熱裂解-氣相層析-質譜法

Pyrolysis–gas chromatography–mass spectrometry
英文缩写	PyGCMS
分类	质谱法
分析对象	聚合物s; 生物分子; 涂料
其它技术
其它技术	气相色谱法

熱裂解-氣相層析-質譜法（英語：Pyrolysis–gas chromatography–mass spectrometry，缩写PyGCMS ）是一種化學分析方法，透過加熱樣品使其裂解生成較小的分子，這些分子再透過气相色谱法進行分離，並利用質譜儀進行偵測與分析。^[1] ^[2]

運作原理

熱裂解是指在惰性氣體或真空環境中，使材料經由加熱發生熱分解的過程。樣品可直接接觸鉑絲，或放置於石英樣品管中，並迅速加熱至600–1000 °C。視應用需求，甚至可使用更高的溫度。實際應用中，熱解器通常採用三種不同的加熱技術：等溫爐、感應加熱（居里點燈絲）以及使用鉑絲的電阻加熱。在高溫下，大分子在其最弱的鍵結處斷裂，產生較小、揮發性較高的碎片。這些碎片隨後可藉由氣相層析法進行分離。由於熱裂解會產生種類繁多的分解產物，因此其氣相層析圖譜通常較為複雜。這些數據可做為材料指紋以確認材料身分，亦可結合質譜資訊，解析各個碎片以獲取結構資訊。為了提高極性碎片的揮發性，在熱裂解前可在樣品中添加各種甲基化試劑。^[3]

除了使用專用的熱解器外，固態與液態樣品也可直接於程式控溫汽化器(PTV)進樣口中進行熱裂解氣相層析。PTV進樣器可提供快速加熱（最高達每秒60 °C）與高達600–650 °C的最高溫度，對於許多熱裂解應用而言已足夠。其主要優勢在於無需額外購置專用儀器，便可在常規的氣相層析分析中整合熱裂解程序。在此情況下，可使用石英製的氣相層析進樣內襯。此方法可獲得定量數據，且已有文獻顯示，在 PTV進樣器內進行衍生化反應亦能產生良好結果。^[4]^[5]

應用

熱裂解氣相層析可用於鑑別非揮發性化合物。^[6]此類材料包括高分子聚合物，例如壓克力或醇酸樹脂。^[7]聚合物在進入氣相層析分離之前的裂解模式，有助於辨識其化學組成。熱裂解氣相層析亦應用於環境樣品之分析^[8] ，包括化石分析^[9]和微塑膠檢測^[10] 。本技術亦為法醫實驗室常用方法之一，用以分析犯罪現場取得之證物，例如塗料、黏著劑、塑膠、合成纖維以及土壤萃取物。^[11]

參考來源

^ Goodacre, R.; Kell, D. B. (1996). "Pyrolysis mass spectrometry and its applications in biotechnology". Curr. Opin. Biotechnol. 7 (1): 20–28. doi:10.1016/S0958-1669(96)80090-5. PMID 8791308.
^ Peacock, P. M.; McEwen, C. N. (2006). "Mass Spectrometry of Synthetic Polymers. Anal. Chem". Analytical Chemistry. 78 (12): 3957–3964. doi:10.1021/ac0606249. PMID 16771534.
^ Halket JM, Zaikin VG (2006). "Derivatization in mass spectrometry --7. On-line derivatisation/degradation". European Journal of Mass Spectrometry. 12 (1): 1–13. doi:10.1255/ejms.785. PMID 16531644. S2CID 36931671.
^ Erwin R. Kaal; Mitsuhiro Kurano; Margit Geißler; Hans-Gerd Janssen (2008). "Hyphenation of aqueous liquid chromatography to pyrolysis-gas chromatography and mass spectrometry for the comprehensive characterization of water-soluble polymers". Journal of Chromatography A. 1186 (1–2): 222–227. doi:10.1016/j.chroma.2007.10.035. PMID 17988672.
^ Eckerle, P.; Pursch, M.; Cortes, H. J.; Sun, K.; Winniford, B. & Luong, J. (2008). "Determination of short-chain branching content in polyethylene by pyrolysis comprehensive multidimensional gas chromatography using low thermal mass column technology". Journal of Separation Science. 31 (1): 3416–3422. doi:10.1002/jssc.200800218. PMID 18798214.
^ Hans-Joachim Hübschmann (27 July 2015). Handbook of GC-MS: Fundamentals and Applications. John Wiley & Sons. pp. 68–. ISBN 978-3-527-33474-2.
^ "National Gallery of Art Conservation: Scientific Research". Archived from the original on 2007-09-16. Retrieved 2007-08-21.
^ Janos P (2003). "Separation methods in the chemistry of humic substances". Journal of Chromatography A. 983 (1–2): 1–18. doi:10.1016/S0021-9673(02)01687-4. PMID 12568366.
^ Poinar HN (2002). "The genetic secrets some fossils hold". Acc. Chem. Res. 35 (8): 676–84. doi:10.1021/ar000207x. PMID 12186573.
^ Santos, Lúcia H. M. L. M.; Insa, Sara; Arxé, Marta; Buttiglieri, Gianluigi; Rodríguez-Mozaz, Sara; Barceló, Damià (2023-01-01). "Analysis of microplastics in the environment: Identification and quantification of trace levels of common types of plastic polymers using pyrolysis-GC/MS". MethodsX. 10: 102143. doi:10.1016/j.mex.2023.102143. hdl:10261/305864. ISSN 2215-0161.
^ Wheals, B. B.; Noble, W. (1972-09-01). "Forensic applications of pyrolysis gas chromatography". Chromatographia. 5 (9): 553–557. doi:10.1007/BF02277631. ISSN 1612-1112. S2CID 102208189.

