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1.
G. Saravanan M. Ravikumar M. J. Jadhav M. V. Suryanarayana N. Someswararao P. V. R. Acharyulu 《Chromatographia》2007,66(3-4):291-294
This study deals with a stability indicating HPLC reverse phase method for quantitative determination of temozolomide. A chromatographic
separation was achieved on an Inertsil ODS 3V, 250 × 4.6 mm ID, 5 μm column using mobile phase A (buffer 5 mL glacial acetic
acid in 1,000 mL of Milli Q water ) and mobile phase B (methanol). Forced degradation studies were performed on bulk sample
of temozolomide using acid (0.5 N hydrochloric acid), base (0.5 N sodium hydroxide), oxidation (10% v/v hydrogen peroxide), heat (60 °C) and UV light (254 nm). Degradation of the drug substance was observed in base hydrolysis
and oxidation. Degradation product formed under these conditions was found to be Imp-A. When the stress samples were assayed,
the mass balance was close to 99.5%. The sample solution was stable up to 48 h at 5 °C and mobile phase was found to be stable
up to 48 h at 25 °C. The developed method was validated with respect to linearity, accuracy, precision, robustness and forced
degradation studies prove the stability indicating power of the method. 相似文献
2.
G. Saravanan M. V. Suryanarayana M. J. Jadhav M. Ravikumar N. Someswararao P. V. R. Acharyulu 《Chromatographia》2007,66(5-6):431-434
This present work describes the development of a stability-indicating high performance liquid chromatographic method for the
quantitative determination of pemetrexed disodium. Pemetrexed disodium is an antifolate antineoplastic agent that exerts its
action by disrupting folate-dependent metabolic processes essential for cell replication. The chromatographic separation was
achieved on an ACE 3 C18 HPLC column using a mobile phase consisting of a mixture of buffer (solvent A) and organic modifier
acetonitrile (solvent B). Forced degradation studies were performed on bulk sample of pemetrexed disodium using acid (0.5 N
hydrochloric acid), base (0.5 N sodium hydroxide), oxidation (10% v/v hydrogen peroxide), heat (60 °C) and UV light (254 nm). Degradation of the drug substance was observed in base hydrolysis.
Degradation product formed under acid and base hydrolysis was found to be starting material. The stressed samples were assayed
using the developed LC method and the mass balance found was close to 99.5%, thus proving its stability-indicating power.
The developed method was validated with respect to linearity, accuracy, precision and robustness. 相似文献
3.
G. Saravanan M. V. Suryanarayana N. Balaji N. Someswararao N. M. Sekhar 《Chromatographia》2008,67(1-2):179-182
This paper describes the development of a stability-indicating high-performance liquid chromatographic (HPLC) method for quantitative
determination of topotecan hydrochloride, a semi-synthetic derivative of camptothecin and anti-tumor drug with topoisomerase
I-inhibitory activity. Chromatographic separation was achieved on a C18 column with a mixture of phosphate buffer and acetonitrile as mobile phase. The method was validated for linearity, accuracy,
precision, and robustness. Forced degradation studies were performed by treating bulk samples of topotecan hydrochloride with
acid (0.5 M hydrochloric acid), base (0.5 M sodium hydroxide), oxidizing agent (10% v/v hydrogen peroxide), heat (60 °C), and UV light (254 nm). 相似文献
4.
G. Saravanan G. Jyothi Y. Suresh A. Annerao M. Ramakrishna M. Yogeshwar Reddy B. Ravibabu 《Chromatographia》2008,67(1-2):173-177
Levetiracetam is used in combination with other medications to treat certain types of seizures in people with epilepsy. Levetiracetam
is in a class of medications called anticonvulsants and it works by decreasing abnormal excitement in the brain. A chromatographic
separation was achieved on a YMC pack ODS AQ, 250 mm × 4.6 mm, 5 μm column using diluted phosphoric acid and acetonitrile
in the ratio 85:15 v/v. Forced degradation studies were performed on the levetiracetam drug substance. The drug substance was degraded to Imp-B
during acid and base hydrolysis. When the stress samples were assayed, the mass balance was matching. The sample solution
and mobile phase was found to be stable up to 48 h at 25 °C. The developed method was validated with respect to linearity,
accuracy, precision and robustness. 相似文献
5.
