Simultaneous Determination of Four Off-flavors in Freshwater Fish by Gas Chromatography-Mass Spectrometry Combined with Silica Solid Phase Extraction
10.19756/j.issn.0253-3820.241398
- VernacularTitle:硅胶固相萃取结合气相色谱-质谱法同时测定淡水鱼中的4种土腥味物质
- Author:
Liang-Liang TIAN
1
;
Dong-Mei HUANG
;
Yuan WANG
;
Xuan-Yun HUANG
;
Yong-Fu SHI
;
Hong-Li YE
Author Information
1. 中国水产科学研究院东海水产研究所农业农村部远洋与极地渔业创新重点实验室,上海 200090
- Keywords:
Odors;
n-Hexane;
Silica solid phase extraction;
Gas chromatography-mass spectrometry;
Fresh water fish
- From:
Chinese Journal of Analytical Chemistry
2025;53(7):1158-1166
- CountryChina
- Language:Chinese
-
Abstract:
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 C18,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∶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 μg/kg for GSM and MIB,0.2 μg/kg for IPMP and IBMP.The limits of quantitation(LOQ)were 1.0 μg/kg for GSM and MIB,0.6 μg/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.
