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选择一维或二维气相色谱-质谱联用仪,在单次进样中同时使用多个检测器进行定量分析。

Quantitative analysis of fragrance in selectable one dimensional or two dimensional gas chromatography-mass spectrometry with simultaneous detection of multiple detectors in single injection.

机构信息

Firmenich Asia Pte Ltd, 10 Tuas West Road, 638377 Singapore.

Firmenich Asia Pte Ltd, 10 Tuas West Road, 638377 Singapore.

出版信息

J Chromatogr A. 2014 Mar 14;1333:106-15. doi: 10.1016/j.chroma.2014.01.073. Epub 2014 Feb 1.

Abstract

A selectable one-dimensional ((1)D) or two-dimensional ((2)D) gas chromatography-mass spectrometry (GC-MS) system coupled with flame ionization detector (FID) and olfactory detection port (ODP) was employed in this study to analyze perfume oil and fragrance in shower gel. A split/splitless (SSL) injector and a programmable temperature vaporization (PTV) injector are connected via a 2-way splitter of capillary flow technology (CFT) in this selectable (1)D/(2)D GC-MS/FID/ODP system to facilitate liquid sample injections and thermal desorption (TD) for stir bar sorptive extraction (SBSE) technique, respectively. The dual-linked injectors set-up enable the use of two different injector ports (one at a time) in single sequence run without having to relocate the (1)D capillary column from one inlet to another. Target analytes were separated in (1)D GC-MS/FID/ODP and followed by further separation of co-elution mixture from (1)D in (2)D GC-MS/FID/ODP in single injection without any instrumental reconfiguration. A (1)D/(2)D quantitative analysis method was developed and validated for its repeatability - tR; calculated linear retention indices (LRI); response ratio in both MS and FID signal, limit of detection (LOD), limit of quantitation (LOQ), as well as linearity over a concentration range. The method was successfully applied in quantitative analysis of perfume solution at different concentration level (RSD≤0.01%, n=5) and shower gel spiked with perfume at different dosages (RSD≤0.04%, n=5) with good recovery (96-103% for SSL injection; 94-107% for stir bar sorptive extraction-thermal desorption (SBSE-TD).

摘要

本研究采用可选择的一维(1D)或二维(2D)气相色谱-质谱联用仪(GC-MS)系统,结合火焰电离检测器(FID)和嗅觉检测端口(ODP),用于分析香波中的香水油和香精。在这个可选择的 1D/2D GC-MS/FID/ODP 系统中,分流/不分流(SSL)进样器和程序升温汽化(PTV)进样器通过毛细管流技术(CFT)的 2 路分流器连接,分别用于液体样品进样和搅拌棒吸附萃取(SBSE)技术的热解吸(TD)。双链接进样器设置允许在单个序列运行中使用两个不同的进样口(一次一个),而无需将 1D 毛细管柱从一个入口重新定位到另一个入口。目标分析物在 1D GC-MS/FID/ODP 中进行分离,然后在单次进样中,从 1D 进一步分离 2D GC-MS/FID/ODP 中的共洗脱混合物,无需任何仪器重新配置。建立并验证了 1D/2D 定量分析方法的重复性 - tR;计算线性保留指数(LRI);在 MS 和 FID 信号中的响应比、检测限(LOD)、定量限(LOQ)以及浓度范围内的线性度。该方法成功应用于不同浓度水平的香水溶液的定量分析(RSD≤0.01%,n=5)和不同剂量的香波中添加香水的定量分析(RSD≤0.04%,n=5),回收率良好(SSL 进样为 96-103%;搅拌棒吸附萃取-热解吸(SBSE-TD)为 94-107%)。

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