Validasi Metode dan Analisis Penetapan Kadar Sibutramin HCl Pada Jamu Pelangsing dengan KCKT Fase Terbalik

Abstract

Abstrak

            Sibutramin hidroklorida (sibutramin HCl) merupakan bahan kimia obat yang sering ditambahkan pada jamu pelangsing. Penelitian ini bertujuan untuk mengidentifikasi dan memvalidasi metode penetapan kadar sibutramin HCl pada jamu pelangsing di Banjarmasin dengan menggunakan RP HPLC dengan detektor UV-Vis. Kondisi analisis menggunakan kolom Eurospher (5 µm, 250mm x 4,6 mm), fase gerak campuran dari kalium dihidrogen fosfat 50 mM dengan asetonitril (pH 5,5 dengan menambahkan asam ortofosfat 10%) (30:70 v/v), kecepatan alir 1 mL/menit pada panjang gelombang 225 nm. Waktu retensi dari sibutramin HCl adalah 4,69 menit. Hasil validasi metode dari linieritas, akurasi dan presisi telah sesuai dengan persyaratan validitas. Linieritas memperoleh koefisien korelasi (r)= 0,998 pada kisaran konsentrasi analisis 100 ppm sampai 300 ppm. Akurasi memperoleh  nilai 99,02% hingga 103,73%, dan presisi 3,34% hingga 6,84%. Batas deteksi (LOD) dan batas kuantifikasi (LOQ) masing-masing 16 ppm dan 53 ppm. Hasil menunjukan bahwa metode validasi ini akurat dan baik diaplikasikan untuk penetapan kadar sibutramin HCl pada jamu pelangsing. Metode penetapan kadar menunjukkan bahwa jamu pelangsing merek A dan merek B mengandung sibutramin HCl dengan kadar masing-masing 15,39 mg/kapsul dan 12,83 mg/kapsul.

Kata Kunci: KCKT, Fase Terbalik, validasi metode, sibutramin HCl

Abstract

Sibutramine hydrochloride (sibutramine HCl) is usually found in slimming traditional medicine as adulterant. The aims of this study were identification and validation method of quantitative determination of sibutramine HCl in slimming traditional medicine in Banjarmasin by reverse phase HPLC (High performance liquid chromatography) with UV-Vis detector. Condition analysis were used a Eurospher column (5 µm, 250 mm x 4,6 mm), mobile phase mixed buffer potassium dihydrogen phosphate 50 mM with acetonitrile (pH 5,5 adjusted with 10% Orthophosphoric acid) (30:70v/v), flow rate 1 mL/minute in 225 nm wave length. The retention time of sibutramine HCl was 4,69 minutes.Validation method result on linierity, accuracy, precision, limit of detection and quantification were effectively performed. The linierity was obtained with a correlation coefficient of 0.998 for analitycal range from  100 ppm to 300 ppm. Accuracy was 99.02% to 103.73%, and precision 3.34% to 6.84%. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 16 ppm and 53 ppm. The results indicated that this validation method were accurate and successfully applied for quantitative determination of sibutramine HCl in slimming traditional medicine. Quantitative determination method showed the slimming traditional medicine brand A and brand B contain sibutramine HCl of 15.39 mg/capsule and 12.83 mg/capsule respectively.

Keywords: RP HPLC, method validation, sibutramine hydrochloride