Impurity profile study of lopinavir and validation of HPLC method for the determination of related substances in lopinavir drug substance

Chitturi, Sreenivasa Rao; Bharathi, Ch.; Reddy, A. Venugopal; Reddy, K. Krishna; Sharma, Hemant; Handa, V. K.; Dandala, Ramesh; Bindu, V. Hima

doi:10.1016/j.jpba.2008.09.015

Cited by 20 publications

(10 citation statements)

References 19 publications

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“…It is necessary to analyze within a suitable range for which the instrument's response must be proportional to the drug concentration. Normally, value of co-relation coefficient (R 2 ) >0.998 is acceptable [28].…”

Section: Linearitymentioning

confidence: 99%

Nano Formulation Analysis: Analytical Method Development of Isoniazid and Simultaneous Estimation of Anti-Tubercular Drugs Isoniazid and Rifampicin by Rp-HPLC

Hakkimane

Guru

2017

Asian J Pharm Clin Res

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Objective: The objective of the study was to develop and validate a simple and reproducible reverse phase high pressure liquid chromatography (RP-HPLC) method for hydrophilic drug isoniazid (INH) to apply for the analysis of the INH in nanoparticle drug formulations. Furthermore, to estimate simultaneously rifampicin (RIF) and INH in combined form. Methods:Isocratic elution with 10 minutes runtime on a C-18 Luna, 5 µ, 100Å, 150 mm column, methanol, and water as mobile phase with detection wavelength at 268 nm was used. INH nanoformulations were prepared by double emulsion solvent evaporation technique. Quantitative analysis of encapsulated drug was estimated via developed RP-HPLC method. Simultaneous estimation for the two drugs was carried out by gradient elution. All chromatographic separation and estimations were obtained on Shimadzu HPLC system. Results:INH eluted with a short retention time (RT) of 4.06 minutes. Method showed good linearity in the range of concentrations 0.01-100 µg/ml. The limit of detection (LOD) and quantification (LOQ) for INH was 0.03 and 0.12 µg/mL, respectively, and developed method has been successfully applied for the analysis of drugs in nanoparticle formulations. Simultaneous estimation of antitubercular drugs INH and RIF showed two separate peaks within specified runtime. Conclusion:Developed method showed good resolved peaks. Since the RT is short, in a shorter duration more samples could be completed and developed method will be easy for analyzing greater number of samples. Analysis of nanoformulation results have shown that this method is simple, reliable, reproducible, hence can be applied for drug delivery analysis.

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Section: Linearitymentioning

confidence: 99%

Nano Formulation Analysis: Analytical Method Development of Isoniazid and Simultaneous Estimation of Anti-Tubercular Drugs Isoniazid and Rifampicin by Rp-HPLC

Hakkimane

Guru

2017

Asian J Pharm Clin Res

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“…conventional liquid chromatography (Lc) coupled to mass spectrometry (MS) has been widely employed in the field of impurity profiling. 1,2 However, in addition to being time consuming, Lc-MS analysis sometimes brings a requirement for sample work-up, such as extraction, evaporation or filtration. In recent years, the use of several ambient desorption ionisation techniques have been reported for surface analyses of liquid and solid samples with subsequent MS detection.…”

Section: Journal Of Mass Spectrometrymentioning

confidence: 99%

Rapid Detection and Identification of Impurities in Ten 2-Naphthalenamines Using an Atmospheric Pressure Solids Analysis Probe in Conjunction with Ion Mobility Mass Spectrometry

Pan

Lundin

2011

Eur J Mass Spectrom (Chichester)

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The atmospheric pressure solids analysis probe (ASAP), in conjunction with ion mobility time-of-flight mass spectrometry (IM-ToF-MS), has been applied to the impurity profiling study of ten 2-naphthalenamines. The impurity profiles achieved by ASAP-IM-MS were compared with those obtained by liquid chromatography-electrospray ionisation-mass spectrometry (LC-ESI-MS). All the impurities at the level of 0.1 area % and above, except for one, detected by LC-ESI-MS, were also found by ASAP-IMS analyses. In addition, one non-polar compound was detected by ASAP-IM-MS alone. The IM-MS plot of ion drift time versus m/z values offered sufficient separation between the impurities with different m/z. Therefore, instead of LC as a separation tool, IM-MS is able to provide fingerprint profiling for the ten samples analysed. The time of each analysis has been reduced from 25 min by LC-MS to less than 3 min by ASAP-IM-MS. When collision energy was applied for the selected precursor ion in the transfer T-wave, a clean MS/MS spectrum was obtained for structural elucidation of unknown impurities. The hyphenation of ASAP and IM-MS techniques represents a highly efficient approach for rapid detection and identification of impurities generated in complex reactions involved in pharmaceutical development.

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“…According to ICH guidelines on impurities in new drug products, identification of impurities below the 0.1% level is not considered to be necessary, unless potential impurities are expected to be unusually potent or toxic. According to ICH, the maximum daily dose qualification threshold is considered as follows; ≤ 2g/day 0.1% or 1 mg per day intake (whichever is lower) ≥ 2g/day 0.05% [9][10][11][12].…”

Section: Introductionmentioning

confidence: 99%

Development and Validation of RP-HPLC Method for the Identification of Process Related Impurities of Zolmitriptan

Dighe¹

2017

JAPLR

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The study was focused toward synthesis, characterization and quantification of 3-Ethyl-indole impurity in Zolmitriptan formulations by Reverse Phase High Performance Liquid Chromatography method. The synthesis of a process related impurity of Zolmitriptan was successfully carried out by Fischer indole procedure. The impurity was purified by column chromatography. Characterization was done by I.R, 1 H-NMR, 13C-NMR and GC-MS. Based on the spectral data, the structure of impurity was characterized as 3-Ethyl-indole. An efficient isocratic RP-HPLC was developed and validated according to ICH guidelines with respect to specificity, accuracy, linearity and precision. The validated HPLC method was used for detection and quantitation of 3-Ethyl-indole, a process related impurity of Zolmitriptan, from Zolmitriptan tablet formulations. The above method was found to be specific, accurate, precise, rugged and robust and can be used for routine analysis.

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Impurity profile study of lopinavir and validation of HPLC method for the determination of related substances in lopinavir drug substance

Cited by 20 publications

References 19 publications

Nano Formulation Analysis: Analytical Method Development of Isoniazid and Simultaneous Estimation of Anti-Tubercular Drugs Isoniazid and Rifampicin by Rp-HPLC

Nano Formulation Analysis: Analytical Method Development of Isoniazid and Simultaneous Estimation of Anti-Tubercular Drugs Isoniazid and Rifampicin by Rp-HPLC

Rapid Detection and Identification of Impurities in Ten 2-Naphthalenamines Using an Atmospheric Pressure Solids Analysis Probe in Conjunction with Ion Mobility Mass Spectrometry

Development and Validation of RP-HPLC Method for the Identification of Process Related Impurities of Zolmitriptan

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