G. Saravanan B. M. Rao M. Ravikumar M. V. Suryanarayana N. Someswararao P. V. R. Acharyulu 《Chromatographia》2007,66(3-4):219-222
A stability-indicating HPLC method for the quantitative determination of Bicalutamide is described. Bicalutamide is a nonsteroidal
antiandrogen and is an oral medication that is used for treating prostate cancer. Separation was achieved on a Waters Symmetry
shield RP18 HPLC column using a mobile phase consists of a mixture of phosphate buffer (Solvent A) and organic modifier acetonitrile
(Solvent B). Degradation studies were performed on bulk samples of bicalutamide using acid (0.5 N methanolic hydrochloric
acid), base (0.5 N methanolic sodium hydroxide), oxidation (10% v/v methanolic hydrogen peroxide), heat (60 °C) and UV light
(254 nm). Degradation was observed under base hydrolysis to give the starting material used during the synthesis of bicalutamide.
The degraded samples were assayed and gave a mass balance greater than 99.5%, thus proving the stability-indicating power
of the developed method. The method was validated with respect to linearity, accuracy, precision and robustness. 相似文献
6.
A simple, isocratic, rapid and accurate reversed phase high performance liquid chromatography method was developed for the
quantitative determination of tazarotene. The developed method is also applicable for the related substance determination
in bulk drugs. The chromatographic separation was achieved on a Hypersil C18 (250 mm × 4.6 mm 5 μm) column using water pH
2.5 with orthophosphoric acid:acetonitrile (15:85, v/v) as a mobile phase. The chromatographic resolutions between tazarotene and its potential impurity A and B were found greater
than three. The limit of detection and limit of quantification of impurities were found to be 25 and 75 ng mL−1. The percentage recovery of impurities in bulk drug sample was ranged from 96.8 to 103.5.The percentage recovery of tazarotene
in bulk drug sample was ranged from 98.4 to 100.9. The developed RPLC method was validated with respect to linearity, accuracy,
precision and robustness. 相似文献
7.
G. Saravanan B. M. Rao M. Ravikumar M. V. Suryanarayana N. Someswararao P. V. R. Acharyulu 《Chromatographia》2007,66(3-4):287-290
Chromatographic separation of lenalidomide and its impurities was achieved on an Inertsil ODS-3 V column using a mobile phase
consisting of a mixture of buffer, acetonitrile and methanol in the ratio 80:8:12 v/v. Degradation studies were performed on bulk samples of lenalidomide subjected to 0.5 N hydrochloric acid, 0.5 N sodium hydroxide,
10% v/v hydrogen peroxide, heating to 60 °C and UV light at 254 nm. Degradation was observed only under base hydrolysis conditions.
The developed LC method gave a mass balance close to 99.5%, proving it to be suitable for stability studies and was validated
with respect to linearity, accuracy, precision and robustness. 相似文献
8.
The present paper describes stability indicating reverse phase high-performance liquid chromatography (RP-HPLC) assay method
for nitazoxanide in bulk drugs. The developed method is also applicable for the related substances determination in bulk drug.
The drug substance was subjected to stress conditions of hydrolysis, photolysis and thermal degradation. The considerable
degradation of nitazoxanide was observed under base and peroxide hydrolysis. The drug was found to be stable in other stress
conditions attempted. The chromatographic separation of the drug was achieved on reversed-phase C-18 column. Eluents were
monitored on photo-diode array detector at a wavelength of 240 nm. The mobile phase was aqueous 0.005 M tetra butyl ammonium
hydrogen sulphate and acetonitrile (45:55, v/v). In the developed HPLC method, resolution between nitazoxanide and its potential impurities, namely Imp-A (5-nitro-1,3-thiazol-2-amine),
Imp-B (N-(5-nitro-1,3-thiazol-2-yl) acetamide) and Imp-C (2-{[(5-nitro-1,3-thiazol-2-yl) amino] carbonyl} phenyl 2-(acetyloxy) benzoate)
was found greater than three. The developed RP-HPLC method was validated with respect to response function, accuracy, precision,
specificity, stability of analytical solutions and robustness. Also to determine related substances and assay determination
of nitazoxanide that can be used to evaluate the quality of regular production samples. The developed method can also be conveniently
used for the assay determination of nitazoxanide in pharmaceutical formulations. 相似文献
9.
