Advertisement

Steroid Analysis pp 1097-1153 | Cite as

Industrial and Compendial Steroid Analysis

  • Sándor GörögEmail author
Chapter

Abstract

The aim of this section is to give an overview of the requirements of steroid analysis in pharmaceutical industry and to cover the methodological aspects of these requirements with regard to quality control of bulk steroid drugs and drug formulations. Although this is an important area, the challenges here are not comparable with those in biological–clinical steroid analysis, which was the sole topic of the first edition of this book. This is reflected by the much smaller number of research publications dealing with this pharmaceutical area of steroid analyses. Only a few (more or less obsolete) books are available (Görög and Szász, 1978; Görög, 1983, 1989). The newer developments in this area are summarised in a comprehensive review (Görög, 2004), on which this chapter is based.

Keywords

Fluticasone Propionate Triamcinolone Acetonide Beclomethasone Dipropionate Supercritical Fluid Chromatography Mometasone Furoate 
These keywords were added by machine and not by the authors. This process is experimental and the keywords may be updated as the learning algorithm improves.

References

  1. Agbaba D, Eric S, Markovic G, Nedeljkovic V, Veselinovic S, Vucetic M (2000) The application of HPTLC in the quantitative analysis of drugs. J. Planar Chromatogr. 13; 333–336.Google Scholar
  2. Agbaba D, Milojevic Z, Eric S, Aleksic M, Markovic G, Solujic M (2001) The high-performance thin-layer chromatographic determination of dexamethasone and xylometazoline in nasal drops containing different preservatives. J. Planar Chromatogr. 14; 322–325.Google Scholar
  3. Ahmed SM, Arcuri F, Li F, Moo-Young AJ, Monder C (1995) Accelerated stability studies on 16-methylene-17 a-acetoxy-19-nor-pregne-4-ene-3,20-dione (NestoroneTM). Steroids. 60; 534–539.Google Scholar
  4. Amundsen LK, Kokkonen JT, Rovio S, Siren H (2004) Analysis of anabolic steroids by partial filling micellar electrokinetic capillary chromatography and electrospray mass spectrometry. J. Chromatogr. A 1040; 123–131.Google Scholar
  5. Anderson NH, Gray MR, Hinds CJ (1990) Diode-array detection of low-level co-eluting species in high-performance liquid chromatography. J. Pharm. Biomed. Anal. 8; 853–857.Google Scholar
  6. Arthur KE, Wolff J-C, Carrier DJ (2004) Analysis of betamethasone, dexamethasone and related compounds by liquid chromatograph/electrospray mass spectrometry. Rapid. Commun. Mass Spectrom. 18; 678–684.Google Scholar
  7. Assi KH, Tarsin W, Chrystyn H (2006) High performance liquid chromatography assay for simultaneous determination of formeterol and budesonide in Symbicort Turbuhaler. J. Pharm. Biomed. Anal. 41; 325–328.Google Scholar
  8. Aubeck R, Bräuchle C, Hampp N (1990) Ion-selective membrane electrodes for the determination of the muscle relaxants pancuronium, tubocuranine, gallamine and succinylcholine. Anal. Chim. Acta 238; 405–110.Google Scholar
  9. Babják M, Balogh G, Gazdag M, Görög S (2002) Analysis of Steroids. Part 55. LC/UVMS study of the impurity profile of ethynodiol diacetate. J. Pharm. Biomed. Anal. 29; 1153–1157.Google Scholar
  10. Bachman WJ, Gambertoglio JG (1990) A stability-indicating LC assay for prednisolone sodium phosphate in inplantable infusion pumps. Anal. Lett. 23; 893–900.Google Scholar
  11. Baggiani C, Giraudi G, Trotta R, Giovannoli C, Vanni A (2000) Chromatographic characterization of a molecular imprinted polymer binding cortisol. Talanta. 51; 71–75.Google Scholar
  12. Bagócsi B, Fábián D, Laukó A, Mezei M, Mahó S, Végh Z, Ferenczi-Fodor K (2002) Comparison of OPLC and other chromatographic methods (TLC, LC, and GC) for in-process purity testing of nandrolone. J. Planar Chromatogr. 15; 42–257.Google Scholar
  13. Bagócsi B, Rippel G, Mezei M, Végh Z, Ferenczi-Fodor K (2003) OPLC, a method between TLC and LC, for purity testing of norethisterone bulk drug substance and tablet. J. Planar Chromatogr. 16; 359–362.Google Scholar
  14. Balogh G, Csizér É, Ferenczy GyG, Halmos Zs, Herényi B, Horváth P, Laukó A, Görög S (1995) Analysis of steroids. Part 46. Isolation and identification of an isomeric impurity in danazol. Pharm. Res. 12; 295–298.Google Scholar
  15. Barron D, Pascual JA, Segura J, Barbosa J (1995) Prediction of LC retention of steroids using solvatochromic parameters. Chromatographia. 41; 573–580.Google Scholar
  16. Bartolomei M (2000) Solid-state studies on the hemihydrate and anhydrous forms of flunisolide. J. Pharm. Biomed. Anal. 24; 81–93.Google Scholar
  17. Bartolomei M, Ramusino MC, Ghetti P (1997) Solid-state investigation of fluocinolone acetonide. J. Pharm. Biomed. Anal. 15; 1813–1820.Google Scholar
  18. Beckstead HD, Neville GA, Shurvell HF (1993) Differentiation of solvated spironolactone samples by FT-Raman and FT-IR diffuse reflectance spectroscopy. Fresenius J. Anal. Chem. 345; 727–732.Google Scholar
  19. Belu AM, Davies MC, Newton JM, Patel N (2000) TOF-SIMS characterization and imaging of controlled-release drug delivery systems. Anal. Chem. 72; 5625–5638.Google Scholar
  20. Bernal JL, Del Nozal MJ, Garcia Buj GA, Juárez JM (1992) Use of methyl and ethyl acetate as organic modifiers in reversed-phase high-performance liquid chromatography. J. Chromatogr. 607; 175–181.Google Scholar
  21. Berthod A, Jin HL, Beesly, T.E., Duncan, J.D. and Armstrong, D.W. (1990) Cyclodextrin stationary phases for liquid chromatographic separation of drug stereoisomers. J. Pharm. Biomed. Anal. 8; 123–130.Google Scholar
  22. Berzas JJ, Rodríguez J, Castañeda G (1997a) Simultaneous spectrophotometric determination of ethinylestrediol and levonorgestrel by partial least squares and principal component regression multivariate calibration. Anal. Chim. Acta. 340; 257–265.Google Scholar
  23. Berzas JJ, Rodríguez J, Castañeda G (1997b) Determination of ethinylestradiol and gestodene in pharmaceuticals by a partial least-squares and principal component regression multivariate calibration, Anal. Sci. 13; 1029–1032.Google Scholar
  24. Berzas JJ, Rodríguez J, Castañeda G (1997c) Simultaneous determination of ethinylestradiol and levonorgestrel in oral contraceptive by derivative spectrophotometry. Analyst. 122; 41–44.Google Scholar
  25. Berzas JJ, Rodríguez J, Castañeda G, Guzmán Bernardo FJ (1997d) Simultaneous determination of ethinylestradiol and gestodene in oral contraceptives by derivative spectro-photometry. Anal. Lett. 30; 2221–2233.Google Scholar
  26. Berzas JJ, Del Castillo B, Castañeda G, Pinilla MJ (1999a) Micellar electrokinetic capillary electrochromatography as an alternative method for the determination of ethinylestradiol and levo-norgestrel. Talanta. 50; 261–268.Google Scholar
  27. Berzas JJ, Rodríguez J, Castañeda G, Pinilla MJ (1999b) Determination of ethinylestradiol and gestodene in oral contraceptives by micellar electrokinetic chromatography. Chromatographia. 49; 65–70.Google Scholar
  28. Blom Y, Ek M, Martin JT, Stjernström NE (1993) Chiral analysis in the Related Substances test: a comparison of the methods for the determination of dextronorgestrel impurities in levonorgesterel. Pharmeuropa. 5; 381–385.Google Scholar
  29. Bousquet E, Santagati NA, Tirendi S (1997) Determination of chenodeoxycholic acid in pharmaceutical preparations of ursodeoxycholic acid by high performance liquid chromatography with coulometric electrochemical detection. J. Liquid. Chromatogr. Rel. Technol. 20; 757–770. Google Scholar
  30. Britz-McKibbin P, Ichihashi T, Tsubota K, Chen DDY, Terabe S (2003) Complementary on-line preconcentration strategies for steroids by capillary electrophoresis. J. Chromatogr. A. 1013; 65–76.Google Scholar
