共查询到20条相似文献,搜索用时 15 毫秒
1.
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
2.
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
3.
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
4.
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
5.
A stability-indicating reversed-phase liquid chromatographic (RPLC) method has been established for analysis of ramipril (RAM)
and moexipril hydrochloride (MOEX.HCl) in the presence of the degradation products generated in studies of forced decomposition.
The drug substances were subjected to stress by hydrolysis (0.1 m NaOH and 0.1 m HCl), oxidation (30% H2O2), photolysis (254 nm), and thermal treatment (80 °C). The drugs were degraded under basic and acidic conditions and by thermal
treatment but were stable under other stress conditions investigated. Successful separation of the drugs from the degradation
products was achieved on a cyanopropyl column with 40:60 (v/v) aqueous 0.01 m ammonium acetate buffer (pH 6)–methanol as mobile phase at a flow rate of 1 mL min−1. Detection was by UV absorption at 210 nm. Response was a linear function of concentration over the range 5–50 μg mL−1 (r > 0.9995), with limits of detection and quantitation (LOD and LOQ) of 0.04 and 0.09 μg mL−1, respectively, for RAM and 0.014 and 0.32 μg mL−1, respectively, for moexipril. The method was validated for specificity, selectivity, solution stability, accuracy, and precision.
Statistical analysis proved the method enabled reproducible and selective quantification of RAM and MOEX as the bulk drug
and in pharmaceutical preparations. Because the method effectively separates the drugs from their degradation products, it
can be used as stability-indicating. 相似文献
6.
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
7.
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
8.
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
9.
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
10.
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
11.
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
12.
A simple, precise, and accurate HPLC method has been developed and validated for assay of ezetimibe in tablets and for determination
of content uniformity. Reversed-phase liquid chromatographic separation was achieved by use of phosphoric acid (0.1%, v/v)–acetonitrile 50:50 (v/v) as mobile phase. The method was validated for specificity, linearity, precision, accuracy, robustness, and solution stability.
The specificity of the method was determined by assessing interference from the placebo and by stress testing of the drug
(forced degradation). Response was a linear function of drug concentration in the range 20–80 μg mL−1 (r = 0.9999). Intraday and interday system and method precision were determined. Accuracy was between 100.8 and 102.7%. The
method was found to be robust, and was suitable for assay of ezetimibe in a tablet formulation and for determination of content
uniformity.
An erratum to this article can be found at 相似文献
13.
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
14.
Kiran R. Patil Vipul P. Rane Jaiprakash N. Sangshetti Devanand B. Shinde 《Chromatographia》2008,67(7-8):575-582
A simple, rapid, and precise method is developed for the quantitative simultaneous estimation of telmisartan and ramipril
in combined pharmaceutical dosage form. A chromatographic separation of the two drugs was achieved with an ACE 5 C18, 25-cm analytical column using buffer–acetonitrile (55:45 v/v). The buffer used in mobile phase contains 0.1 M sodium perchlorate monohydrate in double distilled water pH adjusted 3.0
with trifluoroacetic acid. The instrumental settings are flow rate of 1.5 mL min−1, column temperature at 30 °C, and detector wavelength of 215 nm using a photodiode array detector. The resolution between
ramipril and telmisartan were found to be more than 5. Theoretical plates for ramipril and telmisartan were 13,022 and 6,629.
Tailing factor for ramipril and telmisartan was 0.94 and 0.98. Telmisartan, ramipril and their combination drug product were
exposed to thermal, photolytic, hydrolytic and oxidative stress conditions, and the stressed samples were analysed by the
proposed method. Peak homogeneity data of telmisartan and ramipril is obtained using photodiode array detector, in the stressed
sample chromatograms, demonstrated the specificity of the method for their estimation in presence of degradants. The described
method shows excellent linearity over a range of 20–400 μg mL−1 for telmisartan and 2.5–50 μg mL−1 for ramipril. The correlation coefficient for telmisartan and ramipril are 1. The relative standard deviation for six measurements
in two sets of each drug in tablets was always less than 2%. The proposed method was found to be suitable and accurate for
quantitative determination and the stability study of telmisartan and ramipril in pharmaceutical preparations. 相似文献
15.
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
16.
