气相色谱-飞行时间质谱测定鱼肉中蓝藻异味代谢物
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Determination of Cyanobacteria Odor Metabolites in Fish Samples by Gas Chromatography-Time-of-Flight Mass Spectrometry
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    摘要:

    通过优化微波蒸馏(microwave distillation,MD)及固相微萃取(solid-phase microextration,SPME)等提取富集条件,采用全二维气相色谱分离,有效实现了蓝藻中常见的8种异味代谢物的完全分离,以高分辨特征离子的精确质量数进行内标法定量分析,建立了一种鱼肉中蓝藻异味代谢物的检测方法。结果表明,8种异味代谢物在质量浓度0.01~100.00 μg/L时呈良好线性,方法的检出限为0.07~3.30 μg/kg,定量限为0.2~10.0 μg/kg,加标回收率在72.5%~103.7%,相对标准偏差(RSD)为2.26%~14.30% (n=6)。对淡水鱼肉产品进行分析检测,二甲基三硫、土臭素、β-环柠檬醛、β-紫罗兰酮、吲哚质量分数最高分别可达7.21×102、3.18、1.85×102、94.6、4.69×102 μg/kg。该分析方法准确、灵敏度高、稳定性好,极大降低了假阳性问题,可作为水产品中蓝藻异味筛查及确证方法。

    Abstract:

    Efficient separation of eight common off-flavor metabolites in cyanobacteria was successfully achieved by optimizing extraction and enrichment conditions such as microwave distillation and solid-phase microextraction, and utilizing comprehensive two-dimensional gas chromatography separation. A detection method for odor metabolites from cyanobacteria in fish meat was established by the quantitative analysis using internal standards with precise mass-to-charge ratios of characteristic ions. The results demonstrated that the eight off-flavor metabolites exhibited good linearity within a concentration range of 0.01 to 100.00 μg/L. The method had detection limits ranging from 0.07 to 3.30 μg/kg and quantification limits ranging from 0.2 to 10.0 μg/kg. The recovery rates ranged from 72.5% to 103.7%, and the relative standard deviations(RSD) were between 2.26% and 14.30%(n=6). Analysis of freshwater fish products revealed the highest concentration of dimethyl trisulfide, geosmin, β-cyclocitral, β-ionone and indole could reach 7.21×102, 3.18, 1.85×102, 94.6, 4.69×102 μg/kg, respectively. This analytical method is accurate, highly sensitive, and exhibits good stability, greatly reducing false positive issues. It can be used as a screening and confirmation method for the presence of cyanobacteria odor metabolites in aquatic products.

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宋启军,王利平,吴胜芳,虞锐鹏.气相色谱-飞行时间质谱测定鱼肉中蓝藻异味代谢物[J].食品与生物技术学报,2023,42(9):82-89.

SONG Qijun, WANG Liping, WU Shengfang, YU Ruipeng. Determination of Cyanobacteria Odor Metabolites in Fish Samples by Gas Chromatography-Time-of-Flight Mass Spectrometry[J]. Journal of Food Science and Biotechnology,2023,42(9):82-89.

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  • 在线发布日期: 2023-10-30
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