  31. Brombacher S, Owen SJ, Volmer DA (2003) Automated coupling of capillary LC with matrix-assisted laser desorption ionization mass spectrometry for the analysis of small molecules utilizing a reactive matrix. Anal. Bioanal. Chem. 376; 773–779.Google Scholar
  32. Buranaosot J, Ungboriboonpisal S, Sriphong L (2006) A stability-indicating LC method for medroxyprogesterone acetate in bulk drug and injection formulation. J. Pharm. Biomed. Anal. 40; 1068–1072.Google Scholar
  33. Buszewski B, Jezierskawitala M, Kowalska S (2003) Stationary phase with specific surface properties for the separation of estradiol diastereomers. J. Chromatogr. B. 792; 279–286.Google Scholar
  34. Cardoso CE, Martins ROR, Telles CAS, Aucelio RQ (2004) Sequential determination of hydrocortisone and epinephrine in pharmaceutical formulations via photochemically enhanced fluorescence. Microchim. Acta. 146; 79–84.Google Scholar
  35. Cauhan V, Conway B (2005) Optimisation of a selective liquid chromatography procedure for hydrocortisone acetate, hydrocortisone alcohol, and preservatives in a pharmaceutical emulsion. Chromatographia. 61; 555–559.Google Scholar
  36. Cavina G, Alimenti R, Gallinella B, Valvo L (1992) The identification of related substances in triamcinolone acetonide by means of high-performance liquid chromatography with diode-array detector and mass spectrometry. J. Pharm. Biomed. Anal. 9; 685–692.Google Scholar
  37. Cenderowska I, Buszewski B (1999) Determination of finasteride and related compounds by reversed-phase high-performance liquid chromatography. I. Choosing the mobile phase composition. J. Liquid. Chromatogr. Rel. Technol. 22; 2259–2270.Google Scholar
  38. Chang H-Y, Kuo C-H, Sun S-W (2003) Determination of ursodeoxycholic acid in pharmaceutical preparations by capillary electrophoresis with indirect UV detection. J. Pharm. Biomed. Anal. 32; 949–956.Google Scholar
  39. Chankvetadze B, Kartozia I, Breitkreutz J, Okamoto Y, Blaschke G (2001) Effect of organic solvent, electrolyte salt and a loading of cellulose tris(3,5-dichlorophenyl-carbamate) on silica gel on enantioseparation characteristics in capillary electrochromatography. Electrophoresis. 22; 3327–3334.Google Scholar
  40. Chankvetadze B, Kartozia I, Yamamoto C, Okamoto Y (2002a) Comparative enantioseparation of selected chiral drugs on four different polysaccharide-type chiral stationary phases using polar organic mobile phases. J. Pharm. Biomed. Anal. 27; 467–478.Google Scholar
  41. Chankvetadze L, Kartozia I, Yamamoto C, Chankvetadze B, Blaschke G, Okamoto J (2002b) Enantioseparations in capillary liquid chromatography and capillary electrochromatography using amylose tris(3,5-dimethyphenylcarbamate) in combination with aqueous organic mobile phase. J. Sep. Sci. 25; 653–660.Google Scholar
  42. Chen C, Carillo M, Haltiwanger RC, Bradley P (2005) Solid state characterisation of momethasone furoate anhydrous and monohydrate forms. J. Pharm. Sci. 94; 2496–2509.Google Scholar
  43. Chen H, Wang X-Y, Yang Z-D, Li Y-C (2004) Novel spironolactone-analogs as impurities in spironolactone. Steroids. 69; 647–652.Google Scholar
  44. Chen H, Wang Y-F, Yang Z-D, Li Y-C (2006) Isolation and identification of novel impurities in spironolactone, J. Pharm. Biomed. Anal. 40; 1263–1267.Google Scholar
  45. Cifuentes A, Bernal JL, Diez-Masa JC (1998) Use of detergents and high content of organic solvents for simultaneous quantitation of ionic and nonionic drugs by electrokinetic chromatography. J. Chromatogr. A 824; 99–108.Google Scholar
  46. Claussen S, Böse M, Dittgen M (2001) X-ray diffraction, DSC and thermogravimetry combined with infrared analysis of freeze-dried prednisolone hemisuccinate. Pharmazie. 56; 475–476.Google Scholar
  47. Collier A, Wang J, Diamond D, Dempsey E (2005) Microchip micellar electrokinetic chromatography coupled with electrochemical detection for analysis of synthetic oestrogen mimicking compounds. Anal. Chim. Acta. 550; 107–115.Google Scholar
  48. Conrow RE, Dillow GW, Bian L, Xue L, Papadopoulou O, Baker JK, Scott S (2002) Corticosteroid decomposition via a mixed anhydride. J. Org. Chem. 67; 6835–6836.Google Scholar
  49. Corti P, Dreassi E, Corbini G, Lonardi S, Gravina S (1990) Application of near infrared reflectance spectroscopy to pharmaceutical control. I. Preliminary investigation of the uniformity of tablets’ content. Analysis. 18; 112–116.Google Scholar
  50. Das Gupta V, Mathew M (1995) Effect of mobile phase pH on the separation of drugs using high-performance liquid chromatography. Drug Dev. Ind. Pharm. 21; 833–837.Google Scholar
  51. Datta K, Das SK (1993) Densitometric quantification of corticosteroid sodium phosphate salts in parenteral preparations or eye and ear drops after reversed-phase ion-pair TLC. J. Planar Chromatogr. 6; 204–207.Google Scholar
  52. De Beer TRM, Vergote GJ, Baeyens WRG, Remon JP, Vervaet C, Verpoort F (2004) Development and validation of a direct non-destructive method for medroxyprogesterone acetate in a pharmaceutical suspension using FT-Raman spectroscopy. Eur. J. Pharm. Sci. 23; 355–362.Google Scholar
  53. De Orsi D, Gagliardi L, Chimenti F, Tonell D (1995) LC determination of beclomethasone dipropionate and its degradation products in bulk drug and pharmaceutical formulations. Anal. Lett. 28; 1655–1663.Google Scholar
  54. Dean JR, Lowdon J (1993) Application of supercritical fluid extraction in the pharmeceutical industry: supercritical fluid extraction of megestrol acetate from a tablet matrix. Analyst. 118; 747–751.Google Scholar
  55. Deftereos NT, Calokerinos AC (1994) Flow-injection chemiluminometric determination of steroids, Anal. Chim. Acta 290; 190–200.Google Scholar
  56. Demir H, Cucu A, Sakaraya S (2006) Determination of finasteride in the tablet form by liquid chromatography and its analytical method validation. Anal. Chim. Acta. 557; 252–255.Google Scholar
  57. Deng H, Van Berkel GJ, Takano H, Gazda D, Porter MD (2000) Electrochemically modulated liquid chromatography coupled on-line with electrospray mass spectrometry. Anal. Chem. 72; 2641–2647.Google Scholar
  58. Deng Y, Huang M-Y (2004) Capillary electrophoretic separation and theoretical study of inclusion complexes of sulfobutyl ether |3-cyclodextrin with estrogens. Int. J. Quant. Chem. 100; 746–752.Google Scholar
  59. Di Pietra AM, Andrisano V, Gotti R, Cavrini V (1996) On-line post-column photochemical derivatisation in liquid chromatographic – diode-array detection analysis of binary steroid mixtures. J. Pharm. Biomed. Anal. 14; 1191–1999.Google Scholar
  60. Dinc E, Yücesoy C, Palabiyiki M, Üstündag Ö, Onur F (2003) Simultaneous spectrophotometric determination of cyproterone acetate and estradiol valerate in pharmaceutical preparations by ratio-spectra derivative and chemometric methods. J. Pharm. Biomed. Anal. 32; 539–547.Google Scholar
  61. Djordjevic NM, Fitzpatrick F, Houdiere F, Lerch G, Rozing G (2000) High temperature and temperature programming in capillary electrochromatography, J. Chromatogr. 887; 245–252.Google Scholar
  62. El-Saharty YS, Hassan NY, Metwally FH (2002) Simultaneous determination of terbinafine HCl and triamcinolone acetonide by UV derivative spectrophotometry and spectrodensitometry. J. Pharm. Biomed. Anal. 28; 569–580.Google Scholar
  63. Erk N (1999) Ratio-spectra zero-crossing derivative spectrophotometric determination of certain drugs in two-component mixtures. Anal. Lett. 32; 1371–1388.Google Scholar
  64. Euerby MR, Gilligan D, Johnson CM, Roulin SCP, Myers P, Bartle KD (1997) Applications of capillary electrochromatography in pharmaceutical analysis. J. Microcol. Sep. 9; 373–387.Google Scholar
