DEVELOPMENT OF ANALYTICAL METHOD FOR IDENTIFICATION OF SIBUTRAMINE HCL IN TRADITIONAL MEDICINE USING SOLID PHASE EXTRACTION – HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

Authors

  • Tarita Kamardi Institut Teknologi Bandung

DOI:

https://doi.org/10.22159/ajpcr.2016.v9i6.14174

Abstract

Object: The purpose of this study is to develop a rapid and sensitive method for identifying sibutramine HCl.

 

Methods: Reversed phase solid phase extraction (SPE) method with Hydrophilic-Lipophilic Balance (HLB) cartridge was selected to be developed and optimized. Optimization was done by optimizing solvent in sample preparation and rinse solvent in washing step. The extract of SPE was injected into reversed phase HPLC with C18 column with PDA detector. Furthermore, the optimized results was validated which included specificity and determination of the detection limit. Validated analytical method was used to analyze sibutramine HCl qualitatively in slimming herbal medicine which was obtained from the market.

 

Results: Analysis method optimization results showed that the optimum sample solvent to extract sibutramine HCl in solid phase extraction was 3% orthophosphoric acid. Then it was shaken for 30 min and filtered, the filtrate was put in SPE cartridge that had been conditioned using ethanol and water. After rinsing with NH4OH solution in water and NH4OH solution in 80% ethanol, the analyte was eluted with acetonitrile. Identification of sibutramine HCl was done by HPLC at wavelength 254 nm. Sibutramine HCl gave maximum wavelength at 222 nm. Sibutramine HCl calibration curve gave quite linear results in the range from 0.10 to 0.50 mg/ml with R2 = 0.9966. The detection limit of this assay was 2.326 µg/ml. Specificity of this method is quite good. Simulation sample gave resolution for diethylpropion 2.415; sibutramine HCl 2.877 and amphetamine sulfate 5.673.This methods recovery was 38.0 to 45.0 %.

 

Conclusion: This study showed faster and specific method for identifying sibutramine HCl in traditional medicine.

 

Keywords: sibutramine HCl, solid phase extraction, HLB, slimming herbal medicine, HPLC

References

Doménech-Carbó A, Martini M, de Carvalho LM, Viana C, Doménech-Carbó MT, Silva M. Screening of pharmacologic adulterant classes in herbal formulations using voltammetry of microparticles. J Pharm Biomed Anal 2013;74:194-204.

Blahova E, Brandsteterova E. Approaches in sample handling before HPLC analysis of complex matrices. Chem Pap 2004;58(5):362-73.

Camel V. Solid phase extraction of trace elements (review). Spectrochim Acta Part B 2003;58(7):1177-233.

Zwir-Ferenc A, Biziuk M. Solid phase extraction technique – Trends, opportunities and applications (review). J Environ Stud 2006;15(5):677-90.

Waters, Oasis sample preparation - Diclofenac in rat plasma by LC/MS/MS. USA: Water Corporation; 2008. p. 31-2.

Ravichandran V, Shalini S, Sundram KM, Rajak H. Validation of analytical methods – Strategies & importance. Int J Pharm Pharm Sci 2010;2(3):18-22.

Imran MD, Pathade P. Development and validation of stability indicating uv spectrophotometric method for the estimation of sibutramine hydrochloride monohydrate in bulk and capsule dosage form. Int J Pharm Pharm Sci 2011;3(4):53-6.

Bhatt J, Shah B, Kambli S, Subbaiah G, Singh S, Ameta S. Rapid and sensitive method for the determination of sibutramine active metabolites in human plasma by reversed-phase liquid chromatography-tandem mass spectroscopy. J Chromatogr Sci 2007;45(2):91-6.

O’Neil MJ, Smith A, Heckelman PE, editors. The Merck Index. 13th ed. Whitehouse Station, NJ, USA: Merck&Co., Inc.; 2001. p. 1522.

Aceves-Hernández JM, Vázquez IN, Hinojosa-Torres J, Carrillo GP, Razo GA, Ruvalcaba RM. Sibutramine characterization and solubility, A theoretical study. J Mol Struct 2013;1038:163-9.

Tak YH, Toraño JS, Somsen GW, de Jong GJ. Optimization of in-line fritless solid-phase extraction for capillary electrophoresis-mass spectrometry. J Chromatogr A 2012;1267:138-43.

de Carvalho LM, Martini M, Moreira AP, de Lima AP, Correia D, Falcão T, et al. Presence of synthetic pharmaceuticals as adulterants in slimming phytotherapeutic formulations and their analytical determination. Forensic Sci Int 2011;204(1-3):6-12.

Phattanawasin P, Sotanaphun U, Sukwattanasinit T, Akkarawaranthorn J, Kitchaiya S. Quantitative determination of sibutramine in adulterated herbal slimming formulations by TLC-image analysis method. Forensic Sci Int 2012;219(1-3):96-100.

Ul Haq K, Kumar N. Validation of LC-MS method for the simultaneous estimation of itraconazole and its metabolite hydroxy itraconazole in plasma. Asian J Pharm Clin Res 2014;7(1):131-6.

Published

2016-11-01

How to Cite

Kamardi, T. “DEVELOPMENT OF ANALYTICAL METHOD FOR IDENTIFICATION OF SIBUTRAMINE HCL IN TRADITIONAL MEDICINE USING SOLID PHASE EXTRACTION – HIGH PERFORMANCE LIQUID CHROMATOGRAPHY”. Asian Journal of Pharmaceutical and Clinical Research, vol. 9, no. 6, Nov. 2016, pp. 201-9, doi:10.22159/ajpcr.2016.v9i6.14174.

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