Simultaneous Determination of Four Off-flavors in Freshwater Fish by Gas Chromatography-Mass Spectrometry Combined with Silica Solid Phase Extraction

文献类型： 外文期刊

第一作者： Tian, Liang-Liang

作者： Tian, Liang-Liang;Shi, Yong-Fu;Ye, Hong-Li;Huang, Dong-Mei;Wang, Yuan;Huang, Xuan-Yun

作者机构：

关键词： Odors; n-Hexane; Silica solid phase extraction; Gas chromatography-mass spectrometry; Fresh water fish

期刊名称：CHINESE JOURNAL OF ANALYTICAL CHEMISTRY （ 影响因子：1.3； 五年影响因子：1.0 ）

ISSN： 0253-3820

年卷期： 2025 年 53 卷 7 期

页码：

收录情况： SCI

摘要： An effective method for simultaneously detecting four semivolatile earthy-musty odors in freshwater fish by gas chromatography-mass spectrometry (GC-MS) was developed. The concurrent extraction of geosmin (GSM), 2-methylisoborneol (MIB), 2-isopropyl-3-methoxypyrazine (IPMP), and 2-isobutyl-3-methoxypyrazine (IBMP) in fish tissue was conducted with n-hexane. The optimized QuEChERS material was implemented, and it was found that C 18, primary secondary amine (PSA) and MgSO4 could adsorb the target analytes in n-hexane. So only the graphitized carbon black (GCB) could be used to purify the extraction. The adsorption rates of different materials for the four kinds of odors materials were explored in n-hexane and ethyl acetate. The experimental results revealed that the adsorption rates of silica for the four targets were 99.5%-100% in n-hexane and 0.7%- 5.0% in ethyl acetate respectively. Then the silica solid phase extraction (SPE) method was utilized to eluent the compounds using 1.0 mL n-hexane/ethyl acetate in different proportions. The results of the comparative analysis demonstrated that n-hexane/ethyl acetate (4 & ratio;1, V/V) was the optimized eluent. Based on the obtained results, n-hexane extraction and GCB purification combined with silica SPE were used to isolate GSM, MIB, IPMP and IBMP from fish and the method was validated. It was found that the method showed good linearity in the range of 0.5-200 ng/mL, and with detection limits of 0.6 mu g/kg for GSM and MIB, 0.2 mu g/kg for IPMP and IBMP. The limits of quantitation (LOQ) were 1.0 mu g/kg for GSM and MIB, 0.6 mu g/kg for IPMP and IBMP. Good recoveries (77.5%- 112.0%) and relative standard deviations (1.56%-9.42%) were also obtained. The use of silica SPE greatly mitigated the issue that the off-flavor compounds were easily lost in the gas blowing concentration process. There was no cross contamination in this method because the sample pretreatments were conducted separately, which was different with the most commonly used HS-SPME method for detecting semi-volatile substances. The sensitivity of this method was high enough to produce good quantitative results below the odor thresholds of the examined off-flavor compounds.

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