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采用搅拌棒吸附萃取-热解吸联用气相色谱-质谱法测定三文鱼片中的异味化合物 2-甲基异莰醇和土臭素。

Determination of off-flavor compounds, 2-methylisoborneol and geosmin, in salmon fillets using stir bar sorptive extraction-thermal desorption coupled with gas chromatography-mass spectrometry.

机构信息

Lacombe Research Centre, Agriculture and Agri-Food Canada, 6000 C&E Trail, Lacombe, AB T4L 1W1, Canada.

出版信息

J Chromatogr A. 2013 Dec 20;1321:133-6. doi: 10.1016/j.chroma.2013.10.038. Epub 2013 Oct 16.

DOI:10.1016/j.chroma.2013.10.038
PMID:24252650
Abstract

A sensitive and solvent-less method for the determination of musty and earthy off-flavor compounds, 2-methylisoborneol (MIB) and geosmin (GSM), in salmon tissue was developed using stir bar sorptive extraction-thermal desorption coupled with gas chromatography-mass spectrometry (SBSE-TD-GCMS). MIB and GSM were solid phase extracted using polydimethylsiloxane (PDMS) coated stir bars, analyzed by gas chromatography, and detected in full scan mode of mass selective detector (MSD). Using this method, the calibration curves of MIB and GSM were linear in the range of 0.3-100ng/L, with a correlation coefficient above 0.999 and RSDs less than 4% (n=4). The limit of detection (LOD, S/N=3, n=6) and limit of quantification (LOQ, S/N=10, n=6) of MIB and GSM were both ∼0.3 and 1ng/L, respectively. The recoveries of MIB and GSM were 22% and 29% by spike in 30ng/L standard compounds, 23% and 30% by spike-in 100ng/L standard compounds in salmon tissue samples with good precision (<8% of RSDs, n=6), respectively. The recoveries of MIB and GSM were better than reported methodologies using SPME fibres (<10%) in fish tissue samples. This method was successfully applied to monitor and characterize depurated salmon fillet samples (0, 3, 6 and 10 days).

摘要

一种灵敏、无需溶剂的方法用于鲑鱼肉组织中霉土味化合物 2-甲基异莰醇(MIB)和土臭素(GSM)的测定,该方法采用搅拌棒吸附萃取-热解吸与气相色谱-质谱联用(SBSE-TD-GCMS)。MIB 和 GSM 采用聚二甲基硅氧烷(PDMS)涂层搅拌棒进行固相萃取,用气相色谱分析,并在质量选择性检测器(MSD)的全扫描模式下进行检测。使用该方法,MIB 和 GSM 的校准曲线在 0.3-100ng/L 范围内呈线性,相关系数均大于 0.999,相对标准偏差(RSD)小于 4%(n=4)。MIB 和 GSM 的检测限(LOD,S/N=3,n=6)和定量限(LOQ,S/N=10,n=6)均约为 0.3 和 1ng/L。在鲑鱼肉样品中,以 30ng/L 标准化合物添加时,MIB 和 GSM 的回收率分别为 22%和 29%,以 100ng/L 标准化合物添加时,回收率分别为 23%和 30%,精密度良好(RSD<8%,n=6)。该方法的回收率优于使用 SPME 纤维在鱼组织样品中报道的方法(<10%)。该方法成功应用于监测和表征脱盐鲑鱼片样品(0、3、6 和 10 天)。

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