Journal : Acta Chromatographica
Article : Development and validation of a high-performance liquid chromatographic method for analysis of nimesulide residues on manufacturing equipment surfaces

Authors :
Daszykowski, M.
Silesian University Department of Chemometrics, Institute of Chemistry 9 Szkolna Street 40-006 Katowice Poland,
Sajewicz, M.
Silesian University Department of General Chemistry and Chromatography 9 Szkolna Street 40-006 Katowice Poland,
Rzepa, J.
Silesian University Department of General Chemistry and Chromatography 9 Szkolna Street 40-006 Katowice Poland,
Hajnos, M.
Medical University of Lublin Department of Pharmacognosy 1 Chodźki Street 20-093 Lublin Poland,
Staszek, D.
Silesian University Department of General Chemistry and Chromatography 9 Szkolna Street 40-006 Katowice Poland,
Wojtal, Ł.
Silesian University Department of General Chemistry and Chromatography 9 Szkolna Street 40-006 Katowice Poland,
Kowalska, T.
Silesian University Department of General Chemistry and Chromatography 9 Szkolna Street 40-006 Katowice Poland,
Waksmundzka-Hajnos, M.
Medical University of Lublin Department of Inorganic Chemistry 6 Staszica Street 20-081 Lublin Poland,
Walczak, B.
Silesian University Department of Chemometrics, Institute of Chemistry 9 Szkolna Street 40-006 Katowice Poland, beata@us.edu.pl,
Skalicka-Woźniak, K.
Medical University of Lublin Department of Pharmacognosy with Medicinal Plant Laboratory 1 Chodzki Str. 20-093 Lublin Poland,
Markowski, W.
Medical University of Lublin Department of Physical Chemistry Staszica 6 20-081 Lublin Poland,
Świeboda, R.
Medical University of Lublin Department of Inorganic and Analytical Chemistry Staszica 6 20-081 Lublin Poland,
Głowniak, K.
Medical University of Lublin Department of Pharmacognosy with Medicinal Plant Laboratory 1 Chodzki Str. 20-093 Lublin Poland,
Sultana, N.
University of Karachi Research Institute of Pharmaceutical Sciences, Department of Pharmaceutical Chemistry, Faculty of Pharmacy Karachi 75270 Pakistan,
Arayne, M. S.
University of Karachi Department of Chemistry Karachi 75270 Pakistan,
Naveed, S.
University of Karachi Research Institute of Pharmaceutical Sciences, Department of Pharmaceutical Chemistry, Faculty of Pharmacy Karachi 75270 Pakistan,
Shamshad, H.
University of Karachi Research Institute of Pharmaceutical Sciences, Department of Pharmaceutical Chemistry, Faculty of Pharmacy Karachi 75270 Pakistan,
Li, X.
China Agricultural University Department of Applied Chemistry, College of Science Beijing 100193 China,
Xu, J.
China Agricultural University Department of Applied Chemistry, College of Science Beijing 100193 China,
Jiang, Y.
China Agricultural University Department of Applied Chemistry, College of Science Beijing 100193 China,
Chen, L.
China Agricultural University Department of Applied Chemistry, College of Science Beijing 100193 China,
Xu, Y.
China Agricultural University Department of Applied Chemistry, College of Science Beijing 100193 China,
Pan, C.
China Agricultural University Department of Applied Chemistry, College of Science Beijing 100193 China,
Sheikhloie, H.
slamic Azad University, Science and Research Branch Department of Chemistry, Faculty of Science Poonak-Hesarak, Tehran Iran,
Saber-Tehrani, M.
slamic Azad University, Science and Research Branch Department of Chemistry, Faculty of Science Poonak-Hesarak, Tehran Iran,
Abrumand-Azar, P.
slamic Azad University, Science and Research Branch Department of Chemistry, Faculty of Science Poonak-Hesarak, Tehran Iran,
Waqif-Husain, S.
slamic Azad University, Science and Research Branch Department of Chemistry, Faculty of Science Poonak-Hesarak, Tehran Iran,
Mincea, M.
West University of Timişoara Faculty of Chemistry-Biology-Geography, Department of Chemistry Pestalozzi Street, 16 Timişoara 300115 Romania,
Lupşa, I.
Institute of Public Health Timişoara Department of Food Hygiene V. Babeş 16-18 Timişoara 300226 Romania,
Talpoş, I.
West University of Timişoara Multidisciplinary Research Platform “Nicholas Georgescu-Roegen” Oituz 4 Timişoara Romania,
Ostafe, V.
West University of Timişoara Faculty of Chemistry-Biology-Geography, Department of Chemistry Pestalozzi Street, 16 Timişoara 300115 Romania, vostafe@cbg.uvt.ro,
Milenović, D. M.
Zdravlje-Actavis Company, R&D Analytical Department 16000 Leskovac Serbia, dmilenovic@actavis.rs,
Todorović, Z. B.
University of Niš Faculty of Technology 16000 Leskovac Serbia,
Abstract : In the pharmaceutical industry it is important to remove drug residues from the equipment and areas used. Cleaning procedures must be validated, so special attention must be devoted to the methods used for analysis of trace amounts of drugs. To monitor a cleaning procedure, a high-performance liquid chromatographic method for analysis of nimesulide residues in swab samples has been developed and validated. The swabbing procedure was optimized to achieve suitable recovery of nimesulide from stainless steel. Mean recovery was >80% when two swabs were used. The precision of the results, reported as the relative standard deviation (RSD), was <2.00%. The method was validated over the concentration range 0.30–50.00 μg mL-1. Small amounts of the drug residues were analysed by HPLC with an ODS column (250 mm × 4.6 mm, 5-μm particles), at 20°C, with 65:35:3:0.13 ( v/v/v/w ) methanol-water-phosphate buffer (pH 3; 0.05 M )-sodium heptane sulfonate as mobile phase at a flow rate of 0.8 mL min-1. Nimesulide was detected at 235 nm. This procedure enabled simple, sensitive, and convenient HPLC analysis of nimesulide residues on stainless steel.