D. V. Subba Rao P. Radhakrishnanand M. V. Suryanarayana V. Himabindu 《Chromatographia》2007,66(7-8):499-507
An isocratic reversed-phase liquid chromatographic method has been developed for quantitative determination of candesartan
cilexetil, used to treat hypertension, in the bulk drug and in pharmaceutical dosage forms. The method is also applicable
to analysis of related substances. Chromatographic separation was achieved on a 250 mm × 4.6 mm, 5 μm particle, CN column
with a 50:50 (v/v) mixture of phosphate buffer, pH 3.0, and acetonitrile as mobile phase. The flow rate was 1.0 mL min−1 and the detection wavelength was 210 nm. Resolution of candesartan cilexetil and six potential impurities was greater than
2.0 for all pairs of compounds. The drug was subjected to hydrolytic, oxidative, photolytic, and thermal stress and substantial
degradation occurred in alkaline and acidic media and under oxidative and hydrolytic stress conditions. The major product
obtained as a result of basic hydrolysis was different from that produced by acid hydrolysis and aqueous hydrolysis. The stress
samples were assayed against a reference standard and the mass balance was found to be close to 99.6%. The method was validated
for linearity, accuracy, precision, and robustness. 相似文献
10.
Development of a New Analytical Method for Determination of Related Components in Nateglinide 总被引:1,自引:0,他引:1
An isocratic reverse phase liquid chromatographic (RP-LC) assay method has been developed for the quantitative determination
of nateglinide and its related components namely imp-1 and imp-2 in bulk drug and in pharmaceutical dosage form, used for
the treatment of type II diabetes mellitus. The developed method is stability indicating and also can be used for stability
testing. The chromatographic separation was achieved on C-8, 150 × 4.6 mm, 3.5 μm stationary phase. The LC method employs
solution A as mobile phase. Solution A contains a mixture of phosphate buffer pH 3.0: acetonitrile (50:50 v/v). The flow rate was 1.0 mL min−1 and the detection wavelength was 210 nm. In the developed LC method the resolution between nateglinide and its potential impurities
namely imp-1 and imp-2 was found to be greater than 5.0. The drug was subjected to stress conditions of hydrolysis, oxidation,
photolysis and thermal degradation. Considerable degradation was found to occur in acid medium, alkaline medium and oxidative
stress conditions. The stress samples were assayed against a qualified reference standard and the mass balance was found close
to 99.2%. The developed RP-LC method was validated with respect to linearity, accuracy, precision and robustness. 相似文献
11.
A. Singh B. M. Rao G. R. Deshpande S. Sangaraju M. K. Srinivasu M. Lalitha Devi P. V. V. Satyanarayana K. B. Chandrasekhar 《Chromatographia》2007,65(3-4):191-196
A simple and rapid reversed-phase liquid chromatographic method was developed for the related substances determination and
quantitative evaluation of ziprasidone hydrochloride, which is used as an antipsychotic agent. Forced degradation studies
were performed on bulk sample of ziprasidone hydrochloride using acid, base, oxidative hydrolysis, thermal stress and photolytic
degradation. Mild degradation of the drug substance was observed during thermal stress and considerable degradation observed
during base hydrolysis. The chromatographic method was fine tuned using the samples generated from forced degradation studies.
Good resolution between the peaks corresponds to synthetic impurities and degradation products from the analyte were achieved
on YMC Pack Pro C18 column using the mobile phase consists of a mixture of 0.05% v/v of phosphoric acid in water and acetonitrile. The stressed test solutions were assayed against the qualified working standard
of ziprasidone hydrochloride and the mass balance in each case was close to 99.7% indicating that the developed method was
stability-indicating. Validation of the developed method was carried out as per ICH requirements. 相似文献
12.
Marcelo Donadel Malesuik Simone Gonçalves Cardoso Martin Steppe 《Chromatographia》2008,67(1-2):131-136
A reversed-phase liquid chromatographic (LC) method was developed for the assay of nitazoxanide (NTZ) in solid dosage formulations.
An isocratic LC separation was performed on a Phenomenex Synergi Fusion C18 column (250 mm × 4.6 mm, i.d., 4 μm particle size) using a mobile phase of 0.1% o-phosphoric acid solution, pH 6.0: acetonitrile (45:55, v/v) at a flow rate of 1.0 mL min−1. Detection was achieved with a photodiode array detector at 240 nm. The detector response for NTZ was linear over the concentration
range from 2 to 100 μg mL−1 (r = 0.9999). The specificity and stability-indicating capability of the method were proved using stress conditions. The RSD
values for intra-day precision were less than 1.0% for tablets and powder for oral suspension. The RSD values for inter-day
precision were 0.6 and 0.7% for tablets and powder for oral suspension. The accuracy was 100.4% (RSD = 1.8%) for tablets and
100.9% (RSD = 0.3%) for powder for oral suspension. The limits of quantitation and detection were 0.4 and 0.1 μg mL−1. There was no interference of the excipients on the determination of the active pharmaceutical ingredient. The proposed method
was precise, accurate, specific, and sensitive. It can be applied to the quantitative determination of drug in tablets and
powder for oral suspension. 相似文献
13.
