Penetapan Kadar Simultan Deksametason dan Metilprednisolon dengan Metode Kromatografi Gas Spektrometri Massa melalui Derivatisasi

  • Swasono R. Tamat Pusat Radioisotop dan Radiofarmaka BATAN
  • Ernawati Ernawati Laboratorium Pengawasan Doping, LABKESDA Jakarta
  • Linda Rosalina Laboratorium Pengawasan Doping, LABKESDA Jakarta
  • Sonny Pujianto Universitas Pancasila

Abstract

This investigation is intended to find a simultaneous assay method for glucocorticosteroids declared as doping compound by the International Olympic Committee. Experiments were carried out in the determination of dexamethason and methylprednisolon in urine matrix by gas chromatography-mass spectrometry (GC-MS) using various derivatisation reagents, reaction temperature and time. Selection of the best derivatisation reagent was based on the separation of total ion chromatogram (TIC) and appearance of three characteristic ions, m/z 305, 345,680 or m/z 206,456, 662 for dexamethasone; and m/ z 279, 369, 459 or m/z 147, 424, 644 for methylprednisolone. Dexamethasone and methylprednisolone derivates in the GC-MS spectra were identified by characteristic ions of m/z 305 (dexamethasone) and m/ z 279 (methylprednisolone). The best derivatisation yield was achieved by a combination of TMSI - [BSTFA-TMCS (99:1)](2:1) reacted at 90°C for 90 minutes, which produced a linear correlation between concentration (0-150 ng/ml ) and ratio of quantitation-ion abundance of standard compound/ion abundance of D3-testosterone internal standard with r= 0.9937 for dexamethasone and r=0.9823 for methylprednisolone; high precision CV=12.14% (dexamethasone) and CV=13.87%(methylprednisolone); high recovery for both dexamethasone and methylprednisolone, and LOD values of 4,44ng/ml (dexamethasone) and 1.80ng/ml (methylprednisolone). The method can be used for simultaneous quantitative assay of glucocorticosteroids, and has been validated for ten other glucocorticosteroid compounds.

References

1. Magiakou MA, Chrousos GP. Glucocorticoid therapy and adrenal supression; 2002. diambil dari: http:// www.endotext.com/adrenal/adrenal14/adrenalframe14.htm. diakses 14 Juli, 2004.

2. Glucocorticoids. diambil dari: http://cpharm.vetmed.vt.edu/vm8784/GLUCOCORTICOIDS/glucocort.htm.
diakses 14 Juli, 2004.

3. Laboratorium Pemeriksaan Doping dan Kesehatan Masyarakat. Buku panduan atlet. Jakarta: Pemerintah Provinsi Daerah Khusus Ibukota Jakarta, 2004; hal.1-2

4. Pereira HMG, Marques MAS, Cardoso JN, Neto FRA. Derivatization study on endogenous and synthetic corticosteroid by gas chromatography mass spectrometry. Rio de Janeiro: Ladetec Doping Control Laboratory; 2001. p.1-15.
5. Knapp DR. Handbook of analytical derivatization reaction. South Carolina: South Carolina's Departement of Pharmacology Medical University of South Carolina; 1979.p.2,9, 12.

6. Poole CF, Polle SK. Chromatography today. Amsterdam: Elsevier Science; 1991. p. 982.

7. Departemen Kesehatan Republik Indonesia. Farmakope Indonesia. Edisi IV. Jakarta: Direktorat Jenderal Pengawasan Obat dan Makanan; 1995. hal.286-7.

8. Moffat AC, Clarke's. Isolation and identification of drug. Second edition. London: The Pharmaceutical Press; 1986.p.772.

9. Laboratorium Pengawasan Doping Jakarta. Instruksi kerja pembuatan urin blanko. Jakarta: Laboratorium Kesehatan Provinsi Daerah Khusus Ibukota Jakarta; 2003. hal. 1.

10. Laboratorium Pengawasan Doping Jakarta. Instruksi kerja skrinning anabolik steroid dengan seppak C18. Jakarta : Laboratorium Kesehatan Provinsi Daerah Khusus Ibukota Jakarta; 2003. hal. 3-4.

11. Badan Pengawas Obat dan Makanan. Petunjuk operasional penerapan cara pembuatan obat yang baik. Edisi 2001. Jakarta: Badan Pengawas Obat dan Makanan; 2001. hal.412-21.

12. Sumardi. Validasi metode pengujian. Jakarta : Badan Standardisasi Nasional; 2001. hal.15.

13. Sriwoelan S. Validasi dan pemilihan metode analisis. Jakarta: Prosiding Temu Ilmiah Nasional Bidang
Farmasi VI; 1997. hal.17.

14. Laboratorium Pengawasan Doping Jakarta. Instruksi kerja pelaksanaan validasi metode analisis. Jakarta: Laboratorium Kesehatan Provinsi Daerah Khusus Ibukota Jakarta; 2003. hal.13.

15. Urine, anatomy and physiology. diambil dari http:// reference.allrefer.com/encyclopedia/U/urinehtml diakses 17 Agustus, 2004.
How to Cite
TAMAT, Swasono R. et al. Penetapan Kadar Simultan Deksametason dan Metilprednisolon dengan Metode Kromatografi Gas Spektrometri Massa melalui Derivatisasi. JURNAL ILMU KEFARMASIAN INDONESIA, [S.l.], v. 4, n. 2, p. 60-73, sep. 2006. ISSN 2614-6495. Available at: <http://jifi.farmasi.univpancasila.ac.id/index.php/jifi/article/view/589>. Date accessed: 05 nov. 2024.
Citation Formats
Issue
Vol 4 No 2 (2006): JIFI
Section
Articles

Licencing
All articles in Jurnal Ilmu Kefarmasian Indonesia are an open-access article, distributed under the terms of the Creative Commons Attribution-NonCommercial-ShareAlike 4.0 International License which permits unrestricted non-commercial used, distribution and reproduction in any medium.

This licence applies to Author(s) and Public Reader means that the users mays :

  • SHARE:
    copy and redistribute the article in any medium or format
  • ADAPT:
    remix, transform, and build upon the article (eg.: to produce a new research work and, possibly, a new publication)
  • ALIKE:
    If you remix, transform, or build upon the article, you must distribute your contributions under the same license as the original.
  • NO ADDITIONAL RESTRICTIONS:
    You may not apply legal terms or technological measures that legally restrict others from doing anything the license permits.

It does however mean that when you use it you must:

  • ATTRIBUTION: You must give appropriate credit to both the Author(s) and the journal, provide a link to the license, and indicate if changes were made. You may do so in any reasonable manner, but not in any way that suggests the licensor endorses you or your use.

You may not:

  • NONCOMMERCIAL: You may not use the article for commercial purposes.

Creative Commons License

This work is licensed under a Creative Commons Attribution-NonCommercial-ShareAlike 4.0 International License.