共查询到20条相似文献,搜索用时 15 毫秒
1.
《Analytical letters》2012,45(12):1855-1867
Abstract A simple stability-indicating high-performance liquid-chromatographic (HPLC) method for the assay of erlotinib in the presence of its degradation products was developed on a C18 column using a mobile phase of 0.01 M ammonium formate–acetonitrile–containing formic acid with a flow rate of 1.0 mL min?1. The method was validated. Selectivity was validated by subjecting the stock solution of erlotinib to acidic, basic, photolysis, oxidative, and thermal degradation. The linearity range and values for limits of detection (LOD) and quantification (LOQ) were found to be 1–198, 0.33, and 1.1 µg mL?1, respectively. The analysis of the tablets containing erlotinib was quite precise (relative standard deviation <1%). 相似文献
2.
《液相色谱法及相关技术杂志》2012,35(4):533-546
A simple, sensitive, and reproducible ultra-performance liquid chromatography (UPLC) coupled with a photodiode array detector method was developed for the quantitative determination of Paliperidone palmitate in API and pharmaceutical injectable forms. The method is applicable to the quantification of related substances and assay of Paliperidone palmitate. Chromatographic separation was achieved on Acquity UPLC BEH (50 mm, 2.1 mm, and 1.7 µm) C-18 column, and the impurities are eluted with a gradient program of runtime about 10.0 min. The eluted compounds were monitored at 238 nm, the flow rate was 0.5 mL/min, and the column oven temperature was maintained at 35°C. The resolution of Paliperidone palmitate and eight (potential, bi-products and degradation) impurities was greater than 2.0 for all pairs of components. The high correlation coefficient (r2 > 0.999) values indicated clear correlations between the investigated compound concentrations and their peak areas within the test ranges. The repeatability and intermediate precision, expressed by RSD, were less than 10.0%. The accuracy and validity of the method were further ascertained by performing recovery studies via a spike method. The accuracy of the method expressed as relative error was satisfactory. The drug was subjected to the International Conference on Harmonization (ICH) prescribed hydrolytic, oxidative, photolytic, and thermal stress conditions. The performance of the method was validated according to the present ICH guidelines for specificity, limit of detection, limit of quantification, linearity, accuracy, precision, ruggedness, 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.
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.
《液相色谱法及相关技术杂志》2012,35(15):1568-1577
A sensitive stability indicating reverse phase high performance liquid chromatographic method was developed for the simultaneous determination of formoterol fumarate and ciclesonide in dry powder inhaler. The chromatographic separation was achieved on Hypersil BDS C8 250 × 4.6 mm, 5 um column using a mobile phase consisting of 0.1% orthophospheric acid and acetonitrile in the ratio of 35:65 (v/v), at a flow rate of 2.0 mL min−1. The column compartment temperature was set at 40°C. The typical HPLC chromatograms were extracted at 214 nm using photodiode array detector (PDA). The described method shows excellent linearity over a range of 3.6 µg mL−1 to 1.1 ng mL−1 for formoterol fumarate and 120 µg mL−1 to 34 ng mL−1 for ciclesonide. The correlation coefficient for formoterol fumarate and ciclesonide was 0.9998. The limit of detection and limit of quantification for formoterol fumarate was 0.33 ng mL−1, 1.1 ng mL−1 and for ciclesonide 10.2 ng mL−1, 34 ng mL−1, respectively. The proposed method was found to be very sensitive and accurate for the determination of Formoterol Fumarate and ciclesonide indry powder inhaler. 相似文献
6.
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
7.
《液相色谱法及相关技术杂志》2012,35(10):1088-1093
The proposed stability indicating method for the determination of tramadol hydrochloride by high-performance thin-layer chromatography in the pharmaceutical formulations was found to be specific, precise, and validated. The stationary phase employed was a precoated silica gel 60 F254 aluminum TLC plate. Several mobile phase combinations of varying polarity of solvent were tried for the method development, as well as for the resolution of degradation products from the parent densitogram of drug. Finally, the mobile phase containing a mixture of ethyl acetate:methanol:ammonia (9:0.8:0.5 v/v/v) was found to be satisfactory for the resolution of degradation products from the parent drug. Densitometric analysis of tramadol hydrochloride was carried out in the reflectance–absorbance mode at 271 nm. The Rf value of the drug was obtained at 0.64 ± 0.02 with sharp symmetrical peak. The degraded products formed under acidic, oxidative, and an alkali conditions were strongly retained. Linear relationships between concentration of analyte and corresponding peak area were observed over the range of 1000–6000 ng at the selected wavelength with an R2 value of 0.999 ± 0.0007. The validation for specificity, precision, robustness, and recovery of the method was also performed. The present method effectively separated the tramadol hydrochloride from its degradation products. 相似文献
8.
