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相比、聚二甲基硅氧烷体积和尺寸以及采样温度和时间对精油领域中某些挥发性化合物顶空吸附萃取回收率的影响。

Impact of phase ratio, polydimethylsiloxane volume and size, and sampling temperature and time on headspace sorptive extraction recovery of some volatile compounds in the essential oil field.

作者信息

Bicchi Carlo, Cordero Chiara, Liberto Erica, Rubiolo Patrizia, Sgorbini Barbara, Sandra Pat

机构信息

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

出版信息

J Chromatogr A. 2005 Apr 15;1071(1-2):111-8. doi: 10.1016/j.chroma.2004.09.054.

Abstract

This study evaluates concentration capability of headspace sorptive extraction (HSSE) and the influence of sampling conditions on HSSE recovery of an analyte. A standard mixture in water of six high-to-medium volatility analytes (isobutyl methyl ketone, 3-hexanol, isoamyl acetate, 1,8-cineole, linalool and carvone) was used to sample the headspace by HSSE with stir bars coated with different polydimethylsiloxane (PDMS) volumes (20, 40, 55 and 110 microL, respectively), headspace vial volumes (8, 21.2, 40, 250 and 1000 mL), sampling temperatures (25, 50 and 75 degrees C) and sampling times (30, 60 and 120 min, and 4, 8 and 16 h). The concentration factors (CFs) of HSSE versus static headspace (S-HS) were also determined. Analytes sampled by the PDMS stir bars were recovered by thermal desorption (TDS) and analysed by capillary GC-MS. This study demonstrates how analyte recovery depends on its physico-chemical characteristics and affinity for PDMS (octanol-water partition coefficients), sampling temperatures (50 degrees C) and times (60 min), the volumes of headspace (40 mL) and of PDMS (in particular, for high volatility analytes). HSSE is also shown to be very effective for trace analysis. The HSSE CFs calculated versus S-HS with a 1000 mL headspace volumes at 25 degrees C during 4 h sampling ranged between 10(3) and 10(4) times for all analytes investigated while the limits of quantitation determined under the same conditions were in the nmol/L range.

摘要

本研究评估了顶空吸附萃取(HSSE)的浓缩能力以及采样条件对分析物HSSE回收率的影响。使用六种高中等挥发性分析物(异丁基甲基酮、3-己醇、乙酸异戊酯、1,8-桉叶素、芳樟醇和香芹酮)的水标准混合物,通过HSSE对顶空进行采样,采用涂覆有不同聚二甲基硅氧烷(PDMS)体积(分别为20、40、55和110微升)、顶空瓶体积(8、21.2、40、250和1000毫升)、采样温度(25、50和75摄氏度)以及采样时间(30、60和120分钟,以及4、8和16小时)。还测定了HSSE与静态顶空(S-HS)的浓缩因子(CFs)。通过热解吸(TDS)回收由PDMS搅拌棒采样的分析物,并通过毛细管气相色谱-质谱联用仪进行分析。本研究表明分析物回收率如何取决于其物理化学特性以及对PDMS的亲和力(正辛醇-水分配系数)、采样温度(50摄氏度)和时间(60分钟)、顶空体积(40毫升)以及PDMS体积(特别是对于高挥发性分析物)。HSSE在痕量分析中也显示出非常有效。在25摄氏度下4小时采样期间,对于所有研究的分析物,相对于具有1000毫升顶空体积的S-HS计算的HSSE CFs在10³至10⁴倍之间,而在相同条件下测定的定量限在纳摩尔/升范围内。

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