HPLC/UV–Vis/ESI MS for the analysis of textile dyes was successfully applied in a forensic setting. These results demonstrate that LC/MS is a viable method for the analysis of dyes in polyester and acrylic fibers. Parameters were optimized for disperse and basic dye classes that allowed for the separation and identification of dyes through mass spectral and UV–Vis data. Single fibers were successfully extracted and analyzed using these methods, including the use of a novel acetonitrile extraction for disperse dyes from polyester fibers in lieu of pyridine. Finally, a master method was developed that could separate and identify both disperse and basic dye standards. Continuing development of LC/MS analysis for all dye classes as well as the development of an extended spectral database will provide a greater discrimination capability in forensic fiber analysis. The authors wish to thank Faye Springer (Sacramento County District Attorney's Laboratory of Forensic Services, CA) and S. Kay Obendorf (Cornell University, NY) for their help with manuscript preparation. We wish to thank an anonymous source for donating the acrylic fibers. This work was sponsored by NSF CHE-0133758, State of California's Local Forensic Laboratory Improvement Program (LFLIP) through Coverdell 02 Federal Funding, and CAC A. Reed and Virginia McLaughlin Endowment Research Award. This work was carried out at Sacramento County District Attorney's Laboratory of Forensic Services. 1. Grieve M. Fibres and their examination in forensic science. In: Maehly A, Williams RL, editors. Forensic science progress, Vol. 4. Berlin: Springer-Verlag; 1990:44–119. 2. Okamura N, Miki H, Harada T, Yamashita S, Madaoka Y, Nakamoto Y, et al. Simultaneous determination of ephedrine, pseudoephedrine, norephedrine and methylephedrine in Kampo medicines by high-performance liquid chromatography A. J Pharm Biomed Anal 1999;20:363–72. 3. Samanidou V, Nikolaidou K, Papadoyannis I. Development and validation of a gradient-HPLC-PDAD method for the identification of ballpoint pen ink components: study of their decomposition on aging for forensic science applications. J Liq Chromatogr Relat Technol 2004;27(2):215–35. 4. Ng L-K, Lafontaine P, Brazeau L. Ballpoint pen inks: characterization by positive and negative ion-electrospray ionization mass spectrometry for the forensic examination of writing inks. J Forensic Sci 2002;47(6):1238–47. 5. Griffin R, Speers S, Elliot L, Todd N, Sogomo W, Kee T. An improved high-performance liquid chromatography system for the analysis of basic dyes in forensic casework. J Chromatogr A 1994;674:271–80. 6. Chen M, Moir D, Benoit F, Kubwabo C. Purification and identification of several sulphonated azo dyes using reversed-phase preparative high-performance liquid chromatography. J Chromatogr A 1998;825(1):37–44 7. Holčapek M, Jandera P, Přikryl J. Analysis of sulphonated dyes and intermediates by electrospray mass spectrometry. Dyes Pigments 1999;43:127–37. 8. Laing D, Gill R, Blacklaws C, Bickley H. Characterization of acid dyes in forensic fibre analysis by high performance liquid chromatography using narrow-bore column and DAD. J Chromatogr A 1988;442:187–208. 9. Speers S, Little B, Roy M. Separation of acid, basic and dispersed dyes by a single gradient elution reversed-phase high-performance liquid chromatography. J Chromatogr A 1994;674:263–70. 10. Yinon J, Saar J. Analysis of dyes extracted from textile fibers by thermospray high-performance liquid chromatography-mass spectrometry. J Chromatogr A 1991;586(1):73–84. 11. West JC. Extraction and analysis of disperse dyes on polyester textiles. J Chromatogr A 1981;208:47–54 12. Huang M, Yinon J, Sigman M. Forensic identification of dyes extracted from textile fibers by liquid chromatography mass spectrometry (LC-MS). J Forensic Sci 2004;49(2):238–49. 13. iggins K. Thin layer chromatographic analysis of fiber dyes. In: Robertson J, Grieve M, editors. Forensic examination of fibers. 2nd ed. Philadelphia: Taylor and Francis; 1999:298–300. 14. Agilent Technologies. Agilent 1100 Series LC/MSD reference collection. Palo Alto, CA: Agilent Technologies; 2002.
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LC-MS实验瓶颈的突破与优化
