02198nas a2200181 4500008004100000022001400041245014500055210006900200260008000269300001200349490000700361520143000368100002601798700002401824700002501848700002101873856012201894 2009 eng d a1060-327100aApplication of a stability-indicating thin-layer chromatographic method to the determination of tenatoprazole in pharmaceutical dosage forms0 aApplication of a stabilityindicating thinlayer chromatographic m a481 N FREDRICK AVE, STE 500, GAITHERSBURG, MD 20877-2504 USAbAOAC INTcMAR a387-3930 v923 a

A sensitive, selective, precise, and stability-indicating thin-layer chromatographic (TLC) method was developed and validated for the determination of tenatoprazole both as a bulk drug and in formulation. The method uses TLC aluminum plates precoated with Silica Gel 60(F-254) as the stationary phase and the solvent system toluene-ethyl acetate-methanol (6 + 4 + 1, v/v/v). This system gave compact spots for tenatoprazole (R(f) value of 0.34 +/- 0.02). Tenatoprazole was subjected to acid and alkali hydrolysis, oxidation, and photodegradation. The peaks of the degradation products were well-resolved from that of the pure drug and had significantly different Rf values. Densitometric analysis of tenatoprazole was performed in the absorbance mode at 306 nm. The linear regression analysis data for the calibration plots showed a good linear relationship over the concentration range of 100-1500 ng/spot. The mean values of the correlation coefficient, slope, and intercept were 0.9989 +/- 1.42, 10.27 +/- 0.965, and 4894.2 +/- 1.24, respectively. The method was validated for precision, robustness, and recovery. The limit of detection and limit of quantitation were 50 and 100 ng/spot, respectively. Statistical analysis showed that the method is repeatable and selective for estimation of tenatoprazole. Because the method can separate the drug from its degradation products, it can be used to monitor stability.

1 aDhaneshwar, Sunil, R.1 aBhusari, Vidhya, K.1 aMahadik, Mahadeo, V.1 aSanthakumari, B. uhttps://library.ncl.res.in/content/application-stability-indicating-thin-layer-chromatographic-method-determination-002218nas a2200157 4500008004100000245016200041210006900203260000800272300001200280490000700292520155300299100002601852700002501878700002501903856013201928 2009 eng d00aColumn liquid chromatography-ultraviolet and column liquid chromatography/mass spectrometry evaluation of stress degradation behavior of escitalopram oxalate0 aColumn liquid chromatographyultraviolet and column liquid chroma cJAN a138-1470 v923 a

{The objective of this work was to study the degradation behavior of escitalopram oxalate under different International Conference on Harmonization (ICH)-recommended stress conditions by column liquid chromatography (LC)-UV and LC/mass spectrometry (LC/MS) and to establish a validated stability-indicating LC assay method. Escitalopram oxalate was subjected to stress conditions of hydrolysis, oxidation, photolysis, and thermal decomposition. Extensive degradation was found to occur in alkaline medium. Mild degradation was observed in acidic and oxidative conditions. Escitalopram oxalate was stable to neutral, photolytic, and thermal stress. Successful separation of the drug from degradation products formed under stress conditions was achieved on a PerfectSil-100 ODS-3 column [C(18) (5 mu m, 25 cm x 4.6 mm id)] using methanol-0.01 M acetate buffer pH 3.8 adjusted with acetic acid (45 + 55) as the mobile phase. The flow rate was 1 mL/min, and the detection wavelength was 239 nm. The method was validated according to ICH guidelines. Major degradation products formed in hydrolysis and oxidative conditions were isolated, and structural elucidation of degradation products was done by LC/MS and infrared spectrometry studies. The major hydrolysis degradation product was confirmed as 1-(3-dimethylaminopropyl)-1-(4-fluoro-phenyl)-1,3dihydroisobenzofuran-5- carboxylic acid, and the major oxidative degradation product was confirmed as 1-{[3-dimethylamino(oxide)-propyl]-1(4-flurophenyl)}-1,3-dihydro-iso benzofuran-5-carbonitrile.

1 aDhaneshwar, Sunil, R.1 aMahadik, Mahadeo, V.1 aKulkarni, Mahesh, J. uhttps://library.ncl.res.in/content/column-liquid-chromatography-ultraviolet-and-column-liquid-chromatographymass-spectrometry-002207nas a2200241 4500008004100000022001400041245008000055210006900135260010600204300001200310490000700322520133200329653000901661653003201670653001901702653001801721653001501739100002501754700002401779700002501803700002601828856011101854 2009 eng d a0731-708500aLC-UV and LC-MS evaluation of stress degradation behaviour of tenatoprazole0 aLCUV and LCMS evaluation of stress degradation behaviour of tena aTHE BOULEVARD, LANGFORD LANE, KIDLINGTON, OXFORD OX5 1GB, ENGLANDbPERGAMON-ELSEVIER SCIENCE LTDcDEC a787-7930 v503 a

In the present study, comprehensive stress testing of tenatoprazole was carried out according to ICH guideline Q1A (R2). Tenatoprazole was subjected to stress conditions of hydrolysis, oxidation, photolysis and neutral decomposition. Additionally, the solid drug was subjected to 50 degrees C for 60 days in dry-bath, and to the combined effect of temperature and humidity at 40 degrees C/75% RH. Extensive degradation was found to occur in acidic, neutral and oxidative conditions. Mild degradation was observed in basic conditions. The drug is relatively stable in the solid-state. The products formed under different stress conditions were investigated by LC and LC-MS. Successful separation of drug from degradation products formed under stress conditions was achieved on a Chemito ODS-3 column [C(18) (5 mu m, 250 mm x 4.6 mm, i.d.)] using methanol: 0.01 M acetate buffer pH 4.5 adjusted with glacial acetic acid (55:45) as the mobile phase at flow rate of 1 mL/min and the peak was detected using a UV detector set at 306 nm. The LC-MS m/z values and fragmentation patterns of degradation products formed under different stress conditions were studied and characterized through LC-MS fragmentation. Based on the results, degradation pathway for drug has been proposed. (C) 2009 Elsevier B.V. All rights reserved.

10aHPLC10aStability-indicating method10aStress studies10aTenatoprazole10aValidation1 aMahadik, Mahadeo, V.1 aBhusari, Vidhya, K.1 aKulkarni, Mahesh, J.1 aDhaneshwar, Sunil, R. uhttps://library.ncl.res.in/content/lc-uv-and-lc-ms-evaluation-stress-degradation-behaviour-tenatoprazole-0