  65. Euerby MR, Graham JA, Johnson CM, Lewis RJ, Wallace DB (1996) The S-oxidative degradation of a novel corticosteroid tipredane (INN). Part III. Detailed investigations into the disuphoxidation of tipredane. J. Pharm. Biomed. Anal. 15; 299–313.Google Scholar
  66. Ferenczi-Fodor K, Végh Z, Pap-Sziklay Zs (1993) Validation of the quantitative planar chromatographic analysis of drug substances. 1. Definitions and practice in TLC. J. Planar Chromatogr. 6; 198–203.Google Scholar
  67. Ferenczi-Fodor K, Nagy-Turák A, Végh Z (1995) Validation and monitoring of quantitative thin-layer chromatographic purity test for bulk drug substances. J. Planar Chromatogr. 8; 349–356.Google Scholar
  68. Ferenczi-Fodor K, Mahó S, Pap-Sziklay S, Török I, Borka L (1997) Purity testing of levonorgestrel/norgestrel bulk drug substances by personal OPLC. Pharmeuropa. 9; 736–742.Google Scholar
  69. Ferenczi-Fodor K, Laukó A, Wiszkidenszky A, Végh Z, Újszászy K (1999) Chromatographic and spectroscopic investigation of “irreversible adsorption” in the course of multiple development in conventional TLC and HPTLC and OPLC. J. Planar Chromatogr. 12; 30–37.Google Scholar
  70. Ferenczi-Fodor K, Végh Z, Renger B (2006) Thin-layer chromatography in purity testing of pharmaceuticals. Trends Anal. Chem. 25; 778–789.Google Scholar
  71. Fialkov AB, Gordin A, Amirav A (2003) Extending the range of compounds amenable for gas chromatography–mass spectrometric analysis. J. Chromatogr. A 991; 217–240.Google Scholar
  72. Flood KG, Reynolds ER, Snow NH (2001) Determination of apparent association constants of steroid – cyclodextrin inclusion complexes using a modified Hummel-Dreyder method. J Chromatogr A 913; 261–268.Google Scholar
  73. Fountain W, Dumstorf K, Lowell A, Lodder RA, Mumper RJ (2003) Near-infrared spectroscopy for the determination of testosterone in thin-film composites. J. Pharm. Biomed. Anal. 33; 181–189.Google Scholar
  74. Gabel-Jensen C, Hansen SH, Pedersen-Bjergaard S (2001) Separation of neutral compounds by microemulsion electrokinetic chromatography: fundamental studies on selectivity. Electrophoresis. 22; 330–1336.Google Scholar
  75. Gad Kariem EA, Abounassif MA, Hagga ME, Al-Khamees HA (2000) Photodegradation study and stability-indicating assay of danazol using high-performance liquid chromatography. J. Pharm. Biomed. Ana. 23; 413–420.Google Scholar
  76. Gagliardi L, de Orsi D, del Giudice MR, Gatta F, Porra R, Chimenti P, Tonelli D (2002) Development of a tandem thin-layer chromatography–high performance liquid chromatography for the identification and determination of corticosteroids in cosmetic products. Anal. Chim. Acta. 457; 187–198.Google Scholar
  77. Galmier MJ, Beyssac E, Petit J, Aiache JM, Lartigue C (1999) Validation of a reversed-phase liquid chromatographic method for the determination of hydrocortisone phosphate disodium in a gel formulation. J. Pharm. Biomed. Anal. 20; 405–409.Google Scholar
  78. Gamiz-Gracia L, Jimenez-Carmona MM, Luque de Castro MD (2000) Determination of vitamins D 2 and D 3 in pharmaceuticals by supercritical fluid extraction and LC determination by UV detection. Chromatographia. 51; 428–432.Google Scholar
  79. Gau YS, Sun SW, Chen RR-L (1995) Optimization of high-performance liquid-chromatographic separation of progestogenic, oestrogenic, and androgenic steroids using factorial design. J. Liquid. Chromatogr. 18; 2373–2382.Google Scholar
  80. Gazdag M, Szepesi G, Mihályfi K (1988) Some aspects of the selection of high-performance liquid chromatographic methods for the separation of chiral compounds in pharmaceutical analysis. J. Chromatogr. 450; 145–155.Google Scholar
  81. Gazdag M, Babják M, Kemenes-Bakos P, Görög S (1991) Analysis of steroids. Part 41. Ion-pair high-performance liquid chromatographic separation of quaternary ammonium steroids on silica. J. Chromatogr. 550; 639–644.Google Scholar
  82. Gazdag M, Babják M, Brlik J, Mahó S, Tuba Z, Görög S (1998) Analysis of steroids. Part 53. Impurities and degradation products of mazipredone. J. Pharm Biomed. Anal. 17; 1029–1036.Google Scholar
  83. Gergely A (1994) Application of circular dichroism spectroscopy to the determination of steroids. In Analytical Applications of Circular Dichroism (eds Purdie N, Brittain HG). Elsevier, Amsterdam, pp. 293–305.Google Scholar
  84. Ghoneim MM, Baumann W, Hammam E, Tawfik A (2004) Voltammetric behavior and assay of the contraceptive drug levonorgestrel in bulk, tablets, and human serum at a mercury electrode. Talanta 64; 857–864.Google Scholar
  85. Glaser T, Albert K (2002) Unequivocal structural assignment of steroids in galenic emulsions empolying LC-NMR coupling. J. Sep. Sci. 25; 393–398.Google Scholar
  86. Goicoechea HC, Collado MS, Satuf ML, Olivieri AC (2002) Complementary use of partial least-squares and artificial neural networks for the non-linear spectrophotometric analysis of pharmaceutical samples. Anal. Bioanal. Chem. 374; 460–465.Google Scholar
  87. Gonzalo-Lumbreras R, Santos-Montes A, Garcia-Moreno E, Izquierdo-Hornillos R (1997) High-performance liquid chromatographic separation of corticoid alcohols and their derivatives: a hydrolysis study including application to pharmaceuticals. J. Chromatogr. Sci. 35; 439–445.Google Scholar
  88. Gonzalo-Lumbreras R, Izquierdo-Hornillos R (2000) High-performance liquid chromatographic optimisation study for the separation of natural and synthetic anabolic steroids. Application to urine and pharmaceutical samples. J. Chromatogr. B. 742; 1–11.Google Scholar
  89. Görög S, Szász Gy (1978 ) Analysis of Steroid Hormone Drugs. Elsevier, Amsterdam.Google Scholar
  90. Görög S (1983) Quantitative Analysis of Steroids. Elsevier, Amsterdam.Google Scholar
  91. Görög S (ed) (1989) Steroid Analysis in the Pharmaceutical Industry. Ellis Horwood, Chichester, UK.Google Scholar
  92. Görög S (1995) Ultraviolet-Visible Spectrophotometry in Pharmaceutical Analysis. CRC, Boca Raton, FL, pp. 323–334.Google Scholar
  93. Görög S (2000) Steroids. In Identification and Determination of Impurities in Drugs (ed Görög S). Elsevier, Amsterdam, pp. 712–731.Google Scholar
  94. Görög S (2003a) Estimation of impurity profiles in drugs and related materials, Part 23. Chemical and analytical characterization of related organic impurities in drugs. Anal. Bioanal. Chem. 377; 852–862.Google Scholar
  95. Görög S (2003b) Estimation of impurity profiles of drugs and related materials. Part 22. New safe medicines faster: the role of analytical chemistry. Trends Anal. Chem. 22; 407–415.Google Scholar
  96. Görög S (2004) Analysis of steroids. Part 56. Recent advances in the analysis of steroid hormones. Anal. Sci. 20; 767–782.Google Scholar
  97. Görög S (2005) The sacred cow: the questionable role of assay methods in characterising the quality of bulk pharmaceuticals. J. Pharm. Biomed. Anal. 36; 931–937.Google Scholar
  98. Görög S (2008) Drug safety, drug quality, drug analysis. J. Pharm. Biomed. Anal. 14; 247–253.Google Scholar
  99. Görög S, Balogh G, Gazdag M (1991) Analysis of steroids. Part 43 Combined application of high-performance liquid chromatography and NMR spectroscopy in the impurity profiling of drugs. J. Pharm. Biomed. Anal. 9; 829–833.Google Scholar
  100. Görög S, Gazdag M, Kemenes-Bakos P (1996) Analysis of steroids. Part 50. Derivatisation of ketosteroids for their separation and determination by capillary electrophoresis. J. Pharm. Biomed. Anal. 14 ; 1115–1124.Google Scholar
  101. Görög S, Balogh G, Csehi A, Csizér É, Gazdag M, Halmos Zs, Hegedüs B, Herényi B, Horváth P, Laukó A (1993) Estimation of impurity profiles of drugs and related materials. Part 11.The role of chromatographic and spectroscopic methods in the estimation of side-reactions in drug syntheses. J. Pharm. Biomed. Anal. 11; 1219–1226.Google Scholar
