A simple, rapid, sensitive, and accurate extractive spectrophotometric method has been developed for the determination of seven nonsteroidal anti-inflammatory drugs (NSAIDs) – namely diclofenac sodium, ibuprofen, indomethacin, ketoprofen, ketorolac tromethamine, mefenamic acid, and naproxen -- in pure forms as well as their pharmaceutical dosage forms (tablets, capsules, effervescent granules, syrups, oral drops, ampules, eye drops, gels, and suppositories). The method depends on the formation of an intensely colored ion-pair complex between the acidic drug and methylene blue in alkaline medium. The complex is stable and extractable into methylene chloride. All parameters were optimized. Beer-Lambert’s law was obeyed in concentrations ranging from 0.04 to 9 μg/mL. Statistical analysis of the calibration data was carried out, and correlation coefficients were in the range from 0.9996 to 0.9998. The developed method was fully validated according to International Conference on Harmonization guidelines, and complied with U.S. Pharmacopeia guidelines. The proposed method was applied to the analysis of the investigated drugs in their pharmaceutical formulations, and good recoveries were obtained. The results obtained were compared with those of reported and official methods, and no significant differences were found with t- and F-tests. Interference effects of some compounds usually present in combination with NSAIDs were studied, and the tolerance limits of these compounds were determined.

Cefpodoxime proxetil (CFP), a broad-spectrum third-generation cephalosporin, has been used most widely in the treatment of respiratory and urinary tract infections. For bioequivalence study of CFP in rabbit plasma, it was necessary to develop a highly sensitive and selective high-performance liquid chromatographic (HPLC) method with fluorescence (FL) detection. The pre-column labeling of cefpodoxime acid (CFA) (active metabolite) with an efficient benzofurazan type fluorogenic reagent, 4-N,N-dimethylaminosulfonyl-7-fluoro-2,1,3-benzoxadiazole (DBD-F) was carried out in the present study in 100 mM borate buffer (pH = 8.5) at 50°C for 15 min. The obtained fluorescent products were separated on C18 column with an isocratic elution of the mobile phase, which consists of 10 mM phosphate buffer(pH = 3.5)/CH3CN (70:30, v/v). The fluorescent product (DBD-CFA) was detected fluorimetrically at 556 nm with an excitation wavelength of 430 nm. Cefotaxime sodium was used as internal standard. The method was validated according to the requirements of US-FDA guidelines. The correlation coefficient of 0.999was obtained in the concentration ranges of 10-1000 ng mL-1. The limits of detection and quantification (S/N = 3) were 3 and 10 ng mL-1, respectively. Plasma CFA levels were successfully determined in rabbit with satisfactory precision and accuracy. The proposed HPLC-FL method was successfully applied to study bioequivalence in rabbits for two formulations of different brands contained CFP (prodrug) in a randomized, two-way, single-dose, crossover study and all pharmacokinetic parameters for the two formulations were assessed.

Context: Identification of optimal solid form of an active pharmaceutical ingredient and form control are very important in drug development. Thus, the structural information of these forms and in-depth insight on the modes of molecular interactions are necessary, and vibrational spectroscopic methods are well suited for this purpose. Objective: In-depth structural analysis of different solid forms of indomethacin (IND) using Raman and infrared (IR) spectroscopy is the objective. We have investigated the modes of molecular interactions in polymorphs ( and ), amorphous and discovered cocrystals of IND with nicotinamide (NIC) and trans-cinnamic acid (CIN) coformers. Materials and methods: The solid forms of IND have been prepared; their purity has been verified by differential scanning calorimetry and powder X-ray diffractometry and then studied in the solid-state by Raman and IR spectroscopy. The modes of the interactions were closely investigated from the vibrational data. Results: The key vibrational features of IND solid forms have been specified. The IR (C=O) band at 1713 cm-1 attributed to cyclic acid dimer of  IND has disappeared in IND–NIC/CIN whilst retained in IND–SAC cocrystal. Discussion: IND cocrystallizes in different conformations and crystal lattices with different coformers. The cyclic acid dimer of IND has been kept on its cocrystallization with saccharin and it could have been broken with NIC and CIN. Conclusions: The complementary nature of Raman and IR spectroscopy allowed unambiguous investigation of the chemical composition of pharmaceutical materials which is of particular importance in the absence of detailed structural information, as in the case of IND–NIC and IND–CIN.

A simple, selective, precise, and stability-indicating thin-layer chromatographic method has been developed and validated for analysis of some angiotensin II receptor antagonists (AIIRAs), namely, Losartan potassium (Los-K), Irbesartan (Irb), and Candesartan cilexetil (Cand) in the bulk drug and in pharmaceutical formulations (tablets). The method was based on using TLC plates pre-coated with silica gel G 60 on aluminum sheets as stationary phase and the development system was performed using chloroform:methanol (9:1) giving well separated and compact spots for all the studied drugs (RF values 0.41–0.53). The separated spots were characterized by viewing under the UV lamp, then visualized as orange spots by spraying with Dragendorff’s reagent and measured by densitometry. Under the optimum chromatographic conditions, linear relationships were obtained between response and concentrations of each studied drug with high correlation coefficients (0.9985–0.9994). Good accuracy and precision were successfully obtained for the analysis of tablets containing each drug alone or combined with diuretic drug hydrochlorothiazide (HCTZ). No interferences could be observed from the co-formulated HCTZ, commonly encountered excipients present in tablets as well as the degradation products. The results were compared successfully with reported methods and can be used as a stability-indicating assay.

