Firmenich Asia Pte Ltd, 10 Tuas West Road, 638377 Singapore.
Firmenich Asia Pte Ltd, 10 Tuas West Road, 638377 Singapore.
J Chromatogr A. 2014 Mar 14;1333:106-15. doi: 10.1016/j.chroma.2014.01.073. Epub 2014 Feb 1.
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).
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%)。