Authors:Hanadi A. Al Shaker, Nidal A. Qinna, Hamza Al Hroub, Mahmoud M. H. Al Omari, and Adnan A. Badwan
Propranolol is chemically described as 2-propanol, 1-[(1-methylethyl) amino]-3-(1-naphthalenyloxy) (Figure 1 ). Propranolol is a highly lipophilic drug that is almost completely absorbed from the gastrointestinal
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. Mohan, S. Dhayalamurthi, P. Anandan, and D. Saravanan
The present study reports the dissolution method for a novel fixed dose combination (FDC) containing etodolac (ET) and propranolol hydrochloride (PH) developed utilizing USP Apparatus 1 (basket) at 100 rpm with 1000 mL of phosphate buffer (pH 6.8; 0.05 M) medium at 37°C. An isocratic reversed-phase liquid chromatographic (RPLC) method was also developed for the simultaneous determination of ET and PH on an octadecylsilica column using phosphate buffer (pH 5.5) and acetonitrile (60:40, υ/υ) as the mobile phase with ultraviolet (UV) detection at 292 nm. Validation data were obtained, which demonstrated that the dissolution methodology is accurate, precise, linear, and rugged for the combination tablets.
Authors:A. K. Shakya, N. M. Hakooz, T. A. Arafat, A. N. A. Abu-Awwad, J. A. El-Ghani, and M. Melhim
A sensitive and specific high-performance liquid chromatographic-electrospray ionization tandem mass spectrometric (HPLC-ESI-MS-MS) method for quantification of tamsulosin in human plasma, using propranolol as internal standard (IS), has been developed, validated successfully, then used in a clinical study. Plasma (0.5 mL) was mixed with 50 μL 1 m sodium carbonate solution. Tamsulosin and propranolol were isolated from the mixture by liquid-liquid extraction with 7:3 (v/v) hexane-ethyl acetate. Reversed-phase chromatography was performed on a C8 column at 25°C with 70:30:0.1 (v/v) methanol-water-formic acid as mobile phase at a flow-rate of 1.0 mL min−1. Quantification was achieved in positive-ion mode by monitoring the product ions at m/z 409.1 → 270.9, 228.0, and 200.0 (tamsulosin) and m/z 260.1 → 183.0 (IS). The lowest limit of quantification was 0.25 ng mL−1, and the calibration range was 0.25–50 ng mL−1. Within and between batch precision (expressed as coefficient of variation, CV) did not exceed 10.8% and accuracy was within 5.0% deviation of the nominal concentration. Recovery of tamsulosin from plasma was >83.0%. The validated method was used for clinical study of tamsulosin in human volunteers.
Authors:Beáta Szalóczi, Ágnes Harmath, Barbara Pete, Eszter Kovács, János Rigó jr., and Júlia Hajdú
A szerzők egy Basedow–Graves-kór miatt korábban thyreoidectomián átesett, kezeletlen anya koraszülöttjének esetét ismertetik. Gondozatlan terhességből magzati tachycardia, fenyegető intrauterin asphyxia miatt sürgős császármetszéssel született a 33. hétnek megfelelő érettségű, 1350 gramm súlyú, dysmaturus (testsúlypercentil <10), nagy nyaki strumával bíró koraszülött. Az újszülött respiratoricus elégtelenség miatt konvencionális és magas frekvenciás gépi lélegeztetésben részesült, súlyos tachycardia (>180/perc), cardialis decompensatio miatt béta-blokkoló, digoxin- és dobutaminterápiát igényelt. Kivizsgálása során cardiomegalia, pericardialis folyadékgyülem, súlyos tüdőhypoplasia, mitralis és tricuspidalis insufficientia, hepatosplenomegalia igazolódott. A pajzsmirigy-szabadhormonok szintje többszörösen meghaladta a referenciaértéket (fT4: > 6 ng/dl, fT3: > 30 pg/ml), a TSH-szint ugyanakkor 0 volt. Légzéstámogatást 7, keringéstámogatást 10 napig igényelt, propranolol- mellett K-jodid-kezelésben részesült. Tachycardiája mérséklődött, a béta-blokkoló kezelést csökkentett adagban kapta tovább, pajzsmirigyhormonszintjei fokozatosan a normális tartományba kerültek. A szerzők felhívják a figyelmet arra, hogy a Basedow–Graves-kórban szenvedő anya újszülöttjénél jelentős súlybeli, növekedésbeli elmaradás, súlyos keringési elégtelenség, thyreotoxicosis tünetei alakulhatnak ki, és hangsúlyozzák az anyai hormon-, valamint antitestszintek nyomon követésének jelentőségét.
Authors:D. S. Patel, N. Sharma, M. C. Patel, B. N. Patel, P. S. Shrivastav, and M. Sanyal
A rapid, selective, and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay has been proposed for the determination of aripiprazole in human plasma. The analyte and propranolol as internal standard (IS) were extracted from 200 μL of human plasma via liquid-liquid extraction using methyl tert-butyl ether under alkaline conditions. The best chromatographic separation was achieved on an Aquasil C18 (100 × 2.1 mm, 5 μm) column using methanol-deionized water containing 2 mM ammonium trifluoroacetate and 0.02% formic acid (65:35, v/v) as the mobile phase under isocratic conditions. Detection of analyte and IS was done by tandem mass spectrometry, operating in positive ion and multiple reaction monitoring (MRM) acquisition mode. The method was fully validated for its selectivity, interference check, sensitivity, carryover check, linearity, precision and accuracy, reinjection reproducibility, recovery, matrix effect, ion suppression/enhancement, stability, ruggedness, and dilution integrity. The assay was linear over the concentration range of 0.10–100 ng mL−1 for aripiprazole. The intra-batch and inter-batch precision (%CV) was ≤4.8%, while the mean extraction recovery was >96% for aripiprazole across quality control levels. The method was successfully applied to a bioequivalence study of 10 mg aripiprazole orally disintegrating tablet formulation in 27 healthy Indian subjects under fasting and fed condition. The reproducibility in the measurement of study data was demonstrated by reanalysis of 260 incurred samples.
Authors:F. Belal, A. M. El-Brashy, N. El-Enany, and M. M. Tolba
A simple, accurate, and sensitive reversed-phase HPLC method was developed for the simultaneous determination of celiprolol HCl (CE) and chlorthalidone (CT). Good chromatographic separation was achieved using a 250 mm × 4.6 mm i.d., 5 μm particle size Hypurity C8 column. Mobile phase containing a mixture of methanol and 0.04 M phosphate buffer (35:65, υ/υ) at pH 7.0 was pumped at a flow rate of 1.2 mL min−1 with UV detection at 225 nm. Lisinopril dihydrate (LIS) was used as internal standard. The method showed good linearity in the ranges 0.2–20 and 0.2–10 μg mL−1 with limits of detection 0.06 and 0.04 μg mL−1 and limits of quantification 0.20 and 0.14μg mL−1 for CE and CT, respectively. The suggested method was successfully applied to the simultaneous analysis of the studied drugs in their synthetic mixture and coformulated tablet. The method was further extended to the determination of CE in biological fluids. The proposed method was also applied to the determination of the studied drugs in presence of some coadministered or related drugs such as atenolol, propranolol, acetazolamide, enalapril, nicardipine, triamterene, and hydrochlorothiazide without any interference.