Keywords : cleaning validation, nimesulide, swab analysis, residues on surfaces,
Publishing house : University of Silesia in Katowice
Publication date : 2009
Number : Vol. 21, no. 4
Page : 603 – 618

Bibliography
: 1 Guide to Inspections Validation of Cleaning Processes, U.S. Food and Drug Administration available at: http://www.fda.gov/ICECI/Inspections/InspectionGuides/ucm074922.htm (accessed 27/10/2009)
2 World Health Organization, Supplementary guidelines on good manufacturing practices (GMP): Validation, Working document QAS/03.055/Rev.2, pp 24–33, available at: http://www.who.int/medicines/services/expertcommittees/pharmprep/Validation_QAS_055_Rev2combined.pdf (accessed 10 Oct, 2009)
3 Guidance on aspects of cleaning validation in active pharmaceutical ingredient plants, Active Pharmaceutical Ingredients Committee (APIC), pp 1–56, available at: http://apic.cefic.org/pub/pub-cleaning-validation.pdf (accessed 10 Oct, 2009)
4 D.A. Leblanc, Pharm. Technol., 22 , 136–148 (1998)
5 G.L. Fourman and M.W. Mullen, Pharm. Technol., 17 , 54–60 (1993)
6 B. Tubić, B. Ivković, M. Zečević, and S. Vladimirov, Acta Chim. Slov. 54 , 583–590 (2007)
7 A. Maltese, F. Maugeri, and C. Bucolo, J. Chromatogr. B, 804 , 441–443 (2004)
8 D.J. Jaworowitz Jr, M.T. Filipowski, and K.M.K. Boje, J. Chromatogr. B, 723 , 293–299 (1999)
9 V.B. Patravale, S. D’souza, and Y. Narkar, J. Pharm. Biomed. Anal., 25 , 685–688 (2001)
10 P.D. Tzanavaras and D.G. Themelis, J. Pharm. Biomed. Anal., 43 , 1483–1487 (2007)
11 S. Altinöz and Ö.Ö. Dursun, J. Pharm. Biomed. Anal., 22 , 175–182 (2000)
12 P. Kovarikova, M. Mokry, and J. Klimeš, J. Pharm. Biomed. Anal., 31 , 827–832 (2003)
13 G. Khaksa and N. Udupa, J. Chromatogr. B, 727 , 241–244 (1999)
14 M. Carini, G. Aldini, R. Stefani, C. Marinello, and R.M. Facino, J. Pharm. Biomed. Anal., 18 , 201–211 (1998)
15 M.J. Nozal, J.L. Bernal, J.J. Jimenez, M.T. Martin, and F.J. Diez, J. Chromatogr. A, 1024 , 115–122 (2004)
16 M.J. Nozal, J.L. Bernal, L. Toribio, M.T. Martin, and F.J. Diez, J. Pharm. Biomed. Anal., 30 , 285–291 (2002)
17 J. Lambropoulos, G.A. Spanos, and N.V. Lazaridis, J. Pharm. Biomed. Anal., 23 , 421–428 (2000)
18 M.B. Boca, Z. Apostolides, and E. Pretorius, J. Pharm. Biomed. Anal., 37 , 461–468 (2005)
19 R. Klinkenberg, B. Streel, and A. Ceccato, J. Pharm. Biomed. Anal., 32 , 345–352 (2003)
20 T. Mirza, M.J. Lunn, F.J. Keeley, R.C. George, and J.R. Bodenmiller, J. Pharm. Biomed. Anal., 19 , 747–756 (1999)
21 International Conference on Harmonization Q2 (R1): Validation of Analytical Procedures: Text and Methodology, available at: http://www.ich.org/cache/compo/276-254-1.html (accessed 10 Oct, 2009)
DOI :
Qute : Daszykowski, M. ,Sajewicz, M. ,Rzepa, J. ,Hajnos, M. ,Staszek, D. ,Wojtal, Ł. ,Kowalska, T. ,Waksmundzka-Hajnos, M. ,Walczak, B. ,Skalicka-Woźniak, K. ,Markowski, W. ,Świeboda, R. ,Głowniak, K. ,Sultana, N. ,Arayne, M. S. ,Naveed, S. ,Shamshad, H. ,Li, X. ,Xu, J. ,Jiang, Y. ,Chen, L. ,Xu, Y. ,Pan, C. ,Sheikhloie, H. ,Saber-Tehrani, M. ,Abrumand-Azar, P. ,Waqif-Husain, S. ,Mincea, M. ,Lupşa, I. ,Talpoş, I. ,Ostafe, V. ,Milenović, D. M. ,Todorović, Z. B. ,Todorović, Z. B. , Development and validation of a high-performance liquid chromatographic method for analysis of nimesulide residues on manufacturing equipment surfaces. Acta Chromatographica Vol. 21, no. 4/2009
facebook