Authors:M. El-Tawoosy, N. Farouk, and A. El-Bayoumy
An adopted method for the preparation of high radiochemical purity 125I-atenolol was investigated. Direct radioiodination of atenolol was carried out using N-bromosuccinamide or hydrogen peroxide as an oxidizing agent. The reaction proceeds well within 30 min at room temperature
(25 ± 1 °C) and afforded a radiochemical yield up to 97% as pure as 125I-atenolol. Different chromatographic techniques (electrophoresis, TLC and HPLC) were used to determine the radiochemical
yield and purity of the labeled product. Biodistribution studies were carried out in normal Albino Swiss mice and the results
indicate that 125I-atenolol can be used safely as myocardial imaging agent.
Authors:P. Deore Deore, A. Shirkhedkar Shirkhedkar, and S. Surana Surana
A new simple, precise, accurate, and selective thin-layer chromatographic (TLC) method has been developed for simultaneous analysis of atenolol and lercanidipine hydrochloride in a tablet dosage form. Chromatographic separation was achieved on aluminum foil plates precoated with silica gel 60F254, with toluene-methanoltriethylamine 3.5:1.5:0.1 (v/v) as mobile phase. Detection was performed densitometrically at 275 nm. The RF of atenolol and lercanidipine hydrochloride were 0.24 and 0.68, respectively. The reliability of the method was assessed by evaluation of linearity (2000–12000 ng per band for atenolol and 400–2400 ng per band for lercanidipine hydrochloride), accuracy (98.94 ± 0.30% for atenolol and 99.75 ± 0.69% for lercanidipine hydrochloride), and specificity, in accordance with ICH guidelines. The method can be used for routine simultaneous analysis of atenolol and lercanidipine hydrochloride in pharmaceutical formulations.
Enantiomeric resolution of two commonly used β-blockers, namely, (±)-propranolol and (±)-atenolol, has been achieved on silica gel layers which were bulkimpregnated with β-cyclodextrin. Solvent systems DMF-ethyl acetate-butanol (3:2:5, υ/υ) and butanol-acetic acid-ethyl acetate-ammonia (5:2:2:0.5, υ/υ) successfully resolved the enantiomers of (±)-propranolol and (±)-atenolol, respectively. The spots were located with iodine vapor. The effects of concentration of the chiral selector and mobile phase variation were also studied.
Authors:A. B. Thomas, U. B. Chavan, R. K. Nanda, L. P. Kothapalli, S. N. Jagdale, S. B. Dighe, and A. D. Deshpande
Simultaneous analysis of atenolol (Atn), hydrochlorothiazide (Hctz) and losartan potassium (Los) in solid dosage forms has been achieved by reversed-phase high-performance liquid chromatography on a C18 column with a 0.035 M potassium dihydrogen orthophosphate-acetonitrile gradient as mobile phase and UV detection at 225 nm. The retention times for Atn, Hctz, and Los were 2.91, 4.75, and 7.52 min, respectively, with mean recoveries of 99.67, 99.89, and 100.69%. The method was validated in accordance with ICH guidelines. Because of its simplicity and high precision and accuracy, the method can be used for analysis of atenolol, hydrochlorothiazide and losartan potassium in pharmaceutical preparations.
Authors:H. M. Albishri, D. Abd El-Hady, and Roaa A. Tayeb
Pharmaceutical industry concerned recently with eco-friendly analytical methods to reduce the environmental pollution. The using of toxic organic solvents for the analysis of drugs is critical. In the current work, several simple and less costly approaches such as micellar and/or cyclodextrin liquid chromatography were discussed. A new eco-friendly and simple chromatographic analysis of the ternary mixture of amiloride hydrochloride (AM), atenolol (AT), and hydrochlorothiazide (HZ) in urine by hydroxypropyl-beta-cyclodextrin (HP-β-CD) bonded stationary phase was investigated. The experimental conditions were optimized and validated based on International Conference on Harmonization (ICH) Q2R1 guidelines to detect analytes by isocratic mobile phase of phosphate buffer (5.0 mmol L−1, pH 7.0) in the presence of 0.5 mL min−1 flow rate, 25.0 °C, and 280 nm. Linearity, accuracy, and precision were found to be acceptable over the concentration range of 0.05–20.0 μg mL−1 for AM, 0.05–50.0 μg mL−1 for AT and 0.05–50.0 μg mL−1 for HZ. The proposed method was precise, selective, and sensitive enough for the routine analysis of ternary mixture at therapeutic urine levels. The inclusion complexation and the appendant hydroxyl groups of HP-β-CD were considered the main reasons for assisting in adequate separation of the drugs. On the other hand, the presence of kosmotropic phosphate ions could solubilize the protein and could strengthen the selective inclusion of drugs inside HP-β-CD cavity. Urinary excretion studies showed that the detection of drugs is possible up to 24 h after their ingestion.
