PENGEMBANGAN METODE ANALISIS IDENTIFIKASI SIBUTRAMIN HCL DALAM OBAT TRADISIONAL SEDIAAN PADAT DENGAN EFP - KCKT

• Main Author: Kamardi, Tarita
• Format: Theses
• Language: Indonesia
• Online Access: https://digilib.itb.ac.id/gdl/view/79066
• Institution: Institut Teknologi Bandung

Background and purpose : The addition of sibutramine HCl in slimming herbal is still found. Whereas this chemical drug has been withdrawn from the market and banned by Badan POM RI. This prohibition is based on the study results of the Sibutramine Cardiovascular Outcomes Trial ( SCOUT ) which showed that an increasing risk of cardiovascular events. The purpose of this study is to develop a rapid and sensitive method for identifying sibutramine HCl. Methods : The old method using liquid extraction - liquid is expected to be accelerated by using solid phase extraction (SPE). Solid phase extraction method with reversed phase type is selected to be developed and optimized because the identified analyte is an organic compound which is nonpolar. Hydrophilic lipophilic balance ( HLB ) Cartridge is chosen because it is a universal sorbent for reversed phase. HLB sorbent contains copolymer of m - divynilbenzene which is lipophilic and N – vinylpyrrolidone which is hydrophilic. Polymer sorbent is more resistant to the effects of water than silica – based sorbent . From the development of analytical methods, it is specified factors which significantly influence the results of the SPE. Optimization is done starting from the optimization of sample solvent before solid phase extraction to the election of washer in washing stage. The extract of SPE is injected into reversed phase HPLC with a C18 column and a spectrophotometer detector. Furthermore, the optimized results are validated which is include specificity and determination of the detection limit. Validated analytical methods are used to analyze sibutramine HCl qualitatively in slimming herbal samples which is obtained from the market. Results : Analysis method development shows that factors which significantly influence the results of extraction are the sample solvent and a rinse solution. Analysis method optimization produces results that the optimum sample solvent to draw sibutramine HCl prior to solid phase extraction is 3% orthophosphoric acid and then shaken for 30 min and filtered , then the filtrate is put in EFP cartridge that had been conditioned with ethanol and water , then rinsed with a solution of NH4OH in water and a solution of NH4OH in 80 % ethanol, the analytes are eluted with acetonitrile. Identification of sibutramine HCl is done by HPLC at a wavelength of 254 nm. Sibutramine HCl gives maximum absorption at a wavelength of 222 nm. Sibutramine HCl calibration curve gives results quite linear in the range from 0,10 to 0,50 mg/mL. Linearity of this method gives a correlation coefficient, R2 = 0,9966. Detection limits are calculated from the linearity curve of sibutramine HCl followed by the determination from the standard deviation. The further results are tested by solid-phase extraction method to obtain the actual detection limit. The obtained detection limit of this assay is 2,326 ug/mL. Specificity of this method is quite good. Simulation test of the slimming herbal sample with addition of sibutramine HCl, dietilpropion and amphetamine sulfate gives resolution dietilpropion 2,415; sibutramin HCl 2,877 and amphetamine sulfate 5,673. From linearity assay, it is also calculated the recovery of this analytical method. Recovery only gives 38,0 to 45,0 % . This small recovery is likely due to some analytes are brought on washing stage or all analytes which are retained in the sorbent are not eluted completely by acetonitrile. Conclusion : This study results in the faster and specific identification methods of sibutramine HCl in traditional medicine. Liquid - liquid extraction followed thin-layer chromatography in the old method is replaced with a solid phase extraction step. But it is still less sensitive than the method of analysis by liquid - liquid extraction.