  102. Görög S, Brlik J, Csehi A, Halmos Zs, Herényi B, Horváth P, Dravecz F, Bor D (1995a) Analysis of steroids. Part 47. Identification of impurities in estradiol. Anal. Meth. Instrum. 2; 154–157.Google Scholar
  103. Görög S, Bihari M, Csizér É, Dravecz F, Gazdag M, Herényi B (1995b) Analysis of steroids. Part 49. The role of LC/diode-array UV spectroscopy in the identification of minor components (impurities, degradation products, metabolites) in various matrices. J. Pharm. Biomed. Anal. 14; 85–92.Google Scholar
  104. Görög S, Babják M, Balogh G, Brlik J, Csehi A, Dravecz F, Gazdag M, Horváth P, Laukó A, Varga K (1997) Analysis of steroids. Part 52. Dug impurity profiling strategies. Talanta. 44; 1517–1526.Google Scholar
  105. Görög S, Babják M, Balogh G, Brlik J, Dravecz F, Gazdag M, Horváth P, Laukó A, Varga K (1998) Analysis of steroids. Part 54. Theme with variations. Identification of impurities in 3-oxosteroids. J. Pharm. Biomed. Anal. 18; 511–525.Google Scholar
  106. Gupta A, Myrdal PB (2004) On-line high performance liquid chromatography method for analyte quantitation from pressurized metered dose inhalers. J. Chtvmatogr. A. 1033; 101–106.Google Scholar
  107. Gupta M, Bhargava H (2006) Development and validation of a high performance liquid chromatographic method for the analysis of budesonide. J. Pharm. Biomed. Anal. 40; 423–428.Google Scholar
  108. Hájková R, Solich P, Dvorák J, Sicha J (2003) Simultaneous determination of methylparaben, propylparaben, hydrocortisone acetate and its degradation products in a topical cream by RP-LC. J. Pharm. Biomed. Anal. 32; 921–927.Google Scholar
  109. Hansen SH, Gabel-Jensen C, Pedersen-Bjergaard S (2001) Comparison of microemulsion electrokinetic chromatography and solvent-modified micellar electrokinetic chromatography. J. Sep. Sci. 24; 643–650.Google Scholar
  110. Harris RK (2004) NMR crystallography. The use of chemical shifts. Solid State Sci. 6; 1025–1037.Google Scholar
  111. Hashem H, Jira Th (2005) Chromatographic applications on monolithic columns: determination of triamcinolone, prednisolone and dexamethasone in pharmaceutical tablet formulations using a solid-phase extraction and monolithic column. Chromatographia. 61; 133–136.Google Scholar
  112. Hauck HE, Junker-Buchheit A, Wenig R (1995) Reproducibility of silica gel 60 precoated plates in TLC and HPTLC. LC-GC Int. 8; 34–38.Google Scholar
  113. Hauck HE, Bund O, Fischer W, Schulz M (2001) Ultra-thin layer chromatography (UTLC) – a new dimension in thin-layer chromatography. J. Planar Chromatogr. 14; 234–236.Google Scholar
  114. Hooijerink D, Schilt R, van Bennekom E, Brouwer B (1994) Determination of anabolic esters in oily formulations and plasma in husbandry using high-performance liquid-chromatography and gas chromatography -mass selective detection. Analyst. 119; 2617–2622.Google Scholar
  115. Horváth P, Balogh G, Brlik J, Csehi A, Dravecz F, Halmos Zs, Laukó A, Rényei M, Varga K, Görög S (1997) Analysis of steroids Pairt 51. Identification of the side-products of the ethinylation step in the synthesis of contraceptive gestogens. J. Pharm. Biomed. Anal. 15; 1343–1349.Google Scholar
  116. Hou S, Hindle M, Byron PR (2001) A stability-indicating LC method for budesonide. J. Pharm. Biomed. Anal. 24; 371–380.Google Scholar
  117. Hou S, Hindle M, Byron PR (2005) Chromatographic and mass spectral characterisation of budesonide and a series of structurally related corticosteroids. J. Pharm. Biomed. Anal. 39; 196–205.Google Scholar
  118. Hsu R, Au AM (2001) Gas chromatography – chemical ionization mass spectrometry for drug screen analyses. Bull. Environ. Contam. Toxicol. 66; 178–183.Google Scholar
  119. Iglesias Y, Fente C, Vazquez BI, Franco C, Cepeda A, Mayo S (2002) Application of luminol chemiluminescence reaction for the determination of nine corticosteroids. Anal. Chim. Acta. 468; 43–52.Google Scholar
  120. IMS Chemical Actives Monitor (2005) IMS Health Inc., Norwalk, CT.Google Scholar
  121. Indrayanto G, Aditama GL, Tanudjaja W, Widjaja S (1998) Simultaneous densitometric determination of betamethasone valerate and clotrimazole in cream, and its validation. J. Planar Chromatogr. 11; 201–204.Google Scholar
  122. Indrayanto G, Widjaja S, Sutiono S (1999) Simultaneous densitometric determination of betamethasone valerate and miconazole nitrate in cream, and its validation. J. Liquid. Chromatogr. Rel. Technol. 22; 143–152.Google Scholar
  123. Izquierdo-Hornillos R, Gonzalo-Lumbreras R (2003) Optimization of the separation of a complex mixture of natural and synthetic anabolic steroids by micellar liquid chromatography. J. Chromatogr. B. 798; 69–77.Google Scholar
  124. Jamshidi A (2004) A convenient and high-throughput HPTLC method for determination of progesterone in release-media of silicone-based controlled-release drug-delivery systems. J. Planar Chromatogr. 17; 229–232.Google Scholar
  125. Josephs JL, Sanders M (2004) Creation and comparison of MS/MS spectral libraries using quadrupole ion trap and triple-quadrupole mass spectrometrs. Rapid Comm. Mass Spectrom. 18; 743–759.Google Scholar
  126. Jung M, Schurig V (1993) Extending the scope of enantiomer separation by capillary supercritical fluid chromatography on immobilized polysiloxan-anchored permethyl-|3-cyclodextrin (Chiralsil-Dex). J. High Res. Chromatogr. 16; 215–223.Google Scholar
  127. Kaehlig H, Valenta C, Dampfhart U, Auner U (2005) Rheology and NMR self diffusion experiments as well as skin permeation of diclofenac-sodium and cyproterone acetate of new gel preparations. J. Pharm. Sci. 94; 288–296.Google Scholar
  128. Kagan MZ (2001) Normal-phase high-performance liquid chromatographic separations using ethoxynonafluoroborate as hexane alternative I. Analytical a chiral applications. J. Chromatogr. 918; 293–302.Google Scholar
  129. Kanazawa H, Yamamoto K, Matsushima Y, Takai N, Kikuchi A, Sakurai Y, Okano T (1996) Temperature-responsive chromatography using poly(N-isopropylacrylamide)-modified silica. Anal. Chem. 68; 100–105.Google Scholar
  130. Kanazawa H, Sunamoto T, Ayano E, Matsushima Y, Kikuchi A, Okano T (2002) Temperature-response chromatography using poly(N-isopropylacrylamide) hydrogel modified silica. Anal. Sci. 18; 45–18.Google Scholar
  131. Kassai A, Szécsi A, Koppány A, Végh Z, Ferenczi-Fodor K (2000) Analytical transfer of an OPLC purity test and its application in in-process monitoring. J. Planar Chromatogr. 13; 30–32.Google Scholar
  132. Katona Z, Vincze L, Végh Z, Trompler Á, Ferenczi-Fodor K (2000) Cleaning vahdation procedure eased by overpressured layer chromatography. J. Pharm. Biomed. Anal. 22; 349–353.Google Scholar
  133. Kaukonen AM, Vuorela P, Vuorela H, Mannermaa J-P (1998) High-performance liquid chromatography method for the separation and quantitation of spironolactone and its degradation products in aqueous solution and its metabolites in rat serum. J. Chromatogr. A 797; 271–281.Google Scholar
  134. Kedor-Hackmann ERM, Gianotto EAS, Santoro MIRM (1997) Determination of triamcinolone acetonide in ointment by UV derivative spectrophotometry and high performance liquid chromatography. Anal. Lett. 30; 1861–1871.Google Scholar
  135. Kerns EH, Di L, Petusky S, Kleintop T, Huryn D, McConnel O, Carter G (2003) Pharmaceutical profiling method for lipophilicity and integrity using liquid chromatography–mass spectrometry. J. Chromatogr. B 791; 381–388.Google Scholar
  136. Khakpour M, Jamshidi A, Entezami AA, Mirzahed H (2005) HPTLC procedure for determination of levonorgestrel in drug-release media of an in-situ forming delivery system. J. Planar Chromatogr. 18; 326–329.Google Scholar
  137. Kotyiyan PN, Vavia PR (2000) Stability indicating HPTLC method for the estimation of estradiol. J. Pharm. Biomed. Anal. 22; 667–671.Google Scholar
