Residual solvent testing: A review of gas-chromatographic and alternative techniques

Pharmaceutical Research

Volumn 20, Issue 3, 2003, Pages 337-344

  B'Hymer, Clayton ^a  

^a UNIVERSITY OF CINCINNATI   (United States)

Author keywords

Gas chromatography; Headspace analysis; Residual solvents; Review; Solid phase micro extraction

Indexed keywords

SOLVENT; VOLATILE AGENT;

ANALYTIC METHOD; DRUG MANUFACTURE; FOOD AND DRUG ADMINISTRATION; GAS CHROMATOGRAPHY; METHODOLOGY; MONITORING; PRIORITY JOURNAL; REVIEW; RISK; SOLID PHASE MICROEXTRACTION; TECHNIQUE; UNITED STATES; VALIDATION PROCESS;

CHROMATOGRAPHY, GAS; PHARMACEUTICAL PREPARATIONS; REPRODUCIBILITY OF RESULTS; SOLVENTS; TECHNOLOGY, PHARMACEUTICAL;

EID: 0037336532     PISSN: 07248741     EISSN: None     Source Type: Journal    
DOI: 10.1023/A:1022693516409     Document Type: Review

References (50)

1. Organic volatile impurities. In The 2002 United States Pharmacopeia XXV and National Formulary XX, The United States Pharmcopeial Convention, Rockville, Maryland, 2001, pp. 1943-1945.
2. M. A. Litchman and R. P. Upton. Head-space GLC determination of triethylamine in pharmaceuticals. J. Pharm. Sci. 62:1140-1142 (1973).
3. K. E. Rasmussen, S. Rasmussen, and A. Baerheim Svendsen. Quantitative determination of residual solvents in steroid hormones by means of gas-liquid chromatography and solid injection. J. Chromatogr. 71:543-544 (1972).
4. Harmonised Tripartite Guideline on Impurities in New Drug Substances. (Q3A), International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use (ICH), Geneva, Switzerland, 1997.
5. G. Rousseau and P. Jeffs. International conference on harmonization impurity guidelines - the industry perspective. J. Drug Informa. 34:903-907 (2000).
6. International Conference on Harmonisation. Guidance on Impurities. Residual Solvents. Federal Register 62:67377-67388 (1997).
7. Guidance for Industry, Q3C Impurities: Residual Solvents, U.S. Food and Drug Administration, Rockville, Maryland, December 1997.
8. K. J. Mulligan and H. McCauley. Factors that influence the determination of residual solvents in pharmaceuticals by automated static headspace sampling coupled to capillary GC-MS. J. Chromatogr. Sci. 33:49-54 (1995).
9. I. G. McWilliam and R. A. Dewar. Flame ionization detector for gas chromatography. Nature 181:760-765 (1958).
10. D. G. Westmorland and G. R. Rhodes. Analytical techniques for trace organic compounds II: Detectors for gas chromatography. Pure Appl. Chem. 61:1148-1160 (1989).
11. C. Witschi and E. Doelker. Residual solvents in pharmaceutical products: acceptable limits, influences on physicochemical properties, analytical methods and documented values. Eur. J. Pharm. Biopharm. 43:215-242 (1997).
12. B. S. Kersten. Drug matrix effect on the determination of residual solvents in bulk pharmaceuticals by wide-bore capillary gas chromatography. J. Chromatogr. Sci. 30:115-119 (1992).
13. I. D. Smith and D. G. Waters. Determination of residual solvent levels in bulk pharmaceuticals by capillary gas chromatography. Analyst 116:1327-1331 (1991).
14. D. W. Foust and M. S. Bergen. Analysis of solvent residues in pharmaceutical bulk drugs by all-coated open tubular gaschromatography. J. Chromatogr. 469:161-173 (1989).
15. Q. C. Li, K. A. Cohen, and G. Zhuang. A capillary gas chromatographic procedure for the analysis of nine common residual solvents in water-insoluble bulk pharmaceuticals. J. Chromatogr. Sci. 36:119-124 (1998).
16. H. Hachenberg and A. P. Schmidt. Gas Chromatographic Headspace Analysis. Heyden Press, Rheine, Germany, 1977.
17. J. Drozd and J. Novak. Headspace gas analysis by gas chromatography. J. Chromatogr 165:141-165 (1979).
18. C. F. Poole and S. A. Schuette. Isolation and concentration techniques for capillary column gas chromatographic analysis. J. High Res. Chromatogr 6:526-549 (1983).
19. A. J. Nunez, L. F. Gonzlez, and J. Janak. Pre-concentration of headspace volatiles for trace organic analysis by gas chromatography. J. Chromatogr. 300:127-162 (1984).
20. A. G. Vitenberg. Methods of equilibrium concentration for the gas chromatographic determination of trace volatiles. J. Chromatogr. 556:1-24 (1991).
21. A. N. Marinchev, A. G. Vitenberg, and A. S. Bureiko. Efficiency of gas extraction in headspace analysis. J. Chromatogr. 600:251-256 (1992).
22. C. C. Camarasu, M. Meqei-Szuts, and G. B. Varga. Residual solvents in pharmaceutical products by GC-HS and GC-MS-SPME. J. Pharm. Biomed 18:623-638 (1998).
23. T. P. Wampler, W. A. Bowe, and E. J. Levy. Dynamic headspace analysis of residual volatiles in pharmaceuticals. J. Chromatogra. Sci. 23:64-67 (1985).
