Isoniazid (INH) and pyrazinamide (PZA) are first-line drugs in the treatment of meningitis of tuberculosis, in addition to rifampicin. The use of these drugs will determine the success of therapy to kill Mycobacterium tuberculosis in brain tissue that is difficult to penetrate by other drugs. Therefore, it is necessary to conduct research and monitor the use of this drug in plasma and cerebrospinal fluid (CSF) patients with TBM. This study aimed to determine the method of analysis of INH and PZA using Ultra Performance Liquid Chromatography Ultra Violet (UPLC-UV). The samples were taken from TBM patients who taken INH-PZA and others besides TBM patients who did not take INH-PZA. The analytic method carried out includes a comparison of the results of the analysis method for measuring levels of standard INH-PZA and INH-PZA in plasma and CSF samples. Analysis of INH-PZA in plasma and CSF can be performed using UPLC with UV detector, at least 100 uL plasma or CSF samples volume, with reproducible and accurate results.
Metformin is oral hypoglycemic or blood sugar-lowering drug which is used for the first-line drug in the treatment of diabetes mellitus type 2. This study presented the validated of Ultra Performance Liquid Chromatography UltraViolet (UPLC-UV) method for the determination of metformin in human plasma. Metformin levels were measured using UPLC with UV detector and liquid-liquid extraction method. Separation was carried out on a Acquity UPLC HSS T3 100mm × 2.1mm i.d. column (1.8μm partikel size) using gradient elution of acetonitrile and phosphate buffer 0.02 M (0.6 mL/min) as mobile phase at 30°C. The analyte was monitored at 236 nm. No endogenous substances were found to interfere with the peaks of drug and internal standard. The value of percent deviation and the coefficient variation obtained respectively less than the percentage set in the FDA guidelines. The linearity factor values were more than 0.997 and LOD was 0.01µg/mL. UPLC with UV detector is able to analyze metformin in a short time with good precision and accuracy which is useful for bioequivalence and bioavailability studies.
Abstrak: Digoksin merupakan glikosida kardioaktif, salah satu senyawa yang penting dalam terapi yang saat ini tersedia sebagai obat untuk pengobatan penyakit jantung. Penggunaan obat ini meningkat sejalan dengan bertambahnya penderita penyakit jantung. Oleh karena itu, perlu dilakukan penelitian dan monitoring penggunaan obat ini pada penderita penyakit jantung dalam proses terapi kesembuhan. Tujuan dari penelitian ini adalah untuk mengetahui metode analisis digoksin dengan menggunakan alat Ultra Performance Liquid Chromatography (UPLC). Digoksin yang digunakan adalah Fargoksin (Injection 0,25 mg/mL, ampoule/berbentuk cairan). Pengenceran digoksin dilakukan dengan penambahan pelarut metanol. Kolom yang digunakan adalah kolom BEH C18. Optimasi metode analisis yang dilakukan meliputi perbandingan pelarut yang digunakan, suhu kolom, dan laju alir. Setelah melakukan optimasi, diperoleh kondisi fasa gerak yang optimum adalah larutan air-asetonitril (72:28%), laju alir 0,3 mL/menit, waktu selama ± 6 menit, suhu kolom off, dan detektor yang digunakan adalah spektrofotometer UV dengan panjang gelombang 218 nm. Pengulangan analisis dengan menggunakan hasil yang diperoleh secara optimum dilakukan sebanyak sepuluh kali. Berdasarkan data tersebut, proses analisis dengan menggunakan UPLC dapat berlangsung lebih cepat dibandingkan dengan menggunakan HPLC. Kata kunci: UPLC, Digoksin, Bioanalisis Abstract: Cardioactive glycoside Digoxin is one of the important compounds in therapy that is currently available as a drug for the treatment of heart disease. The use of these drugs increases as the growth of heart disease patient, so it is necessary to research and to monitor these drugs in patients with heart disease in the process of healing therapy. The purpose of this study was to examine the method of digoxin analysis by using Ultra Performance Liquid Chromatography (UPLC). Digoxin used was Fargoksin (Injection 0.25 mg/mL, ampoule/liquid forms). Methanol was used to prepare digoxin solutions. A BEH C18 column was used.Optimization was conducted by selecting experimental conditions to include composition of eluent used, column temperature, and flow rate of mobile phase. It was found that the optimal conditions were: mobile phase, water:acetonitrile (72:28, v/v); flow rate, 0.3 mL/min; elution time, 6 minutes; column temperature, ambient (room temperature); and detection of eluates, UV detector at 218 nm. The analysis of a digoxin sample has been done using the optimal experimental conditions. In order to get the best analytical data, a ten replicates experiment has been done. Based on data collected, it was found that using UPLC, analysis time was shorter than analysis time in analysis using HPLC.
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