  138. Koukli II, Calokerinos AC (1990) Continuous-flow chemiluminescence determination of some corticosteroids. Analyst. 115; 1553–1557.Google Scholar
  139. Krzek J, Hubicka U, Dabrowska-Tylka M, Leciejewicz-Ziemecka E (2002) Determination of budesonide R(+) and S(-) isomers in pharmaceuticals by thin-layer chromatography with UV densitometric defection. Chromatographia. 56; 759–762.Google Scholar
  140. Kummer M, Werner G (1998) Chiral resolution of enantiomeric steroids by high-performance liquid chromatography on amylose tris(3,5-dimethylphenycarbamate) under reversed-phase conditions. J. Chromatogr. A 825; 107–114.Google Scholar
  141. Kummer M, Palme H-J, Werner G (1996) Resolution of enantiomeric steroids by high-performance liquid chromatography on chiral stationary phases. J. Chromatogr. A 749; 61–68.Google Scholar
  142. Kuo C-Y, Wu S-M (2005) Micellar electrokinetic chromatography for simultaneous determination of six corticosteroids in commercial preparations. J. Sep. Sci. 28; 144–148.Google Scholar
  143. Laban A, Markovic S, Stankov M, Djurdjevic P (2004) Simultaneous determination of gestodene and ethinyl estradiol in contraceptive formulations by RP-LC. Anal. Lett. 37; 273–282.Google Scholar
  144. Lamparczyk H, Ochoczka RJ, Zarzycki P, ZieliÕski JP (1990) Separation of steroids by reversed-phase HPTLC using various binary mobile phases. J. Planar Chromatogr. 3; 34–37.Google Scholar
  145. Lamparczyk H, Zarzycki PK, Nowakowska J (1994) Effect of temperature on separation of norgestrel enantiomers by high-performance liquid chromatography. J. Chromatogr. A 668; 413417.Google Scholar
  146. Lane SJ (2000) CEC/MS. In Identification and Determination of Impurities in Drugs (ed Görög S). Elsevier, Amsterdam, pp. 359–381.Google Scholar
  147. Lane SJ, Boughtflower R, Paterson C, Underwood T (1995) Capillary electrochromatography/ mass spectrometry: principles and potential for application in the pharmaceutical industry. Rapid Comm. Mass Spectrom. 9; 1283–1287.Google Scholar
  148. Laukó A, Csizér É, Görög S (1993) Analysis of Steroids. Part 46. Qualitative and quantitative characterization of bulk cholesterol by gas chromatography and gas chromatography–mass spectrometry. Analyst 118; 609–611.Google Scholar
  149. Lemus Gallego JM, Pérez Arroyo J (2001a) Spectrophotometric resolution of ternary mixtures of dexamethasone, polymyxin B and trimethoprim in synthetic and pharmaceutical formulations. Anal. Chim. Acta 437; 247–257.Google Scholar
  150. Lemus Gallego JM, Pérez Arroyo J (2001b) Micellar electrokinetic capillary chromatography as an alternative method for the determination of dexamethasone, trimethoprim, and polymyxin B. Fresenius J. Anal. Chem. 370; 973–795.Google Scholar
  151. Lemus Gallego JM, Pérez Arroyo J (2002a) Spectrophotometric determination of hydro-cortisone, nystatin and oxytetracycline in synthetic and pharmaceutical preparations based on various univariate and multivariate methods. Anal. Chim. Acta 460; 85–97.Google Scholar
  152. Lemus Gallego JM, Pérez Arroyo J (2002b) Determination of hydrocortisone 21-hemisuccinate, oxytetracycline and nystatin in pharmaceutical preparations by capillary zone electrophoresis. Anal. Lett. 35; 2105–2118.Google Scholar
  153. Lemus Gallego JM, Pérez Arroyo J (2003a) Simultaneous determination of hydrocortisone and Zn-bacitracin by spectrophotometric derivative and multivariate methods. Microchim. Acta. 141; 133–141.Google Scholar
  154. Lemus Gallego JM, Pérez Arroyo J (2003b) Determination of hydrocortisone and associated compounds in pharmaceutical preparations by micellar electrokinetic chromatography. J. Liquid. Chromatogr. Rel. Technol. 26; 1011–1025.Google Scholar
  155. Lemus Gallego JM, Pérez Arroyo J (2003c) Optimized method for the determination of prednisolone, Zn-bacitracin and phenylephrine in local pharmaceutical preparations by micellar electrokinetic capillary chromatography. Chromatographia. 58; 277–281.Google Scholar
  156. Lemus Gallego JM, Pérez Arroyo J (2003d) Determination of prednisolone acetate, sulfac-etamide and phenylefrine in local pharmaceutical preparations by micellar electrokinetic chromatography. J. Pharm. Biomed. Anal. 31; 873–884.Google Scholar
  157. Li J (2001) Prediction of internal standards in reversed-phase liquid chromatography: I. Initial study on predicting internal standards for use with neutral samples based on linear solvation energy relationships. J. Chromatogr. A 927; 19–30.Google Scholar
  158. Li J (2002) Elimination of polymer interference in chromatographic analysis of estradiol degradation products in a transdermal drug delivery formulation by proper selection of extraction solvents. J. Pharm. Sci. 91; 1873–1879.Google Scholar
  159. Li J, Shah DS (2002) Prediction of internal standards in reversed-phase liquid chromatography: II. Selectivity optimation and internal standard prediction for the quantitation of estradiol and levonorgestrel in a transdermal drug delivery formulation based on the linear solvation energy relationships. J. Chromatogr. A 954; 159–171.Google Scholar
  160. Lim JK, Riley MC, Watts ST (2003) The Hitachi LaChrom Elite LC and fast LC pharmaceutical applications: OTC analgesics and steroids. LC-GC N Am. 21; 47–48.Google Scholar
  161. Lin M, Wu N (1999) Comparison between micellar electrokinetic chromatography and LC for the determination of betamethasone dipropionate, clotrimazole and their related substances. J. Pharm. Biomed. Anal. 19; 945–954.Google Scholar
  162. Linares MS, Fraga JMG, Jimenez AI, Jimenez F, Arias JJ (1999) Influence of the selected wavelength range on the simultaneous spectrophotometric determination of mixture components by use of partial least square regression. Anal. Lett. 32; 2489–2505.Google Scholar
  163. Lindholm J, Johansson M, Forstedt T (2003a) Guidelines for analytical method development and validation of biotechnological production of drugs. Production of hydroxyprogesterone as model. J. Chromatogr. B 791; 323–336.Google Scholar
  164. Lindholm J, Westerlund D, Karlsson K-E, Caldwell K, Forstedt T (2003b) Use of liquid chromatography–diode-array detection and mass spectrometry for rapid product identification in biotechnological synthesis of hydroxyprogesterone. J. Chromatogr. A 992; 85–100.Google Scholar
  165. Liu X-Y, Nakamura C Yang Q, Kamo N, Miyake J (2002) Immobilized liposome chromatography to study drug-membrane interactions: correlation with drug absorption in humans. J. Chromatogr. A 961; 113–118.Google Scholar
  166. Liu Y, Pietrzyk DJ (2001) Capillary electrophoretic separations with copolymeric reversed-stationary phase and ion-exchanger-packed columns. J. Chromatogr. A 920; 367–375.Google Scholar
  167. Liu Y, Berthod A, Mitchell CR, Xiao TL, Zhang B, Armstrong DW (2002) Super/subcritical fluid chromatography chiral separations with macrocyclic glycopeptide stationary phases. J. Chromatogr. A 978; 185–204.Google Scholar
  168. Lommen A, Schilt R, Weseman J, Roos AH, van Velde JW, Nielen MWF (2002) Application of 1D 1 H NMR for fast non-targeted screening and compositional analysis of steroid coctails and veterinary drug formulations administered to livestock. J. Pharm. Biomed. Anal. 28; 87–96.Google Scholar
  169. Loran JS, Cromie KD (1990) An evaluation of the use of supercritical fluid chromatography with light scattering detection for the analysis of steroids. J. Pharm. Biomed. Anal. 8; 607–611.Google Scholar
  170. Lubda D, Cabrera K, Nakanishi K, Lindner W (2003) Monolithic silica columns with chemically bonded |3-cyclodextrin as a stationary phase for enantiomer separations of chiral pharmaceuticals. Anal. Bioanal. Chem. 377; 892–901.Google Scholar
