Optimization and validation of an RP-HPLC method for the estimation of 6-mercaptopurine in bulk and pharmaceutical formulations

Somasekhar, Vanita

doi:10.1590/s1984-82502014000400015

Cited by 8 publications

(6 citation statements)

References 9 publications

(9 reference statements)

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“…In the light of available individual methods for the determination of azathioprine, 6-mercaptopurine, 6-thioguanine and folic acid, different chromatographic parameters were tested to establish the most suitable chromatographic conditions for their simultaneous determination in FDCs [20,23,32]. Parameters such as composition of stationary and mobile phases as well as temperature of analysis were systematically studied so as to achieve good resolution of adjacent peaks, symmetric peaks, high column performance and acceptable runtime.…”

Section: Resultsmentioning

confidence: 99%

“…A type of chosen chromatographic column had a significant influence on separation of compounds. Due to considerable differences in polarity of analytes, a compromise between hydrophilic and lipophilic character of sorbents had to be found [20,23,32,33]. Therefore, three kinds of chromatographic columns were investigated: XBridge C18 (150 × 4.6 mm, particle size 5 µm) by Waters (Milford, MA, USA), XBridge Phenyl (150 × 4.6 mm, particle size 5 µm) by Waters (Milford, MA, USA) and Zorbax SB C8 (150 × 4.6 mm, particle size 5 µm) by Agilent Technologies (Santa Clara, CA, USA).…”

Section: Resultsmentioning

confidence: 99%

“…In the last decade, various techniques for determination of azathioprine have been used, including high performance thin-layer chromatography [13], spectrophotometry [14], atomic absorption spectrometry [15], flow injection chemiluminometry [16], electrochemistry [17,18,19] and high-performance liquid chromatography [20]. Several methods have been reported for determination of 6-mercaptopurine in pharmaceutical formulations using analytical techniques such as Raman spectroscopy [21], electrochemistry [22] and high-performance liquid chromatography [23]. In literature, several analytical methods to quantify 6-thioguanine using fluorescence spectroscopy [24], electrochemistry [25] and high performance liquid chromatography with post column iodine-azide reaction [26] can be found.…”

Section: Introductionmentioning

confidence: 99%

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Pharmacokinetic Profiling and Simultaneous Determination of Thiopurine Immunosuppressants and Folic Acid by Chromatographic Methods

et al. 2019

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With the increase in the number of medicines patients have to take, there has been a rapid rise of fixed-dose combinations (FDCs) in the last two decades. Prior to FDC development, pharmacokinetic properties of active pharmaceutical ingredients (APIs) have to be evaluated, as well as methods for their determination developed. So as to increase patient compliance in inflammatory bowel disease, three novel FDCs of thiopurine immunosuppressants and folic acid are proposed; physico-chemical and pharmacokinetic properties such as hydrophobicity, lipophilicity and plasma protein binding of all APIs are evaluated. Moreover, experimental results of different properties are compared to those computed by various on-line prediction platforms so as to evaluate the viability of the in silico approach. A simultaneous method for their determination is developed, optimized, validated and applied to commercial tablet formulations. The method has shown to be fast, selective, accurate and precise, showing potential for reliable determination of API content in proposed FDCs during its development.

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Pharmacokinetic Profiling and Simultaneous Determination of Thiopurine Immunosuppressants and Folic Acid by Chromatographic Methods

et al. 2019

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“…Several stationary and mobile phases were used for the analysis of FA and purine analogues. Most of the chromatographic methods include the use of, almost exclusively, reversed-phase chromatographic columns C18 and C8, detectors such as UV-Vis or, if necessary, MS and mobile phases containing mixtures of polar organic solvent and acidified water (28)(29)(30). Therefore, the analysis of our samples was performed using a Zorbax SB-C8 column that can be used at low pH without degradation.…”

Section: Methods Developmentmentioning

confidence: 99%

Miniaturized shake-flask HPLC method for determination of distribution coefficient of drugs used in inflammatory bowel diseases

et al. 2019

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A new method for determination of distribution coefficient of drugs azathioprine, 6-mercaptopurine and 6-thioguanine and nutrient folic acid used in the treatment of inflammatory bowel disease based on a miniaturized shake-flask and HPLC/DAD was developed. Special attention was made to the most commonly reported problems in the measurement of distribution coefficients using a shake-flask method such as mixing technique, speed and time, the temperature of experiment, type of buffer and its pH as well as n-octanol/buffer phase ratio. The concentration of compounds in the buffer is determined by HPLC directly from shake flasks or conventional 2-mL vials. The developed method was fully validated according to ICH guidelines. Furthermore, experimental data were successfully compared with lipophilicity and human intestinal absorption calculated by the use of four different theoretical approaches. The method shows potential for high-throughput measurements of a large number of compounds.

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“…The results obtained from the system suitability injection were quite satisfactory. Hence it can be confirmed that method is robust [11,12].…”

Section: Robustness Of the Methodmentioning

confidence: 99%

Development and Validation of a Liquid Chromatographic Method for the Quantification of Related Compounds in Cyclophosphamide

Sofiqul¹,

Murugan²,

Premakumari³

et al. 2018

Pharm Anal Acta

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A simple reverse-phase high performance liquid chromatographic method (RP-HPLC) was developed for quantification of the related compounds in Cyclophosphamide. The chromatographic separation was achieved with C18 column (250 × 4.6 mm, 5 µm particle size) with gradient elution composed of 0.02 M Potassium dihydrogen phosphate (pH-7.0) as mobile phase-A and 60:40% v/v Acetonitrile / Water as mobile phase-B at a flow rate of 0.8 mL /min and column compartment maintained at 40°C for separation. Detection was carried out at 195 nm. The correlation coefficient (≥0.99) shows the linearity response against concentration over the range of Limit of Quantification (LOQ). Precision studies showed the Relative Standard Deviation (RSD) values less than 5% for Cyclophosphamide and its related compounds. The method was substantiated with respect to specificity, precision, linearity, accuracy, limit of quantification, and robustness. The proposed method could be used for routine analysis of Cyclophosphamide formulations.

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Optimization and validation of an RP-HPLC method for the estimation of 6-mercaptopurine in bulk and pharmaceutical formulations

Cited by 8 publications

References 9 publications

Pharmacokinetic Profiling and Simultaneous Determination of Thiopurine Immunosuppressants and Folic Acid by Chromatographic Methods

Pharmacokinetic Profiling and Simultaneous Determination of Thiopurine Immunosuppressants and Folic Acid by Chromatographic Methods

Miniaturized shake-flask HPLC method for determination of distribution coefficient of drugs used in inflammatory bowel diseases

Development and Validation of a Liquid Chromatographic Method for the Quantification of Related Compounds in Cyclophosphamide

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