24. C. D. McAullife. GC determination of solutes by multiple phase equilibration. Chem. Tech. 1:46-51 (1971).
25. B. Kolb and P. Pospisil. A gas chromatographic assay for quantitative analysis of volatiles in solid materials by discontinuous gas extraction. Chromatographia 10:705-711 (1977).
26. B. Kolb, P. Pospisil, and M. Auer. Quantitative headspace analysis of solid samples - a classification of various sample types. Chromatographia 19:113-122 (1984).
27. C. B'Hymer. Static headspace gas chromatographic method for the determination of residual solvents in vigabatrin drug substance. J. Chromatogr. 438:103-107 (1988).
28. A. G. Vitenberg and M. I. Kostkina. Gas chromatographic head space analysis on capillary columns. J. Anal. Chem. USSR 43:253-261 (1988).
29. W. C. Kidd. Evaluation of the proposed automated headspace method for organic volatile impurities. Pharm. Forum 19:5063-5066 (1993).
30. K. J. Dennis, P. A. Josephs, and J. Dokladalova. Proposed automated headspace method for organic volatile impurities (467) and other residual solvents. Pharm. Forum 18:2964-2972 (1992).
31. N. Kumar and J. C. Egoville. Headspace gas chromatography method for the analysis of volatile impurities in a hormone replacement transdermal patch. J. Chromatogr. A 859:113-118 (1999).
32. L. Hong and H. Altorfer. A micro-sized technique for determination of organic volatile impurities in water-insoluble pharmaceuticals. Chromatographia 53:76-80 (2001).
33. H. Lord and J. Pawliszyn. Evolution of solid-phase microextraction technology. J. Chromatogr. A 885:153-193 (2000).
34. C. L. Arthur and J. Pawliszyn. Solid-phase microextraction with thermal-desorption using fused-silica optical fibers. Anal. Chem. 62:2145-2148 (1990).
35. Z. Zhang and J. Pawliszyn. Sampling volatile organic compounds using a modified solid phase microextraction device. J. High Resol. Chromatogr. 19:155-160 (1996).
36. C. C. Camarasu. Headspace SPME method development for the analysis of volatile polar residual solvents by GC-MS. J. Pharm. Biomed. 23:197-210 (2000).
37. S. A. Coran, V. Giannellini, S. Furlanetto, M. Banbagiotti-Alberti, and S. Pinznuti. Improving gas chromatographic determination of solvents in pharmaceuticals by combined use of headspace solid-phase microextraction and isotopic dilution. J. Chromatogr. A 915:209-216 (2001).
38. Combi PAL - multiple injection modes on a single GC system. Varian, Inc., Palo Alto, California, 2002 product literature.
39. C. L. Arthur, L. M. Killam, K. D. Buchholz, J. Pawliszyn, and J. R. Berg. Automation and optimization of solid-phase microextraction. Anal. Chem. 64:1960-1966 (1992).
40. J. M. Green. A practical guide to analytical method validation. Anal. Chem. 68:305A-309A (1996).
41. J. Newman and C. J. Nunn. Solvent retention in organic coatings. Prog. Org. Coatings 3:221-243 (1975).
42. J. P. Guimbard, J. Besson, S. Beaufort, J. Pittie, and M. Gachon. Evaluation des solvant residuels. S.T.P. Pharma. Practiques 1:272-277 (1991).
43. J. P. Benoit, F. Courteille, and C. Thies. A physicochemical study of the morphology of progesterone-loaded poly(D,L-lactide) microspheres. Int. J. Pharm. 29:95-105 (1986).
44. C. Dubernet, J. C. Rouland, and J. P. Benoit. Comparative study of two ethylcellulose forms (raw material and microspheres) carried out through thermal analysis. Int. J. Pharm. 64:99-107 (1990).
45. P. H. List and G. Laun. Zusammenhang zwischen Losungsmittelresten und Permeabilitat von Eudragit L-Filmen. Pharm. Ind. 42:399-401 (1980).
46. H. Weitkamp and R. Barth, Bestimmung kleiner Gehaltswerte nach dem Aufstockverfahren. In H. Weitkamp and R. Barth (eds.), Einfurungin die quantitative Infrarot-Spektrophotometrie. Georg Thieme Verlag, Stuttgart, Germany, 1976, pp. 58-67.
47. Z. Osawa and M. Aiba. Effect of residual solvent on photodegradation of poly(vinyl chloride). Poly. Photochem. 2:339-348 (1982).
48. H. W. Avdovich, M. J. Lebelle, C. Savard, and W. L. Wilson. Nuclear magnetic resonance identification of solvent residue in cocaine. Forensic Sci. Int. 49:225-235 (1991).
49. C. Thomasin, P. Johansen, R. Alder, R. Besmsel, G. Hottinger, H. Altorfer, A. D. Wright, G. Wehrli, H. P. Merkle, and B. Gander. A contribution to overcoming the problems of residual solvents in biodegradable microspheres prepared by coacervation. J. Pharm. Biopharm. 42:16-24 (1996).
50. R. J. Mumper and M. Jay. Poly(L-lactic acid) microspheres containing neutron-activatable holmium-165: a study of the physical characteristics of microspheres before and after irradiation in a nuclear reactor. Pharm. Res. 9:149-154 (1992).