[1] Goodacre, R.; Kell, D. B. (1996). "Pyrolysis mass spectrometry and its applications in biotechnology". Curr. Opin. Biotechnol. 7 (1): 20–28. doi:10.1016/S0958-1669(96)80090-5. PMID 8791308.

[2] Peacock, P. M.; McEwen, C. N. (2006). "Mass Spectrometry of Synthetic Polymers. Anal. Chem". Analytical Chemistry. 78 (12): 3957–3964. doi:10.1021/ac0606249. PMID 16771534.

[3] Halket JM, Zaikin VG (2006). "Derivatization in mass spectrometry --7. On-line derivatisation/degradation". European Journal of Mass Spectrometry. 12 (1): 1–13. doi:10.1255/ejms.785. PMID 16531644. S2CID 36931671.

[4] Erwin R. Kaal; Mitsuhiro Kurano; Margit Geißler; Hans-Gerd Janssen (2008). "Hyphenation of aqueous liquid chromatography to pyrolysis-gas chromatography and mass spectrometry for the comprehensive characterization of water-soluble polymers". Journal of Chromatography A. 1186 (1–2): 222–227. doi:10.1016/j.chroma.2007.10.035. PMID 17988672.

[5] Eckerle, P.; Pursch, M.; Cortes, H. J.; Sun, K.; Winniford, B. & Luong, J. (2008). "Determination of short-chain branching content in polyethylene by pyrolysis comprehensive multidimensional gas chromatography using low thermal mass column technology". Journal of Separation Science. 31 (1): 3416–3422. doi:10.1002/jssc.200800218. PMID 18798214.

[6] Hans-Joachim Hübschmann (27 July 2015). Handbook of GC-MS: Fundamentals and Applications. John Wiley & Sons. pp. 68–. ISBN 978-3-527-33474-2.

[7] "National Gallery of Art Conservation: Scientific Research". Archived from the original on 2007-09-16. Retrieved 2007-08-21.

[8] Janos P (2003). "Separation methods in the chemistry of humic substances". Journal of Chromatography A. 983 (1–2): 1–18. doi:10.1016/S0021-9673(02)01687-4. PMID 12568366.

[9] Poinar HN (2002). "The genetic secrets some fossils hold". Acc. Chem. Res. 35 (8): 676–84. doi:10.1021/ar000207x. PMID 12186573.

[10] Santos, Lúcia H. M. L. M.; Insa, Sara; Arxé, Marta; Buttiglieri, Gianluigi; Rodríguez-Mozaz, Sara; Barceló, Damià (2023-01-01). "Analysis of microplastics in the environment: Identification and quantification of trace levels of common types of plastic polymers using pyrolysis-GC/MS". MethodsX. 10: 102143. doi:10.1016/j.mex.2023.102143. hdl:10261/305864. ISSN 2215-0161.

[11] Wheals, B. B.; Noble, W. (1972-09-01). "Forensic applications of pyrolysis gas chromatography". Chromatographia. 5 (9): 553–557. doi:10.1007/BF02277631. ISSN 1612-1112. S2CID 102208189.

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熱裂解-氣相層析-質譜法

運作原理

應用

參考來源

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