  171. Lucangioli SE, Rodríguez VG, Fernandez Otero GC, Vizioli NM, Carducci CN (1997) Development and validation of capillary electrophoresis methods for pharmaceutical dissolution assays. J. Capill. Electrophor. 4; 27–31.Google Scholar
  172. Lucangioli SE, Carducci CN, Scioscia SL, Carlucci A, Bregni C, Kenndler E (2003) Comparison of the retention characteristics of different pseudostationary phases for microemulsion and micellar electrokinetic chromatography of betamethasone and derivatives. Electrophoresis. 24; 984–991.Google Scholar
  173. Luis ML, Garcia JM, Jimenez AI, Jimenez F, Arias JJ (1999), Simultaneous determination of chlorthalidone and spironolactone with univariate and multivariate calibration wavelength range selection. JAOAC Int. 82; 1054–1063.Google Scholar
  174. Lynen F, Buica A, de Villiers A, Crouch A, Sandra P (2005) An efficient slurry packing procedure for the preparation of columns applicable in capillary electrochromatography and capillary electrochromatography-mass spectrometry. J. Sep. Sci. 28; 1539–1549.Google Scholar
  175. Martín E, Hernández O, Arias JJ, Jiménez AI (1997) Simultaneous determination of hydrochlorothiazide and spironolactone in pharmaceutical preparations using batch and dynamic systems. Microchem. J. 56; 207–215.Google Scholar
  176. Matysik G, Toczolowski J, Matysik A (1995) Stepwise gradient thin-layer chromatography and densitometry of prednisolone acetate. Chromatographia. 40; 737–739.Google Scholar
  177. Matyska M, Siouffi A-M, Soczewinski E (1991) Programmed multiple development (PMD) analysis of steroids by planar chromatography with a new modification of the horizontal sandwich chamber. J. Planar Chromatogr. 4; 255–257.Google Scholar
  178. Matysová L, Hájková R, Sicha J, Solich P (2003) Determination of methylparaben, pro-pylparaben, triamcinolone acetonide and its degradation product in a topical cream by RP-LC. Anal. Bioanal. Chem. 376; 440–443.Google Scholar
  179. Mazurek S, Sztosak R (2006) Quantitative determination of captopril and prednisolone in tablets by FT-Raman spectroscopy. J. Pharm. Biomed. Anal. 40; 1225–1230.Google Scholar
  180. Meyyanathan SN, Ramasarma GVS, Suresh B (2001) Analysis of finasteride in pharmaceutical preparations by high performance thin layer chromatography. J. Planar Chromatogr. 14; 188–190.Google Scholar
  181. Millership JS, Parker C, Donelly D (2005) Ratio spectra derivative spectrophotometry for the determination of furosemide and spironolactone in a capsule formulation. Farmaco. 60; 333–338.Google Scholar
  182. Mistry N, Ismail IM, Smith MG, Nicholson JK, Lindon JC (1997) Characterisation of impurities in bulk drug batches of fluticasone propionate using directly coupled LC-NMR spectroscopy and LC-MS. J. Pharm. Biomed. Anal. 16; 697–705.Google Scholar
  183. Mizuguchi T, Ogasawara C, Shimada K (2005) Application of monolithic silica column for LC separation of estrogens. Chromatography. 26; 101–104.Google Scholar
  184. Molero-Monfort M, Escuder-Gilabert L, Villanueva-Camafias RM, Sagrado S, Medina-Hernández MJ (2001) Biopartitioning micellar chromatography: an in vitro technique for predicting human drug absorption. J. Chromatogr. B 753; 225–236.Google Scholar
  185. Monton MRN, Otsuka K, Terabe S (2003) On-line sample preconcentration in micellar electrokinetic chromatography by sweeping with anionic–zwitterionic mixed micelles. J. Chromatogr. A 985; 435–445.Google Scholar
  186. Morris V, Hughes J, Marriott P (2003) Spherical coordinate representations of solvent composition for liquid chromatography method development using experimental design. J. Chromatogr. A. 1008; 43–56.Google Scholar
  187. Mulholland M, Whelan TJ, Rose H, Keegan J (2000) Direct identification and quantitation of prednisone in the presence of overlapping hydrocortisone by liquid chromatography with electrospry and atmospheric-pressure chemical-ionisation mass spectrometry. J. Chromatogr. A. 870; 135–141.Google Scholar
  188. Murnane D, Martin GP, Marriott C (2006) Validation of a reverse-phase high performance liquid chromatographic method for concurrent assay of a weak base (salmeterol xinafoate) and a pharmacologically actice steroid (fluticasone propionate). J. Pharm. Biomed. Anal. 40; 1149–1154.Google Scholar
  189. Nepote AJ, Damiani PC, Olivieri AC (2003) Chemometrics assisted spectroscopic determination of vitamin B6 vitamin B12 and dexamethasone in injectables. J. Pharm. Biomed. Anal. 31; 621–627.Google Scholar
  190. Neville GA, Beckstead HD, Cooney JD (1994) Thermal analyses (TGA and DSC) of some spironolactone solvates. Fresenius J. Anal. Chem. 349; 746–749.Google Scholar
  191. Neville GA, Beckstead HD, Shurvell HF (1992) Utility of Fourier-transform – Raman and Fourier transform infrared diffuse reflectance spectroscopy for differentiation of polymorphic spironolactone samples. J. Pharm. Sci. 81; 1141–1146.Google Scholar
  192. Nielen MWF, Vissers JPC, Fuchs REM, van Velde JW, Lommen A (2001) Screening for anabolic steroids and related compounds in illegal coctails by LC/time-of-flight mass spectrometry and LC/quadrupole time-of-flight tandem MS with accurate mass measurement. Rapid Commun. Mass Spectrom. 15; 1577–1585.Google Scholar
  193. Nishi H, Fukuyama T, Matsuo M, Terabe S (1990) Separation and determination of lipophilic corticosteroids and benzothiazepin analogues by micellar electrokinetic chromatography using bile salts. J. Chromatogr. 513; 279–295.Google Scholar
  194. Noé S, Böhler J, Keller E, Frahm AW (1998) Evaluation and optimisation of separation buffers for the determination of corticosteroids with micellar electrokinetic capillary chromatography (MECC). J. Pharm. Biomed. Anal. 18; 911–918.Google Scholar
  195. Novakova L, Matysova L, Solich P (2006) Advantages of application of UPLC in pharmaceutical analysis. Talanta. 68; 908–918.Google Scholar
  196. Novakovic J, Vastová M (1990) Quantitative HPTLC determination of cyproterone acetate and ethinyl estradiol in pharmaceuticals. J. Planar Chromatogr. 3; 407–409.Google Scholar
  197. Novakovic J, Agbaba D, Vladimirov S, Zivanov-Stakic D (1990) Densitometric determination of conjugated oestrogens in raw material and pharmaceutical preparations. J. Pharm. Biomed. Anal. 8; 253–257.Google Scholar
  198. Novakovic J, Tvrzicka E, Pisarikova A (1991) Simultaneous capillary gas chromatographic determination of cyproterone acetate and ethinylestradiol in pharmaceuticals. Anal. Lett. 24; 1559–1569.Google Scholar
  199. Nygaard L, Drohse Kilde H, Andersen SG, Henriksen L, Overby V (2004) Development and validation of a reversed-phase liquid chromatographic method for analysis of degradation products of estradiol in Vagifem tablets. J. Pharm. Biomed. Anal. 34; 265–276.Google Scholar
  200. Ogata M, Noro Y, Yamada M, Tahara T, Nishimura T (1998) Photodegradation products of methylprednisolone suleptanate in aqueous solution: evidence of bicyclo[3.1.0]hex-3-en-2-one intermediate. J. Pharm. Sci. 87; 91–95.Google Scholar
  201. Okamoto H, Uetake A, Tamaya R, Nakajima T, Sagara K, Ito Y (2001) Simultaneous determination of ingredients in an ointment by hydrophobic interaction electrokinetic chromatography. J. Chromatogr. A 929; 133–141.Google Scholar
  202. Pavic K, Čudina O, Agbaba D, Vladimirov S (2003) Quantitative analysis of cyproterone acetate and ethinyl estradiol in tablets by use of planar chromatography. J. Planar Chromatogr. 16; 45–47.Google Scholar
  203. Pedersen-Bjergaard S, Gabel-Jensen C, Hansen SH (2000) Selectivity in microemulsion electrokinetic chromatography. J. Chromatogr. A 897; 375–381.Google Scholar
  204. Pharm. Eur. 5 (2004) (European Pharmacopoeia 5, 2004). Council of Europe, Strasbourg.Google Scholar
  205. Pharm. Jpn. 14 (2001) (The Japanese Pharmacopoeia 14th Edition, 2001). Society of Japanese Pharmacopoeia, Tokyo.Google Scholar
