Validation of an HPLC-UV method for the determination of digoxin residues on the surface of manufacturing equipment

Abstract

In the pharmaceutical industry, an important step consists in the removal of possible drug residues from the involved equipments and areas. The cleaning procedures must be validated and methods to determine trace amounts of drugs have, therefore, to be considered with special attention. An HPLC-UV method for the determination of digoxin residues on stainless steel surfaces was developed and validated in order to control a cleaning procedure. Cotton swabs, moistened with methanol were used to remove any residues of drugs from stainless steel surfaces, and give recoveries of 85.9, 85.2 and 78.7 % for three concentration levels. The precision of the results, reported as the relative standard deviation (RSD), were below 6.3 %. The method was validated over a concentration range of 0.05-12.5 ?g mL-1. Low quantities of drug residues were determined by HPLC-UV using a Symmetry C18 column (150?4.6) mm, 5 ?m) at 20?C with an acetonitrile-water (28:72, v/v) mobile phase at a flow rate of 1.1 mL min-1, an injection volume of 100 ?L and were detected at 220 nm. A simple, selective and sensitive HPLC-UV assay for the determination of digoxin residues on stainless steel was developed, validated and applied.

Analisis Glikosida Kardioaktif Digoksin Menggunakan Ultra Performance Liquid Chromatography (Uplc)

“…Beberapa penelitian telah dilakukan untuk analisis digoksin menggunakan alat HPLC (High Performance Liquid Chromatography) dengan menggunakan detektor UV (Jedlicka et al, 2003;Todorovic et al, 2009).…”

“…Konsentrasi fasa gerak antara asetonitril-air yang digunakan adalah sebesar 28:72 (%) (Jedlicka et al, 2003), sedangkan penelitian yang dilakukan oleh Kelly et al (1995) fasa gerak yang digunakan adalah asetonitril-air 23:77 (%). Kondisi yang digunakan adalah kondisi isokratik dengan laju alir 1,1 mL/menit (Jedlicka et al, 2003;Todorovic et al, 2009). Panjang gelombang yang digunakan berasal dari berbagai sumber sebagai perbandingan, panjang gelombang yang digunakan dari detektor HPLC-UV sebesar 218 nm (Jedlicka et al, 2003), pada penelitian Todorovic et al (2009) digoksin terdeteksi pada panjang gelombang 220 nm.…”

“…Kondisi yang digunakan adalah kondisi isokratik dengan laju alir 1,1 mL/menit (Jedlicka et al, 2003;Todorovic et al, 2009). Panjang gelombang yang digunakan berasal dari berbagai sumber sebagai perbandingan, panjang gelombang yang digunakan dari detektor HPLC-UV sebesar 218 nm (Jedlicka et al, 2003), pada penelitian Todorovic et al (2009) digoksin terdeteksi pada panjang gelombang 220 nm. Waktu analisis yang digunakan juga bervariasi dengan menggunakan HPLC dengan detektor UV yaitu terdapat waktu analisis selama 6 menit (Milenkovic et al, 2010), 8 menit (Jedlicka et al, 2003, 12 menit (Todorovic et al, 2009;Adamowicz et al, 2002), 13 menit (Sauvage & Marquet, 2007) dan 14 menit (Kelly et al, 1995) BAHAN DAN METODE Peralatan UPLC yang digunakan merupakan UPLC HClass dengan detektor TUV produk Waters.…”

An HPLC method for the determination of digoxin in dissolution samples

“…2 The run time cycle was completed in 10 min, while for the robustness test, it was set on 20 min. Peak areas registered at 220 nm were used for digoxin quantification.…”

“…[2][3][4][5][6][7][8][9][10][11][12][13] There are some methods reported for digoxin determination after a dissolution test. [14][15][16] In the United States Pharmacopoeia (USP), 0.1 M hydochloric acid (HCl) and in the Japanese Pharmacopoeia (JP), diluted HCl is used as the dissolution medium, 17,18 while distilled water is employed as the dissolution medium in the British Pharmacopeia (BP).…”