Aznar M, Úbeda S, Nerin C, Kabir A, Furton K G
Analytical Chemistry Department, GUIA Group, I3A, EINA, University of Zaragoza, Mª de Luna 3, 50018, Zaragoza, Spain.
Analytical Chemistry Department, GUIA Group, I3A, EINA, University of Zaragoza, Mª de Luna 3, 50018, Zaragoza, Spain.
J Chromatogr A. 2017 Jun 2;1500:32-42. doi: 10.1016/j.chroma.2017.04.006. Epub 2017 Apr 8.
A simple, fast and sensitive analyte extraction method based on fabric phase sorptive extraction (FPSE) followed by gas chromatography-mass spectrometry (GC-MS) and ultra-performance liquid chromatography-quadrupole time of flight mass spectrometry (UPLC-QTOF-MS) analysis was developed for the analysis of 12 volatile compounds that represent most of the principal chemical families possessing different polarities and volatilities. Five FPSE media coated with different sol-gel sorbent chemistries having different polarities and selectivities were studied: long chain poly(dimethylsiloxane) (PDMS), short chain poly(tetrahydrofuran) (PTHF), Carbowax 20M (CW20M), short chain poly(dimethyl siloxane) (SC PDMS) and polyethylene glycol-polypropylene glycol-polyethylene glycol triblock copolymer (PEG-PPG-PEG). CW20M coated FPSE media was found to be the most efficient extraction media for the analytes of interest in the intended study. The developed methodology was applied to the analysis of orange juice obtained from fresh oranges and oranges after storing at 5°C for two months in order to identify the best chemical markers, both volatiles and non-volatiles, attributed to the freshness of orange. For this purpose, aliquots of the same juice extracts were analysed by GC-MS as well as by UPLC-QTOF-MS. Monoterpenes and terpenoids, such as terpinene, citronellal or estragole were among the volatile compounds that endured the biggest decrease after the extended storage period. Three non-volatile compounds including one amide (subaphyllin) and two flavanoids (tangeretin and nobiletin) also showed a clear decrease in signal intensity (>70%) after orange stored for two months.
开发了一种基于织物相吸附萃取（FPSE）的简单、快速且灵敏的分析物萃取方法，随后进行气相色谱-质谱联用（GC-MS）和超高效液相色谱-四极杆飞行时间质谱联用（UPLC-QTOF-MS）分析，用于分析12种挥发性化合物，这些化合物代表了大多数具有不同极性和挥发性的主要化学类别。研究了五种涂覆有不同极性和选择性的溶胶-凝胶吸附剂化学物质的FPSE介质：长链聚二甲基硅氧烷（PDMS）、短链聚四氢呋喃（PTHF）、聚乙二醇20M（CW20M）、短链聚二甲基硅氧烷（SC PDMS）和聚乙二醇-聚丙二醇-聚乙二醇三嵌段共聚物（PEG-PPG-PEG）。在本研究中，发现涂覆CW20M的FPSE介质是萃取目标分析物最有效的萃取介质。所开发的方法应用于新鲜橙子和在5°C下储存两个月后的橙子所制得的橙汁分析，以确定归因于橙子新鲜度的最佳化学标志物，包括挥发性和非挥发性标志物。为此，通过GC-MS以及UPLC-QTOF-MS对相同果汁提取物的等分试样进行分析。在延长的储存期后，挥发性化合物中降幅最大的包括萜品烯、香茅醛或草蒿脑等单萜和萜类化合物。三种非挥发性化合物，包括一种酰胺（亚叶素）和两种类黄酮（陈皮素和川陈皮素），在橙子储存两个月后也显示出信号强度明显下降（>70%）。