Primary objective of this study was to develop a stability-indicating reverse-phase high-performance liquid chromatography (HPLC) method for simultaneous quantitation of tramadol and aceclofenac in presence of their degradation products. The drugs were subjected to various International Conference on Harmonization recommended stress conditions, such as acid hydrolysis, alkaline hydrolysis, peroxide oxidation, thermolysis, and photolysis. The major degradation products got well resoluted from the analytes in HPLC analysis with a mobile phase composed of a mixture of 0.01?M ammonium acetate buffer (pH 6.5) and acetonitrile (65:35, v/v) through a Phenomenex Gemini C18 (250?mm?×?4.6?mm, 5?µm particle size) column. The method was linear over a range of 15–60?µg/mL for tramadol and 40–160?µg/mL for aceclofenac concentration. The analytes were detected at a wavelength of 270?nm. The method was validated and found to be specific, accurate, precise, stable, and robust for its intended use. The method can be recommended for its future use in routine quality control, accelerated and real-time stability analysis of the formulations containing tramadol and aceclofenac combination. 相似文献
9.
A sensitive, selective, precise and stability-indicating high-performance thin-layer chromatographic method of analysis of lamivudine both as a bulk drug and in formulations was developed and validated. The solvent system consisted of carbon tetrachloride – methanol – chloroform - acetonitrile (7.0: 3.0: 2.0: 1.5, v/v/v/v). Densitometric analysis of lamivudine was carried out in the absorbance mode at 275 nm. This system was found to give compact spots for lamivudine (RF value of 0.36 ± 0.02) following double development of chromatoplates with the same mobile phase. Lamivudine was subjected to acid and alkali hydrolysis, oxidation, dry heat and wet heat treatment and photo degradation. The drug undergoes degradation under acidic, basic conditions, oxidation, wet heat and photo degradation. Also the degraded products were well resolved from the pure drug with significantly different RF values. Linearity was found to be in the range of 50 – 1000 ng spot–1 with significantly high value of correlation coefficient. The linear regression analysis data for the calibration plots showed good linear relationship with r2 = 0.9994 ± 0.05 in the working concentration range of 300 ng spot–1 to 1000 ng spot–1. The mean value of slope and intercept were 0.11 ± 0.08 and 10.47 ± 1.21, respectively. The method was validated for precision, robustness and recovery. The limit of detection and quantitation were 15 ng spot–1 and 40 ng spot–1 respectively. As the method could effectively separate the drug from its degradation products, it can be employed as a stability indicating one. Moreover, the proposed HPTLC method was utilized to investigate the kinetics of acid degradation process. Arrhenius plot was constructed and activation energy was calculated. 相似文献
10.
Kasturi Rajashekhar;Challa Gangu Naidu;Chebolu Naga Sesha Sai Pavan Kumar;Bondigalla Ramachandra;Raju Padiya; 《SEPARATION SCIENCE PLUS》2024,7(3):2300181
A simple quality by design aided stability indicating method was developed for quantification of sonidegib (SONI) and its process related impurities using on ultra-performance liquid chromatography in bulk drug substance. AutoChrom and Design-Expert software were used to predict physicochemical properties, draw Ionization graphs, and generate analytical target profile. SONI was subjected to forced degradation conditions, such as oxidative, acid hydrolysis, base hydrolysis, hydrolytic, thermal, and photolytic hydrolysis. All degradation products and process contaminants were separated using an Acquity Ethylene Bridged Hybrid C18 column in gradient elution mode with a mobile phase containing 0.02 M ammonium acetate buffer and acetonitrile: methanol (80:20 v/v). The predicted physicochemical properties are accurate and they facilitated for selection of robust conditions in development of chromatographic method with minimal trials. The developed method can be used for quantification of drug and its process related impurities in bulk drugs. 相似文献
11.
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
12.