Reguri Buchireddy Khagga Mukkanti Polisetty Srinivasulu Koduri S. V. Srinivas 《Chromatographia》2008,67(3-4):275-280
We present a simple and reliable method for simultaneous determination of voriconazole and its main metabolite resulting from N-oxidation (UK-121,265), in human plasma. The work-up procedure used acetonitrile and potassium salts to precipitate plasma proteins. No internal standard was used. The chromatographic system used a LiChroCART® 250-4 cartridge packed with LiChrospher® 100 RP-8 (diameter particules, 5 μm). The UV monochromatic detector was set on 260 nm. The mobile phase consisted of a 60/40 (v/v) mixture of acetonitrile and water. The flow rate was 1 mL min?1. The retention times for voriconazole and its metabolite were 8.98 and 4.02 min respectively, and total run time was 12 min. The linearity of the method was investigated from 0.31 to 10.0 mg L?1; the lowest limit of quantification was 0.30 mg L?1. Precision ranged from 2.41% to 6.32% for voriconazole and 0.80% to 11.6% for the N-oxide voriconazole metabolite. Accuracy was between 93.0% and 101% for voriconazole and 90.0% and 101% for the N-oxide voriconazole metabolite. This rapid and accurate method could be interesting to investigate metabolite/voriconazole ratio with respect to CYP2C19 genetic status and CYP3A4 activity changes. 相似文献
17.
G. Saravanan M. V. Suryanarayana Manoj J. Jadhav M. Ravikumar N. Someswararao P. V. R. Acharyulu 《Chromatographia》2007,66(5-6):435-438
This present work narrates the stress stability behavior and development of a liquid chromatographic method for the quantitative
determination of anastrozole. Anastrozole is appropriately used when using substantial amounts of aromatizing steroids, or
when one is prone to gynecomastia and using moderate amounts of such steroids. A chromatographic separation was achieved on
a Hichrom RPB18 (250 × 4.6 mm, 5 μ) column using water and mixture of acetonitrile and methanol (1:1 ratio) as mobile phase.
Forced degradation studies were performed on bulk samples of anastrozole using acid, base, hydrogen peroxide, heat and UV
light. Degradation of the drug substance was observed in base hydrolysis. Degradation product formed under base hydrolysis
was found to be Imp-C. The sample solution and mobile phase were found to be stable up to 48 h. 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
18.
In the present study, a novel, fast and simple liquid chromatographic method was developed and validated for the simultaneous
determination of rosiglitazone and metformin in pharmaceutical preparations. The separation was achieved on a phenyl column
(250 × 4.6 mm i.d., 5 μm) using a mobile phase composed of acetonitrile:10.0 mM phosphate buffer pH 5.5 (70:30, v/v). The flow rate was 1 mL min−1. UV detection was performed at 245 nm and verapamil was used as internal standard. The developed method was validated in
terms of stability, specificity, sensitivity, linearity, accuracy, precision and robustness. The limit of quantification was
0.02 μg mL−1 for both drugs. The method developed was successfully applied to the simultaneous determination of rosiglitazone and metformin
in pharmaceutical preparations. The results were compared to two methods reported in the literature and no significant difference
was found statistically. 相似文献
19.
Rahul P. Dixit Chandrashekhar R. Barhate Mangal S. Nagarsenker 《Chromatographia》2008,67(1-2):101-107
Simvastatin and ezetimibe are used to treat hyperlipidemia. A simple, selective and stability-indicating HPTLC method has
been established for analysis of simvastatin and ezetimibe. The method has been validated so that both drugs can routinely
be analyzed simultaneously. The method uses aluminum-backed silica gel 60F254 TLC plates as stationary phase with n-hexane–acetone 6:4 (v/v) as mobile phase. Densitometric analysis of both drugs was carried out in absorbance mode at 234 nm. This system was found
to give compact bands for simvastatin and ezetimibe (R
F 0.39 ± 0.05 and 0.50 ± 0.05, respectively). Linear relationships were obtained between response and amount of drug in the
range 200–1,600 ng per band with high correlation coefficients (r
2 = 0.9917 ± 0.0018 for simvastatin and r
2 = 0.9927 ± 0.0021 for ezetimibe). The method was validated for precision, robustness, and recovery. The limits of detection
and quantitation were 25 and 150 ng per band, respectively. Simvastatin and ezetimibe were subjected degradation by acid,
pH 6.8 phosphate buffer, oxidation, dry heat, and wet heat. The degradation products were well resolved from the pure drug
with significantly different R
F values. Because the method could effectively separate the drug from its degradation products, it can be used for stability-indicating
analysis. 相似文献
20.
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