Authors:J.F.F. Anderson, M.C.G. Gerlin, R.A. Sversut, L.C.S. Oliveira, A.K. Singh, M.S. Amaral, and N.M. Kassab
The objective of this study was to develop and validate an assay method for simultaneous determination of atenolol, furosemide, losartan, and spironolactone in pharmaceutical formulations. A reverse-phase high-performance liquid chromatography procedure was developed, using a Kinetex® C-18 column (100 mm × 4.6 mm, 2.6 μm). The mobile phase was composed of methanol—water (75:25 v/v, pH 3.0, adjusted with phosphoric acid), with a flow rate of 0.4 mL min−1. All drugs were separated in less than 5 min. The method was validated according to International Conference on Harmonization (ICH) and Association of Official Analytical Chemists (AOAC) guidelines. The method showed linearity in a concentration range of 0.75–12.0 μg mL−1 for atenolol (r = 0.9995), 0.30–12.00 μg mL−1 for furosemide (r = 0.9997), 0.45–12.00 μg mL−1 for losartan (r = 0.9995), and 0.45–12.0 μg mL−1 for spironolactone (r = 0.9999). The method also showed repeatability and precision. The three-day average intra-day precisions were 101.35 ± 0.74% for atenolol, 95.84 ± 1.44% for furosemide, 98.90 ± 1.16% for losartan, and 97.19 ± 0.18% for spironolactone. Similarly, the inter-day precisions were 101.34 ± 0.72% for atenolol, 95.84 ± 0.1.50% for furosemide, 98.90 ± 1.17% for losartan, and 97.19 ± 0.83% for spironolactone. The method accuracy was also tested and validated — in this case, the average recovery values were 100.18 ± 1.20% for atenolol, 99.83 ± 1.54% for furosemide, 100.07 ± 0.95% for losartan, and 99.94 ± 0.93% for spironolactone. Finally, the method was successfully applied in the simultaneous determination of atenolol, furosemide, losartan, and spironolactone in magisterial formulas, as well as in commercial pharmaceutical formulations.
Authors:Hariom Nagar, Jürgen Martens, and Ravi Bhushan
Enantioresolution of three active pharmaceutical ingredients (APIs), namely, atenolol, betaxolol, and orciprenaline, marketed as racemic mixture, has been achieved in a direct mode using (S)-glutamic acid as chiral additive in thin-layer chromatography. Two different approaches were adopted: (1) (S)-glutamic acid was mixed in the silica gel slurry for making thin-layer plates, or (2) it was added in the mobile phase and plain plates without any chiral additive were used. Both (1) and (2) were capable of separating enantiomers of all the three racemates, but different combinations and proportions of solvents were found successful in the two cases. Good resolution was achieved in both cases, and the results are compared for these two sets of studies among themselves and with other literature reports. Iodine was used to locate the spots of the corresponding enantiomers. The detection limits for each enantiomer were found in the range of 1.4–1.9 μg (per spot).
Authors:M. Freitas, R. Alves, J. Matos, and J. Marchetti1
Osmotically controlled and oral drug delivery
systems utilize osmotic pressure for controlled delivery of active agent(s).
Drug delivery from these systems, to a large extent, is independent of the
physiological factors of the gastrointestinal tract and these systems can
be utilized for systemic as well as targeted delivery of drugs. We apply the
thermal methods and IR spectroscopy to study compatibility between atenolol
and several excipients usually found in the osmotic systems formulations (Polyethylene
oxide, MW 3350, 100000, 200000 and 5000000;
HPMC K4000, magnesium stearate and cellulose acetate.
acetate, HPMC K4000 and magnesium stearate have essentially no interaction
with atenolol otherwise all Polyethylene oxide excipients modifies significantly
the drug melting point indicating some extend of interaction.