs were less than 2%), reproducible, and accurate and could be successfully applied for quantitative estimation of nystatin in its dosage form. The statistical results of this method were compared with that of the reported method and showed excellent agreement with respect to accuracy and precision.

An innovational validated spectrofluorimetric technique for determination of 6-Aminocaproic acid in pure form and its tablet: Application to spiked human plasma and urine.

An innovative and sensitive spectrofluorimetric method has been developed for determination of 6-aminocaproic acid (ACA) in its pure form and its laboratory prepared tablets. The aim of this method is the reaction of ethyl acetoacetate and formaldehyde with the primary amino group presented in ACA as aimed in the Hantzsch reaction, this reaction resulted in formation of a yellow fluorescent dihydropyridine derivative that can be easily detected spectrofluorimetrically at 438 nm (excitation at 358 nm). At the optimum conditions of the reaction, the linear range was found to be (0.7-3.5 µg\mL) with limit of detection is 0.231 µg\mL and limit of quantitation is 0.700 µg\mL. The proposed method used for detection of ACA laboratory prepared tablets with average percentage 100.721 ±â€¯0.701% without any interference from any excipients. This method used for in vitro determination of ACA in spiked human plasma with a percent mean recovery 99.874 ±â€¯1.416%. In addition, the developed method used for determination of ACA in spiked human urine with percent mean recovery 100.314 ±â€¯1.793%.

Design and strategy for spectrofluorimetric determination of tranexamic acid in its authentic form and pharmaceutical preparations: application to spiked human plasma.

A creative, very sensitive and noncomplicated spectrofluorimetric technique was established and further validated to determine tranexamic acid in both its authentic form and its pharmaceutical preparation dosage forms. In the introduced technique, a reaction was found between the aliphatic primary amino group of tranexamic acid and ninhydrin/phenylacetaldehyde reagents in the presence of Torell and Steinhagen buffer pH 7.0, which led to the production of a highly fluorescent product; fluorescence intensity was measured at 475 nm after excitation at 391 nm. A calibration curve was drawn with a linear range of 0.3-2 µg/ml. Limit of detection and limit of quantification values were 0.051 and 0.155 µg/ml respectively. The introduced technique was validated based on the International Council for Harmonisation guidelines and agreed for determination of tranexamic acid in its pharmaceutical formulation. Finally, this simple method was also applied for determination of tranexamic acid in spiked human plasma.

Utilization of a complex arrangement approach for spectroscopic examination with Eosin Y of various cephalosporins in their pure or pharmaceutical dosage forms, and in human plasma.

Approved, basic, effective and successful spectroscopic strategies (spectrophotometric and spectrofluorimetric) were created to measure seven cephalosporins: cefpiramide (I), cefuroxime (II), cefoxitin (III), ceftazidime (IV), cefpirome (V), ceftobiprole (VI), and ceftriaxone (VII). These strategies used a two-fold complex arrangement response for the drug amino groups with Eosin Y (EY). The examined drugs were determined spectrophotometrically at 542-550 nm in acetic acid derivative buffer. The examined drugs were determined spectrofluorimetrically by measuring their quenching effect on EY local fluorescence at 545 nm after excitation at 305 nm. The absorbance-intensity plots were rectilinear over the ranges 20-100, 10-130, 20-220, 30-230, 10-210, 20-180 and 10-130 µg ml-1 for I, II, III, IV, V, VI, and VII samples, respectively. The fluorescence-intensity plots were rectilinear over the ranges 0.5-1.5, 0.1-0.9, 0.3-1.5, 0.5-2.5, 0.1-0.9, 0.5-2.5 and 0.1-1.0 µg ml-1 for I, II, III, IV, V, VI, and VII samples, respectively. The recommended materials were certified as adhering to International Council for Harmonisation (ICH) guidelines and were used to examine the tested drugs in different dosage forms and in human plasma tests. The approved materials matched the reference materials.

Derivatization of tranexamic acid for its rapid spectrofluorimetric determination in pure form and pharmaceutical formulations: Application in human plasma.

An ingenious approach for determination of tranexamic acid spectrofluorimetrically has been developed. This experiment is very simple, sensitive and selective method for determination of tranexamic acid in pure form, pharmaceutical dosage forms and in spiked human plasma. All optimal conditions needed in our proposed experiment have been determined and validated precisely. This developed method based on the reaction between the primary amino group found in the chemical structure of tranexamic acid with the fluorescamine reagent in presence of borate buffer (pH 8.3) that result in the formation of fluorescence product measured at 473.5 nm after excitation at 392 nm. We notice that the linearity of the resulted calibration curve found to be (0.1-0.9 µg/mL) with LOD and LOQ results were 0.0237 and 0.0719 respectively. The validation of the developed method is according to the international council for Harmonization (ICH) guidelines indicating good accuracy and precision. Finally, the developed method has been applied for in vitro study of tranexamic acid by making spiked human plasma with a mean percentage recovery 99.430 ± 0.623 as well as in its pharmaceutical dosage forms tablets and ampoules.

Spectrofluorimetric approach for determination of tranexamic acid in pure form and pharmaceutical formulations; Application in human plasma.

Tranexamic acid (TXA) is an important antihemorrhagic drug that needs a simple, sensitive and low cost spectrofluorimetric method for its determination. This method depends on generation of a yellow product which produced from a nucleophilic substitution reaction of the lone pair of electrons on the amino group found in the TXA chemical structure and 4-chloro-7-nitrobenzofurazan (NBD-Cl) in borate buffer PH 9.0. The product was measured at 536 nm (λex = 470.5 nm). All variables that have an effect on the formation and stability of the product have been explored and optimized. The linear range was 20-100 ng mL-1 with a limit of quantitation 12.4 ng mL-1. This method has been applied for assurance of tranexamic acid in ampoules and tablets dosage forms without any interference from excipients present. Also, we study the drug in human plasma.