  206. Piel G, Moutard S, Perly B, de Hassonville SH, Bertholet P, Barillaro V, Piette M, Delatter L, Evrard B (2004) Comparison of two methods currently used to determine the interaction between cyclodextrins and drugs: phase solubility diagrams and NMR spectroscopy. J. Drug Deliv. Sci. Technol. 14; 87–91.Google Scholar
  207. Pomponio R, Gotti R, Fiori J, Cavrini V (2005) Microemulsion electrokinetic chromatography of corticosteroids. Effect of surfactants and cyclodextrins on the separation selectivity. J. Chromatogr. 1081; 24–30.Google Scholar
  208. Poole SK, Patel S, Dehring K, Workman H, Dong J (2003) Estimation of octanol–water partition coefficients for neutral and weakly acidic compounds by microemulsion electrokinetic chromatography using dynamically coated capillary columns. J. Chromatogr. 793; 265–274.Google Scholar
  209. Rajevic M, Betto P (1998) Assay of ursodeoxycholic acid and related impurities in pharmaceutical preparations by LC with evaporative light scattering detector. J. Liquid Chromatogr. Rel. Technol. 21; 2821–2830.Google Scholar
  210. Reepmeyer JC (2001) Screening for corticosteroids in topical pharmaceuticals by LC with a scanning ultraviolet detector. J. Liquid. Chromatogr. Rel. Technol. 24; 693.Google Scholar
  211. Reepmeyer JC, Brower JF, Ye H (2005) Separation and detection of the isomeric equine conjugated estrogens, equilin sulfate and A8,9-dehydroestrone sulfate, by liquid chromatography–electrospray–mass spectrometry using carbon-coated zirconia and porous graphitic carbon stationary phases. J. Chromatogr. A. 1083; 42–51.Google Scholar
  212. Rege PR, Vilivalam VD, Collins CC (1998) Development in release testing of topical dosage forms: use of the Enhancer Cell with automated sampling. J. Pharm. Biomed. Anal. 17; 1225–1233.Google Scholar
  213. Romanyshyn LA, Tiller PR (2001) Ultra-short columns and ballistic gradients: considerations for ultra-fast chromatographic–tandem mass spectrometric analysis. J. Chromatogr. A., 928; 41–51.Google Scholar
  214. Rose U, Fuchs J (1998) Validation of the value for specific absorbance in monographs of the European Pharmacopoeia. Pharmeuropa. 10; 146–148.Google Scholar
  215. Ruiz-Angel MJ, Caballero RD, Simó-Alfonso EF, Garcia-Alvarez-Coque MC (2002) Micellar liquid chromatography: suitable technique for screening analysis. J. Chromatogr. 947; 31–45.Google Scholar
  216. Russel JA, Malcolm RK, Campbell K, Woolfson AD (2000) High-performance liquid chromatographic determination of 17|3-estradiol and 17|3-estradiol-3-acetate solubilities and diffusion coefficients in silicone elastomeric vaginal rings. J. Chromatogr. B 744; 157–163.Google Scholar
  217. Ryan JA, Compton SV, Brooks MA, Compton DAC (1991) Rapid verification of identity and content od drug formulations using mid-infrared spectroscopy. J. Pharm. Biomed. Anal. 9; 303–310.Google Scholar
  218. Saevels J, Wuyts M, Van Schepdael A, Roets E, Hoogmartens J (1999) In-house packing and testing of capillaries for capillary electrochromatography using simple equipment. J. Pharm. Biomed. Anal. 20; 513–520.Google Scholar
  219. Saindon PJ, Cauchon NS, Sutton PA, Chang C-J, Peck GE, Byrn SR (1993) Solid-state nuclear magnetic resonance (NMR) spectra of pharmaceutical dosage forms. Pharm. Res. 10; 197–203.Google Scholar
  220. Salem AA, Barsoum BN, El Said DM (2005) Rapid determination of triethiodide (Flaxedil) and pancuronium bromide (Pavulon) in pharmaceutical and urine matrices by means of modified-carbon-paste ion-selective electrodes. Helv Chim Acta 88; 861–872.Google Scholar
  221. Salole EG (1991) Thermal methods in the solid-state analysis of steroidal drugs. In Advances in Steroid Analysis ‘90 (ed Görög S). Akadémiai Kiadó, Budapest, pp. 473–478.Google Scholar
  222. Sarioglu K, Celebi SS, Mutlu M (2001) A rapid method for determination of vitamins D 2 and D 3 in pharmaceutical preparations by LC. J. Liq. Chromatogr. Rel. Technol. 24; 973–982.Google Scholar
  223. Satínský D, Huclová J, Solich P, Karlícek R (2003) Reversed-phase porous silica rods, as alternative approach to high-performance liquid chromatographic separation using the sequential injection chromatography technique. J. Chromatogr. A, 1015; 239–244.Google Scholar
  224. Segall A, Vitale M, Pérez V, Hormaechea F, Palacios M, Pizzorno MT (2000) A stability-indicating LC method to determine cyproterone acetate in tablet formulations. Drug Dev. Int. Pharm. 26; 867–872.Google Scholar
  225. Segmuller BE, Armstrong BL, Dunphy R, Oyer AR (2000) Identification of autioxidation and photodegradation products of ethinylestradiol by on-line LC-NMR and LC-MS. J. Pharm. Biomed. Anal. 23; 927–937.Google Scholar
  226. Shen H-J, Lin C-H (2006) Comparison of the use of anionic and cationic surfactants for the separation of steroids based on MEKC and sweeping-MEKC modes. Electrophoresis. 27; 1255–1262.Google Scholar
  227. Sherma J, Whitcomb BP, Brubaker K (1990) Determination of clioquinol, hydrocortisone, hydrocortisone acetate in cream and ointment preparations by HPTLC-densitometry. J. Planar Chromatogr. 3; 189–190.Google Scholar
  228. Skogsberg U, Händel H, Gesele E, Sokolliess T, Menyes U, Jira T, Roth U, Albert K (2003) Investigation of the retention behaviour of steroids with calixarene-based stationary phases by modern NMR spectroscopy. J. Sep. Sci. 26; 1119–1124.Google Scholar
  229. Smith NW, Evans MB (1994) The analysis of pharmaceutical compounds using electrochromatography. Chromatographia. 38; 649–657.Google Scholar
  230. Song YX, Wang JQ, Su ZX, Chen DY (2001) High-performance liquid chromatography on on silica modified with temperature-responsive polymers. Chromatographia. 54; 208–212.Google Scholar
  231. Souri E, Jalalizadeh H, Farsam H, Ghadiri R, Amanlou R (2005) Simultaneous determination of cyproterone acetate and ethinylestradiol in tablets by derivative spectrophotometry. Chem. Pharm. Bull. 53; 949–951.Google Scholar
  232. Spangler M, Mularz E (2001) A validated, stability-indicating method for the assay of dexamethasone in drug substance and drug product analyses, and the assay of preservatives in drug product. Chromatographia. 54; 329–334.Google Scholar
  233. Sudsakorn S, Kaplan L, Williams DA (2006) Simultaneous determination of triamcinolone acetonide and oxymetazoline hydrochloride in nasal spray formulation by LC. J. Pharm. Biomed. Anal. 40; 1273–1280.Google Scholar
  234. Szász Gy, Gyimesi-Forrás K, Budvári-Bárány Zs (1998) Optimized and validated LC methods for compendial quality assessment. III. Testing of optical purity applying a-acid-glycoprotein stationary phase. J. Liquid. Chromatogr. Rel. Technol. 21; 2535–2547.Google Scholar
  235. Szegvári D, Horváth P, Gergely A, Németh S, Görög S (2003) CD spectrometric methods for the simultaneous determination of ethisterone and its É5 isomer. Anal. Bioanal. Chem. 375; 713–717.Google Scholar
  236. Szentesi A, Gergely A, Horváth P, Szász Gy (2000) Determination of É3-ketosteroids based on oxime formation by difference circular dichroism spectroscopy. Fresenius J. Anal. Chem. 368; 384–388.Google Scholar
  237. Tárkányi G (2000) Estimation of enantiomeric impurities. NMR spectroscopy. In Identification and Determination of Impurities in Drugs (ed Görög S). Elsevier, Amsterdam, 562–574.Google Scholar
  238. Tárkányi G (2002) Quantitative approach for the screening of cyclodextrins by nuclear magnetic resonance spectroscopy in support of chiral separations in liquid chromatography and capillary electrophoresis. Enantioseparation of norgestrel with α-, β- and γ-cyclodextrins. J. Chromatogr. A 961; 257–276.Google Scholar
  239. Taylor RB, Vorarat S, Reid RG, Boyle SR, Moody RR (1999) Comparison of the separations of some neutral analytes by LC, MEKC and CEC. J. Capill. Electrophor. 6; 131–136.Google Scholar