A simple liquid chromatographic method was developed for the separation and quantification of voriconazole and its enantiomer
in drug substance. The separation was achieved on Chiral cel-OD (250 mm × 4.6 mm × 10 μm) using mobile phase consisting of
n-hexane and ethanol in the ratio 9:1 (v/v) with a flow rate of 1.0 mL min−1, at 27 °C column temperature and detection at 254 nm with an injection volume of 20 μL. Ethanol was used as diluent. The
method is capable of detecting the (2S, 3R) enantiomer down to 0.0075% and can quantify down to 0.021% with respect to sample concentration. The method is rapid and
the resolution achieved was about 3.0. This method can be employed for the quantification of (2S, 3R) enantiomer in voriconazole drug substance. 相似文献
14.
K. Ramulu B. M. Rao P. Madhavan M. Lalitha Devi M. K. Srinivasu K. B. Chandrasekhar 《Chromatographia》2007,65(3-4):249-252
A simple and new isocratic normal phase chiral HPLC method has been developed for the determination of enantiomeric purity
of pemetrexed disodium (l-enantiomer) in bulk drugs with a short run time of about 20 min. Chromatographic separation of l and d-enantiomers of pemetrexed disodium was achieved on an amylose based chiral stationary phase using a mobile phase consists
of hexane, ethanol and trifluoro acetic acid. The resolution between the enantiomers was found to be more than 2.0. The system
precision and method precision were found to be within 5% RSD for the distomer (d-enantiomer) at its specification level (i.e. not more than 1.0% w/w). The limit of detection and limit of quantification of distomer were 1.6 and 5 μg mL−1, respectively for 10 μL injection volume. The percentage recovery of distomer was ranged from 90.6 to 105.7 in bulk drug
samples. The test solution was found to be stable in the diluent for 48 h. The method was found to be specific for the enantiomers
of pemetrexed disodium and can be conveniently used for the quantification of undesired d-enantiomer present in the bulk drug samples of pemetrexed disodium. 相似文献
15.
A stability-indicating HPLC assay method was developed for the quantitative determination of tadalafil in bulk samples and
in pharmaceutical dosage forms in the presence of the degradation products. It involved a 250 mm × 4.6 mm, 5 μm C-18 column.
The gradient LC method employs solution A and B as mobile phase. Solution A contains a mixture of buffer (phosphate buffer
and tetra-n-butyl ammonium hydrogen sulfate) pH 2.5: acetonitrile (80:20, v/v) and solution B contains a mixture of water: acetonitrile (20:80, v/v). The flow rate was 1.0 mL min−1 and the detection wavelength was 220 nm. The retention time of tadalafil is about 17 min. Tadalafil was subjected to different
ICH prescribed stress conditions. Degradation was found to occur in hydrolytic and to some extent in oxidative stress conditions,
while the drug was stable to photolytic and thermal stress. The drug was particularly labile under alkaline hydrolytic conditions.
The drug was subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation. The assay of stress
samples was calculated against a qualified reference standard and the mass balance was close to 99.5%. The developed RP-LC
method was validated with respect to linearity, accuracy, precision and ruggedness. 相似文献
16.
Stability-Indicating LC Determination of Nitazoxanide in Bulk Drug and in Pharmaceutical Dosage Form
Vipul P. Rane Jaiprakash N. Sangshetti Kiran R. Patil Ravindra D. Yeole Devanand B. Shinde 《Chromatographia》2008,67(5-6):455-459
A novel stability-indicating high-performance liquid chromatographic assay method was developed and validated for quantitative
determination of nitazoxanide in bulk drugs and in pharmaceutical dosage form in the presence of degradation products generated
from forced decomposition studies. An isocratic, reversed phase LC method was developed to separate the drug from the degradation
products, using an Ace5- C18 (250 mm × 4.6 mm, 5 μm) column, and 50 mM ammonium acetate (pH 5.5 by acetic acid) and acetonitrile
(55:45 v/v) as a mobile phase. The detection was carried out at a wavelength of 240 nm. The nitazoxanide was subjected to stress conditions
of hydrolysis (acid, base), oxidation, photolysis and thermal degradation. Degradation was observed for nitazoxanide in base,
acid and in 30% H2O2 conditions. The drug was found to be stable in the other stress conditions attempted. The degradation products were well
resolved from the main peak. The percentage recovery of nitazoxanide was from (100.55 to 101.25%) in the pharmaceutical dosage
form. The developed method was validated with respect to linearity, accuracy (recovery), precision, system suitability, specificity
and robustness. The forced degradation studies prove the stability indicating power of the method. 相似文献
17.