A simple isocratic liquid chromatographic method was developed for determination of lopinavir from its related impurities and assay for the first time. This method involves the use of a C(8) (Symmetry Shield RP8, 150 x 4.6 mm, 5 microm) column. The method was validated over the range of limit of quantitation (LOQ) to 120% of impurity specification limit and LOQ to 150% of working concentration for assay. The mobile phase consisted of a mixture of 50 mM of potassium phosphate buffer, acetonitrile and methanol in the ratio of 40:50:10. The flow rate was set at 1.0 mL/min with UV detection monitored at 210 nm. The drug was subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation. The developed method was validated for linearity, range, precision, accuracy and specificity. This method was successfully applied for content determination of lopinavir in pharmaceutical formulations. The method can be conveniently used in a quality control laboratory for routine analysis for assay and related substances as well for the evaluation of stability samples of bulk drugs and pharmaceutical formulations. 相似文献
13.
《液相色谱法及相关技术杂志》2012,35(5):629-639
The present research work was carried out to determine the stability of erlotinib hydrochloride (ERLO) drug under different stress conditions recommended by International Conference on Harmonization (ICH) guideline Q1A (R2). The stability of the drug was studied under hydrolytic, oxidative, photolytic, and thermal stress conditions. The drug was found susceptible to degradation under acidic, basic, and photolytic stress conditions, while it was stable under neutral, oxidative, and thermal stress conditions. A total of three degradation products (DPs) were formed. Separation was carried out by using high-performance liquid chromatography system (HPLC). Better separation was achieved on Kromasil®(150 mm × 4.6 mm, 5 µm) C18 column using gradient elution program. A mixture of stressed samples was subjected to LC-MS/TOF studies to obtain mass spectral data. The information obtained from accurate mass study was first utilized to build a complete mass fragmentation pathway of the drug, and later it was used for its degradants. Structures were proposed for each fragment based on the best possible molecular formula. Three novel DPs 6-(2-hydroxyethoxy)-7-(2-methoxyethoxy)quinazolin-4-amine, 6,7-bis(2-methoxyethoxy)quinazolin-4-amine, and N-(3-ethynylphenyl)-6, 7-bis (2-methoxyethoxy)-2-oxy-quinazolin-4-amine were identified. 相似文献
14.
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
15.
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
16.
稳定回归法用于复方氯丙嗪片的测定 总被引:1,自引:1,他引:1
本文应用稳定回归法用于紫外重叠光谱的分析。以复方氯丙嗪为例,不经分离,测定了盐酸氯丙嗪和盐酸异丙嗪的含量。与最小二乘回归法比较,提高了测定结果的准确度和精密度。结果满意。 相似文献
17.
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
18.
《Analytical letters》2012,45(11):1539-1551
Abstract The surfactant-to-dye binding degree method was used to determine morphine hydrochloride and codeine phosphate. Neutral red and bis(2-ethylhexyl) sulfosuccinate (AOT) were used as the dye and surfactant, respectively, to form dye–surfactant aggregates. Addition of the drug resulted in a decrease in the dye–surfactant binding degree, proportional to the drug concentration. This was measured by monitoring the absorbance changes of the dye at 532 nm. Under the optimum conditions, the calibration graphs were linear up to 32 and 28 µg mL?1 for morphine hydrochloride and codeine phosphate, respectively, with the corresponding detection limits of 0.40 and 0.35 µg mL?1. 相似文献
19.
纳米金探针瑞利共振散射法测定针剂中盐酸普鲁卡因 总被引:4,自引:0,他引:4
采用葡萄糖还原氯金酸的方法制得粒径约15nm的纳米金,在pH3.54酸性介质中它可以与盐酸普鲁卡因作用形成体积更大的纳米金聚集体。这种聚集体的形成可以使纳米金的瑞利共振散射强度急剧增强,其最大散射峰位于354nm左右。在适当的条件下,相对散射强度(ΔI)与盐酸普鲁卡因的浓度成正比。采用标准加入法,对针剂中的普鲁卡因进行测定,得到满意结果。线性范围0~40μg/L(r=0.9996);对含盐酸普鲁卡因30μg/L的溶液平行测定的相对标准偏差为2.51%(n=11);检出限(3σ)为16ng/L;测定限(10σ)为54ng/L。 相似文献
20.
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