Determination and Validation of Duloxetine Hydrochloride in Capsules by HPLC with Pre-Column Derivatization and Fluorescence Detection

• Published in: Journal of chromatographic science Vol. 50; no. 6; pp. 494 - 498
• Main Author: Tatar Ulu, Sevgi
• Format: Journal Article
• Language: English
• Published: Niles, IL Oxford University Press 01.07.2012; Preston Publications
• Subjects: Adjustment; Analysis; Antidepressive Agents - analysis; Biological and medical sciences; Capsules - analysis; Chromatography; Chromatography, High Pressure Liquid - methods; Duloxetine Hydrochloride; Emission; Fluorescence; General pharmacology; Hydrochlorides; Liquids; Medical sciences; Methyl alcohol; Pharmacology. Drug treatments; Spectrometry, Fluorescence - methods; Thiophenes - analysis; Wavelengths; Validation; Fluorescence detector; Chemical analysis; Serotonin; Precolumn; Psychotropic; HPLC chromatography; Oral form; Duloxetine; Reuptake inhibitor; Derivatization; Fluorescent labelling; Dosage form; Antidepressant agent; Hard capsule; Quantitative analysis
• ISSN: 0021-9665; 1945-239X
• DOI: 10.1093/chromsci/bms034

A high-performance liquid chromatographic (HPLC) method is described for the determination of duloxetine hydrochloride in capsules. The method was based on pre-column derivatization with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole using the fluorimetric detection technique. Duloxetine hydrochloride was analyzed by HPLC using an Inertsil C18 column (5 μm, 150 × 4.6 mm) and mobile phase consisted of methanol and water (65:35, v/v). The fluorescence detector was adjusted at excitation and emission wavelengths of 461 and 521 nm, respectively. The linearity of the method was in the range of 10-600 ng/mL. Limits of detection and quantification were 0.51 and 1.53 ng/mL, respectively. The proposed method was successfully applied for determination of duloxetine hydrochloride in its pharmaceutical preparation. The results were in good agreement with those obtained using a reference method.