  240. Teng XW, Cutler DC, Davies NM (2003) Degradation kinetics of mometasone furoate in aqueous systems. Int. J. Pharm. 259; 129–141.Google Scholar
  241. Terabe S, Ishihama Y, Nishi H, Fukuyama T, Otsuka K (1991) Effect of urea addition in Micellar electrokinetic chromatography. J. Chromatogr. 545; 359–368.Google Scholar
  242. Ting E-Y, Porter MD (1997) Separation of corticosteroids using electrochemically modulated liquid chromatography. Anal. Chem. 69; 675–678.Google Scholar
  243. Toral MI, Soto C, Richter R, Tapia AE (2002) Simultaneous determination of estradiol and medroxyprogesterone acetate in pharmaceutical formulations by second-derivative spectrophotometry. JAOAC Int. 85; 883–888.Google Scholar
  244. Torres-Cartas S, Villanueva-Camafias RM, Garcia-Alvarez-Coque MC (2000a) Retention-structure relationship studies for some steroidal hormones in micellar liquid chromatography. Chromatographia. 51; 577–585.Google Scholar
  245. Torres-Cartas S, Villanueva-Camafias RM, Garcia-Alvarez-Coque MC (2000b) Sensitized lanthanide fluorescence detection of steroidal hormones. J. Liquid. Chromatogr. Rel. Technol. 23; 1171–1186.Google Scholar
  246. Torres-Cartas S, Torres-Lapasio JR, Villanueva-Camafias RM, Garcia-Alvarez-Coque MC (2000c) Resolution of mixtures of steroidal hormones with micellar eluents of sodium dodecyl sulphate and acetonitrile or pentanol. Chromatographia. 52; 185–189.Google Scholar
  247. Urban PL, Garcia-Ruiz C, Garcia MA, Marina ML (2005) Separation and online preconcentration by multistep stacking with large-volume injection of anabolic steroids by capillary electrokinetic chromatography using charged cyclodextrines and UV-absorption detection. J. Sep. Sci. 28; 2200–2209.Google Scholar
  248. USP 29 (2006) (United States Pharmacopoeia 29, 2006 ), USP Convention Inc., Rockville, IN.Google Scholar
  249. Valkó K, Espinosa S, Du CM, Bosch E, Rosés M, Bevan C, Abraham MH (2001) Unique selectivity of perfluorinated stationary phases with 2,2,2-trifluoroethanol as organic mobile phase modifier. J. Chromatogr. A. 933; 73–81.Google Scholar
  250. Valvo L, Paris A, Savella AL, Gallinella B, Ciranni Signoretti E (1994) General high-performance liquid chromatography procedures for the rapid screening of natural and synthetic corticosteroids. J. Pharm. Biomed. Anal. 12; 805–810.Google Scholar
  251. Vannecke C, Nguyen Minh Nguyet A, Bloomfield MS, Staple AJ, Vander Heyden AJ, Massart DL (2000) Development and optimisation of a flow injection assay for fluticasone propionate using an asymmetrical design and the variable-size simplex algorithm. J. Pharm. Biomed. Anal. 23; 291–306.Google Scholar
  252. Varjo SJO, Hautala JT, Wiedmer SK Riekkola M-L (2005) Small diamines as modifiers for phosphatidylcholine/phosphatidylserine coatings in capillary electrochromatography. J. Chromatogr. A 1081; 92–98.Google Scholar
  253. Vindevogel J, Sandra P (1991) Resolution optimization in micellar electrokinetic chromatography: use of Plackett-Burman statistical design for the analysis of testosterone esters. Anal. Chem. 63; 1530–1536.Google Scholar
  254. Vomastová L, Miksik I, Deyl Z (1996) Microemulsion and micellar electrokinetic chromatography of steroids. J. Chromatogr. B 681; 107–113.Google Scholar
  255. Wang J, Schaufelberger DE, Guzman NA (1998) Rapid analysis of norgestimate and its potential degradation products by capillary electrochromatography. J. Chromatogr. Sci. 36; 155–160.Google Scholar
  256. Warriner RN, Craze AS, Games DE, Lane SJ (1998) Capillary electrochromatography/mass spectrometry – A comparison of the sensitivity of nanospray and microspray ionization techniques. Rapid Commun. Mass Spectrom. 12; 1143–1149.Google Scholar
  257. Wilson NS, Nelson MD, Dolan JW, Snyder LR, Wolcott RG, Carr PW (2002) Column selectivity in reversed-phase liquid chromatography I,II (A general quantitative relationship; Effect of change in conditions). J. Chromatogr. A 961; 171–193, 195–215.Google Scholar
  258. Wiszkidenszky A, Mahó S, Végh Z, Ferenczi-Fodor K (1998) Validated, stability-indicating semiquantitative purity test for allyestrenol drug substance and tablet by personal OPLC. J. Planar Chromatogr. 11; 463–466.Google Scholar
  259. Wulandari L, Indrayanto G (2003a) Densitometric determination of betamethasone dipropionate and salicylic acid in lotions, and validation of the method. J. Planar Chromatogr. 16; 438–441.Google Scholar
  260. Wulandari L, Indrayanto G (2003b) HPTLC determination of betamethasone in tablets and its validation. J. Liquid. Chromatogr. Rel. Technol. 26; 2709–2717.Google Scholar
  261. Wulandari L, Sia TK, Idrayanto G (2003) TLC densitometric determination of mometha-sone furoate in topical preparations: validation. J. Liquid. Chromatogr. Rel. Technol. 26; 109–117.Google Scholar
  262. Yamini Y, Asghari-Khiavi M, Bahramifar N (2002) Effect of different parameters on supercritical fluid extraction of steroid drugs, from spiked matrices and tablets. Talanta. 58; 1003–1010.Google Scholar
  263. Yan S-K, Xin W-F, Luo G-A, Wang Y-M, Cheng Y-Y (2005) Simultaneous determination of major bioactive components in Quingkailing injection by high-performance liquid chromatography with evaporative light scattering detection. Chem. Pharm. Bull. 53; 1392–1395.Google Scholar
  264. Ye L, Yu Y, Mosbach K (2001) Towards the development of molecularly imprinted artificial receptors for the screening of estrogenic chemicals. Analyst. 126; 760–765.Google Scholar
  265. Yu K, Balogh M (2001) A protocol for high-throughput drug mixture quantitation: fast LC-MS or flow-injection analysis-MS. LC-GC N. Am. 19; 60–72.Google Scholar
  266. Zakhari NA, Walash MI, Rizk MS, Toubar SS, Brooks CJW, Cole WJ (1991) Gas chromatographic assay of methyltestosterone in tablets. J. Pharm. Biomed. Anal. 9; 705–709.Google Scholar
  267. Zarzycki PK (2002) Simple chamber for temperature-controlled planar chromatography. J. Chromatogr. A 971; 193–197.Google Scholar
  268. Zarzycki PK, Smith R (2001) Separation of steroids using temperature-dependent inclusion chromatography. J. Chromatogr. A 912; 45–52.Google Scholar
  269. Zarzycki PK, Kulhanek KM, Smith R (2002) Chromatographic behaviour of selected steroids and their inclusion complexes with |3-cyclodextrin on octadecylsilica stationary phases with different carbon loads. J. Chromatogr. A 955; 71–78.Google Scholar
  270. Zarzycki PK, Kulhanek KM, Smith R, Bartoszuk MA, Lamparczyk H (2005) Planar chromatography versus column chromatography: a performance comparison. LC-GC N. Am. 23; 286–300.Google Scholar
  271. Zecevic M, Zivanovic Lj, Stojkovic A (2002) Validation of a high-performance liquid chromatography method for the determination of pancuronium in Pavulon injections. J. Chromatogr. 949; 61–64.Google Scholar
  272. Zhao Y, Jona J, Chow DT, Rong H, Semin D, Xia X, Zanon R, Spancake C, Maliski E (2002) High-throughput logP measurement using parallel liquid chromatography/ultraviolet/mass spectrometry and sample-pooling. Rapid Commun. Mass Spectrom. 16; 1548–1555.Google Scholar
  273. Zhu J, Coscolluella C (2000) Chromatographic assay of pharmaceutical compounds under column overloading. J. Chromatogr. B. 741; 55–65.Google Scholar
  274. Zivanovic Lj, Zecevic M, Markovic S, Petrovic S, Ivanovic I (2005) Validation of liquid chromatography method for analysis of lidocaine hydrochloride, dexamethasone acetate, calcium dobesilate, butylhydroxyanisol and degradation product hydroquinone in suppositories and ointment. J. Chromatogr. A. 1088; 182–186.Google Scholar

Copyright information

© Springer Science+Business Media B.V. 2010

Authors and Affiliations

  1. 1.Gedeon Richter Plc.BudapestHungary

Personalised recommendations