title: Stability-indicating HPLC determination of gemcitabine in pharmaceutical formulations.
abstract: A simple, sensitive, inexpensive, and rapid stability indicating high performance liquid chromatographic method has been developed for determination of gemcitabine in injectable dosage forms using theophylline as internal standard. Chromatographic separation was achieved on a Phenomenex Luna C-18 column (250 mm × 4.6 mm; 5μ) with a mobile phase consisting of 90% water and 10% acetonitrile (pH 7.00 ± 0.05). The signals of gemcitabine and theophylline were recorded at 275 nm. Calibration curves were linear in the concentration range of 0.5-50 μg/mL. The correlation coefficient was 0.999 or higher. The limit of detection and limit of quantitation were 0.1498 and 0.4541 μg/mL, respectively. The inter- and intraday precision were less than 2%. Accuracy of the method ranged from 100.2% to 100.4%. Stability studies indicate that the drug was stable to sunlight and UV light. The drug gives 6 different hydrolytic products under alkaline stress and 3 in acidic condition. Aqueous and oxidative stress conditions also degrade the drug. Degradation was higher in the alkaline condition compared to other stress conditions. The robustness of the methods was evaluated using design of experiments. Validation reveals that the proposed method is specific, accurate, precise, reliable, robust, reproducible, and suitable for the quantitative analysis.
authors.affiliation: Faculty of Pharmacy, Integral University, Kursi Road, Lucknow 226-026, India.
authors.forename: Rahul
authors.initials: R
authors.lastname: Singh
authors.affiliation: Faculty of Pharmacy and Medical Sciences, Al-Ahliyya Amman University, P.O. Box 263, Amman 19328, Jordan.
authors.forename: Ashok K
authors.initials: AK
authors.lastname: Shakya
authors.affiliation: Faculty of Pharmacy and Medical Sciences, Al-Ahliyya Amman University, P.O. Box 263, Amman 19328, Jordan.
authors.forename: Rajashri
authors.initials: R
authors.lastname: Naik
authors.affiliation: Faculty of Pharmacy and Medical Sciences, Al-Ahliyya Amman University, P.O. Box 263, Amman 19328, Jordan.
authors.forename: Naeem
authors.initials: N
authors.lastname: Shalan
references.citation: J Chromatogr B Analyt Technol Biomed Life Sci. 2003 Jul 5;791(1-2):103-9
references.pmid: 12798170
references.citation: J Chromatogr B Analyt Technol Biomed Life Sci. 2006 May 1;835(1-2):136-42
references.pmid: 16584929
references.citation: J Chromatogr B Analyt Technol Biomed Life Sci. 2006 Aug 7;840(1):44-9
references.pmid: 16725385
references.citation: Farmaco. 2004 May;59(5):425-9
references.pmid: 15120323
references.citation: Acta Pharmacol Sin. 2004 Dec;25(12):1584-9
references.pmid: 15569401
references.citation: J Chromatogr B Analyt Technol Biomed Life Sci. 2003 Feb 25;785(1):65-72
references.pmid: 12535839
references.citation: J Mass Spectrom. 2008 Feb;43(2):216-23
references.pmid: 17941128
references.citation: J Pharm Sci. 2000 Jul;89(7):885-91
references.pmid: 10861589
references.citation: J Chromatogr B Analyt Technol Biomed Life Sci. 2004 Apr 5;802(2):263-70
references.pmid: 15018786
references.citation: Rapid Commun Mass Spectrom. 2007;21(14):2312-22
references.pmid: 17577879
references.citation: J Chromatogr B Biomed Appl. 1995 Mar 10;665(1):171-81
references.pmid: 7795789
references.citation: Curr Drug Targets. 2013 Aug;14(9):1061-9
references.pmid: 23721184
references.citation: J Sep Sci. 2007 Aug;30(12):1811-20
references.pmid: 17638352
references.citation: J Liposome Res. 2012 Dec;22(4):263-9
references.pmid: 22428966
references.citation: J Am Pharm Assoc (Wash). 1999 Jul-Aug;39(4):509-13
references.pmid: 10467815
references.citation: J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Oct 15;858(1-2):71-8
references.pmid: 17851141
references.citation: J Pharm Biomed Anal. 2014 Sep;98:371-8
references.pmid: 24998672
references.citation: Anal Bioanal Chem. 2010 Dec;398(7-8):3033-42
references.pmid: 20927508
references.citation: J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Mar 1;847(2):142-52
references.pmid: 17056304
references.citation: J Pharm Sci. 1994 May;83(5):716-9
references.pmid: 8071827