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以环糊精衍生物作为手性选择剂的常规窄口径短毛细管柱,用于加速对映体选择性气相色谱和对映体选择性气相色谱 - 质谱分析。

Conventional and narrow bore short capillary columns with cyclodextrin derivatives as chiral selectors to speed-up enantioselective gas chromatography and enantioselective gas chromatography-mass spectrometry analyses.

作者信息

Bicchi Carlo, Liberto Erica, Cagliero Cecilia, Cordero Chiara, Sgorbini Barbara, Rubiolo Patrizia

机构信息

Dipartimento di Scienza e Tecnologia del Farmaco, Università degli Studi di Torino, Via Pietro Giuria 9, 10125 Turin, Italy.

出版信息

J Chromatogr A. 2008 Nov 28;1212(1-2):114-23. doi: 10.1016/j.chroma.2008.10.013. Epub 2008 Oct 10.

Abstract

The analysis of complex real-world samples of vegetable origin requires rapid and accurate routine methods, enabling laboratories to increase sample throughput and productivity while reducing analysis costs. This study examines shortening enantioselective-GC (ES-GC) analysis time following the approaches used in fast GC. ES-GC separations are due to a weak enantiomer-CD host-guest interaction and the separation is thermodynamically driven and strongly influenced by temperature. As a consequence, fast temperature rates can interfere with enantiomeric discrimination; thus the use of short and/or narrow bore columns is a possible approach to speeding-up ES-GC analyses. The performance of ES-GC with a conventional inner diameter (I.D.) column (25 m length x 0.25 mm I.D., 0.15 microm and 0.25 microm d(f)) coated with 30% of 2,3-di-O-ethyl-6-O-tert-butyldimethylsilyl-beta-cyclodextrin in PS-086 is compared to those of conventional I.D. short column (5m length x 0.25 mm I.D., 0.15 microm d(f)) and of different length narrow bore columns (1, 2, 5 and 10 m long x 0.10 mm I.D., 0.10 microm d(f)) in analysing racemate standards of pesticides and in the flavour and fragrance field and real-world-samples. Short conventional I.D. columns gave shorter analysis time and comparable or lower resolutions with the racemate standards, depending mainly on analyte volatility. Narrow-bore columns were tested under different analysis conditions; they provided shorter analysis time and resolutions comparable to those of conventional I.D. ES columns. The narrow-bore columns offering the most effective compromise between separation efficiency and analysis time are the 5 and 2m columns; in combination with mass spectrometry as detector, applied to lavender and bergamot essential oil analyses, these reduced analysis time by a factor of at least three while separation of chiral markers remained unaltered.

摘要

对复杂的植物源实际样品进行分析需要快速、准确的常规方法,以便实验室在降低分析成本的同时提高样品通量和生产率。本研究采用快速气相色谱法的方法来研究缩短对映体选择性气相色谱(ES-GC)的分析时间。ES-GC分离是由于对映体与环糊精主体-客体之间的弱相互作用,这种分离是由热力学驱动的,并且受温度的强烈影响。因此,快速升温速率可能会干扰对映体的鉴别;因此,使用短柱和/或窄内径柱是加快ES-GC分析的一种可能方法。将涂有30%的2,3-二-O-乙基-6-O-叔丁基二甲基甲硅烷基-β-环糊精的PS-086常规内径(I.D.)柱(25 m长×0.25 mm内径,0.15微米和0.25微米固定相液膜厚度)的ES-GC性能与常规内径短柱(5 m长×0.25 mm内径,0.15微米固定相液膜厚度)以及不同长度的窄内径柱(1、2、5和10 m长×0.10 mm内径,0.10微米固定相液膜厚度)在分析农药外消旋体标准品以及香料香精领域的实际样品时的性能进行了比较。短的常规内径柱分析时间较短,与外消旋体标准品的分离度相当或更低,这主要取决于分析物的挥发性。窄内径柱在不同的分析条件下进行了测试;它们提供了较短的分析时间,并且分离度与常规内径ES柱相当。在分离效率和分析时间之间提供最有效折衷的窄内径柱是5 m和2 m柱;与作为检测器的质谱联用,应用于薰衣草和佛手柑精油分析时,这些柱将分析时间缩短了至少三倍,而手性标记物的分离保持不变。

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