A simple, selective, precise, and stability-indicating thin-layer chromatographic method has been developed and validated for analysis of some angiotensin II receptor antagonists (AIIRAs), namely, Losartan potassium (Los-K), Irbesartan (Irb), and Candesartan cilexetil (Cand) in the bulk drug and in pharmaceutical formulations (tablets). The method was based on using TLC plates pre-coated with silica gel G 60 on aluminum sheets as stationary phase and the development system was performed using chloroform:methanol (9:1) giving well separated and compact spots for all the studied drugs (RF values 0.41–0.53). The separated spots were characterized by viewing under the UV lamp, then visualized as orange spots by spraying with Dragendorff’s reagent and measured by densitometry. Under the optimum chromatographic conditions, linear relationships were obtained between response and concentrations of each studied drug with high correlation coefficients (0.9985–0.9994). Good accuracy and precision were successfully obtained for the analysis of tablets containing each drug alone or combined with diuretic drug hydrochlorothiazide (HCTZ). No interferences could be observed from the co-formulated HCTZ, commonly encountered excipients present in tablets as well as the degradation products. The results were compared successfully with reported methods and can be used as a stability-indicating assay.

A simple, selective, precise, and stability-indicating thin-layer chromatographic method has been developed and validated for analysis of some angiotensin II receptor antagonists (AIIRAs), namely, Losartan potassium (Los-K), Irbesartan (Irb), and Candesartan cilexetil (Cand) in the bulk drug and in pharmaceutical formulations (tablets). The method was based on using TLC plates pre-coated with silica gel G 60 on aluminum sheets as stationary phase and the development system was performed using chloroform:methanol (9:1) giving well separated and compact spots for all the studied drugs (RF values 0.41–0.53). The separated spots were characterized by viewing under the UV lamp, then visualized as orange spots by spraying with Dragendorff’s reagent and measured by densitometry. Under the optimum chromatographic conditions, linear relationships were obtained between response and concentrations of each studied drug with high correlation coefficients (0.9985–0.9994). Good accuracy and precision were successfully obtained for the analysis of tablets containing each drug alone or combined with diuretic drug hydrochlorothiazide (HCTZ). No interferences could be observed from the co-formulated HCTZ, commonly encountered excipients present in tablets as well as the degradation products. The results were compared successfully with reported methods and can be used as a stability-indicating assay.

A phytochemical study of the aerial parts of Blepharis ciliaris (L.) B.L. Burtt. led to the isolation of one new isoflavone glycoside caffeic acid ester: genistein-7-O-(6"-O-E-caffeoyl--D-glucopyranoside) (4), along with seven known compounds: methyl veratrate (1), methyl vanillate (2), protocatechuic acid (3), naringenin-7-O-(3"-acetyl-6"-E-p-coumaroyl--D-glucopyranoside) (5), naringenin-7-O-(6"-E-p-coumaroyl--D-glucopyranoside) (6), apigenin-7-O-(6"-E-p-coumaroyl--D-glucopyranoside) (7), and acteoside (8). Their structures were established on the basis of detailed analyses of physical, chemical, and spectral data. Compounds 1, 2, 3, 6, and 8 were isolated for the first time from this plant. The antioxidant activity of the different extracts as well as for some of the isolated compounds was evaluated.

A phytochemical study of the aerial parts of Blepharis ciliaris (L.) B.L. Burtt. led to the isolation of one new isoflavone glycoside caffeic acid ester: genistein-7-O-(6"-O-E-caffeoyl--D-glucopyranoside) (4), along with seven known compounds: methyl veratrate (1), methyl vanillate (2), protocatechuic acid (3), naringenin-7-O-(3"-acetyl-6"-E-p-coumaroyl--D-glucopyranoside) (5), naringenin-7-O-(6"-E-p-coumaroyl--D-glucopyranoside) (6), apigenin-7-O-(6"-E-p-coumaroyl--D-glucopyranoside) (7), and acteoside (8). Their structures were established on the basis of detailed analyses of physical, chemical, and spectral data. Compounds 1, 2, 3, 6, and 8 were isolated for the first time from this plant. The antioxidant activity of the different extracts as well as for some of the isolated compounds was evaluated.

Fluoroquinolones (FQs) are among the most important antibacterial agents (synthetic antibiotics) used in human and veterinary medicine. They are employed against all bacterial infections, particularly against urinary tract infections and acute respiratory diseases. In the last decade, there was no review covering all different analytical methods used for the determination of fluoroquinolone antibiotics. The present review presented recently published different electrophoretic and chromatographic methods for determination of seven fluoroquinolones (ciprofloxacin, gatifloxacin, levofloxacin, lomefloxacin, norfloxacin, ofloxacin, and sparfloxacin). Presented applications concern analysis of chosen fluoroquinolones in pure forms, different pharmaceutical formulations, biological fluids, and environmental samples.

Fluoroquinolones (FQs) are among the most important antibacterial agents (synthetic antibiotics) used in human and veterinary medicine. They are employed against all bacterial infections, particularly against urinary tract infections and acute respiratory diseases. In the last decade, there was no review covering all different analytical methods used for the determination of fluoroquinolone antibiotics. The present review presented recently published different electrophoretic and chromatographic methods for determination of seven fluoroquinolones (ciprofloxacin, gatifloxacin, levofloxacin, lomefloxacin, norfloxacin, ofloxacin, and sparfloxacin). Presented applications concern analysis of chosen fluoroquinolones in pure forms, different pharmaceutical formulations, biological fluids, and environmental samples.