Electrochemical Quantitative Assessment of Labetalol Hydrochloride in Pure Form and Combined Pharmaceutical Formulations.

This work describes how to utilize the electrochemical technique to determine labetalol hydrochloride (Lab) in pure form and combined pharmaceutical formulation for quality control purposes. Four membrane sensors were developed using two plasticizers, dioctyl phthalate with 2-hydroxypropyl-?-cyclodextrin and ammonium reineckate (RNC) for sensors 1a and 2a, and tributyl phthalate with 2-hydroxypropyl-?-cyclodextrin and ammonium reineckate for sensors 1b and 2b as ionophores in polyvinyl chloride (PVC) matrix. Fast response and stable Nernstian slopes of 59.60, 57.58, 53.00 and 55.00 mV/decade for sensors 1a, 2a, 1b, and 2b, respectively, were obtained by developed sensors within a concentration range 10-4 M-10-2 M over pH range 2.00-5.10. Developed sensors showed good selectivity for Lab in pure form, in the presence of co-administered drugs, many of interfering ions, and excipients present in pharmaceutical formulation. No remarkable difference was detected upon the statistical comparison between the results of proposed sensors and the official method.

Miniaturized membrane sensors for the determination of rivastigmine hydrogen tartrate.

Novel miniaturized polyvinyl chloride (PVC) membrane sensors in all-solid state graphite and platinum wire supports were developed, electrochemically evaluated and used for the assay of rivastigmine hydrogen tartrate drug (RIV). The RIV sensors are based on the formation of an ion-association complex between the drug cation and tetrakis(4-chlorophenyl)borate (TpClPB) anionic exchanger as electroactive material dispersed in a PVC matrix. Linear responses of 10(-2) - 10(-5) M and 10(-2) - 10(-4) M with cationic slopes of 56.4 mV and 53.6 mV over the pH range 4 - 7 were obtained by using the RIV-coated graphite (sensor 1) and platinum wire (sensor 2) membrane sensors, respectively. The proposed method displays useful analytical characteristics for the determination of RIV in Exelon capsules with average recoveries of 100.01+/-0.835, 100.09+/-0.896, and in plasma with average recoveries of 99.47+/-0.97, 99.58+/-0.82, and in rat brain homogenate with average recoveries of 98.16+/-1.62, 99.02+/-1.57, for sensors 1 and 2, respectively. The methods were also used to determine the intact drug in the presence of its degradation product and thus could be used as stability indicating methods. The results obtained by the proposed procedures were statistically analyzed and compared with those obtained by using a reported method. No significant difference for both accuracy and precision was observed.

Stability indicating methods for the determination of some fluoroquinolones in the presence of their decarboxylated degrades.

Two stability-indicating methods, namely densitometric TLC and derivative spectrophotometry for the determination of the fluoroquinolone antibacterials lomefloxacin (Lfx), moxifloxacin (Mfx), and sparfloxacin (Sfx) in the presence of their acid degrades are described. Acid degradation was adopted and the main decarboxylated product separated by TLC. Degradation products were identified confirming a previously mentioned degradation scheme. The densitometric method is based on the separation of the intact drug from its acid degradation product on silica gel G plates using different mobile phases and the spots of the intact drugs were scanned at 288, 290, and 292 nm for Lfx, Mfx, and Sfx, respectively. The derivative spectrophotometric method utilizes first derivative D(1) UV spectrophotometry with zero crossing points at 295.2 nm for Lfx, 280.4 and 303.4 nm for Mfx, and 280.8 nm for Sfx. Regression analysis of Beer's plots showed good correlation in the concentration ranges 0.2-1.2, 0.1-1.4, and 0.5-2.0 microg/spot for Lfx, Mfx, and Sfx, respectively, in the densitometric method and 2-16 microg/ml for all drugs in the derivative spectrophotometric method. The proposed methods were successfully applied for the determination of the investigated drugs in bulk powder with mean percentage accuracy ranges from 98.93 to 101.25% for the TLC method and from 98.18 to 100.35% for the D(1) method. The proposed methods were also applied for the determination of the investigated drugs in their pharmaceutical dosage forms and their validity was assessed using the standard addition technique with mean percentage recovery ranging from 100.25 to 101.70% in the TLC method and from 99.27 to 102.12% in the D(1) method. The selectivity of the proposed methods was tested by the analysis of laboratory-prepared mixtures containing different percentages of the studied drugs and their acid degrades. The proposed methods were found selective for the determination of the intact drugs in the presence of up to 90% of their degrades in the TLC method and 70% for Lfx and 90% for Mfx and Sfx in the D(1) method.