U. Seshachalam D. V. L. Narasimha Rao B. Haribabu K. B. Chandrasekhar 《Chromatographia》2007,65(5-6):355-358
A forced degradation study was successfully applied for the development of a stability-indicating assay method for the determination
of atazanavir in presence of its degradation products. The method was developed and optimized by analyzing the forcefully
degraded samples. Degradation of the drug was done under acidic, alkaline, oxidative, photolytic and thermal stress conditions.
The proposed method was able to resolve all of the possible degradation products formed during the stress studies. The major
impurities are generated in acidic and alkaline conditions. The product was found stable under thermal, photolytic and oxidative
conditions. The developed method was validated for determination of atazanavir, and the method was found to be equality applicable
to study the impurities formed during routine and forced degradation of atazanavir. 相似文献
18.
Two sensitive and reproducible methods are described for the quantitative determination of dasatinib in the presence of its
degradation products. The first method was based on high performance thin layer chromatography (HPTLC) followed by densitometric
measurements of their spots at 280 nm. The separation was on HPTLC aluminium sheets of silica gel 60 F254 using toluene:chloroform (7.0:3.0, v/v). This system was found to give compact spots for dasatinib after development (R
F
value of 0.23 ± 0.02). The second method was based on high performance liquid chromatography (HPLC) of the drug from its
degradation products on reversed phase, PerfectSil column [C18 (5 μm, 25 cm × 4.6 mm, i.d.)] at ambient temperature using mobile phase consisting of methanol:20 mM ammonium acetate with
acetic acid (45:55, v/v) pH 3.0 and retention time (t
R
= 8.23 ± 0.02 min). Both separation methods were validated as per the ICH guidelines. No chromatographic interference from
the tablet excipients was found. Dasatinib was subjected to acid–alkali hydrolysis, oxidation, dry heat, wet heat and photo-degradation.
The drug was susceptible to acid–alkali hydrolysis and oxidation. The drug was found to be stable in neutral, wet heat, dry
heat and photo-degradation conditions. As the proposed analytical methods could effectively separate the drug from its degradation
products, they can be employed as stability indicating. 相似文献
19.
Monika Piazzon Tagliari Hellen Karine Stulzer Fabio Seigi Murakami Gislaine Kuminek Bruno Valente Paulo Renato Oliveira Marcos Antonio Segatto Silva 《Chromatographia》2008,67(7-8):647-652
A stability-indicating reversed-phase high-performance liquid chromatography (LC) method was developed and validated for the
determination of hydrochlorothiazide in an oral suspension. Isocratic chromatography was performed on a C18 column with 0.1 M sodium phosphate buffer pH 3.0/acetonitrile (70:30 v/v) as mobile phase, at a flow rate of 1.3 mL min−1, and UV detection at 254 nm. The method was linear (r
2 = 0.9998), accurate (mean recovery = 100.3%), and precise (RSD <2%). It was also validated for specificity and robustness.
The method was successfully applied for the quality control analysis of a new pharmaceutical formulation of HCTZ for pediatric
use. 相似文献
20.
Vadde Ravinder S. Ashok A. V. S. S. Prasad G. Balaswamy Y. Ravindra Kumar B. Vijaya Bhaskar 《Chromatographia》2008,67(3-4):331-334
A rapid isocratic chiral HPLC method has been developed for the separation of R-galantamine from S-galantamine. Good resolution viz. Rs > 3 between R- and S- forms of galantamine was achieved with chiralpak AD-H (250 × 4.6 mm) column using n-hexane, 20% propionic acid in isopropanol and diethyl amine in the ratio of 80:20:0.2 (v/v) as mobile phase at ambient temperature. Flow rate was kept as 0.8 mL min−1 and the elution was monitored at 289 nm. This method was further used to determine the amount of R-galantamine in pure and pharmaceutical formulations of S-galantamine. This method is capable to detect and quantitate R-galantamine to the levels of 0.21 and 0.84 μg mL−1, respectively. The method was validated as per International Conference on Harmonization (ICH) guidelines in terms of limit
of detection (LOD), limit of quantification (LOQ), linearity, precision, accuracy, specificity, robustness and ruggedness. 相似文献