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| 固相微萃取‒气质联用法测定鱼肉中土臭味素和2-甲基异莰醇 |
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张艳红1,2,3, 李德祥1,2,3, 张凤枰1,2,3, 邹昌健1,2,3
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1.四川威尔检测技术股份有限公司 四川 成都 610041;2.通威股份有限公司水产畜禽营养与健康养殖农业农村部重点实验室 四川 成都 610093;3.通威股份有限公司水产健康养殖四川省重点实验室 四川 成都 610093
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| 摘要: |
| 采用顶空固相微萃取法建立了以顺式-十氢-1-萘酚为内标物、气相色谱质谱法测定鱼肉中土臭味素和2-甲基异莰醇的定性定量测定方法。考察了鱼肉中土臭味素和2-甲基异莰醇提取和定量方法，优化了顶空固相微萃取条件，并通过实际样品的测定，考察方法的适应性。结果显示，在0.1~10.0 μg/L范围内，土臭味素和2-甲基异莰醇峰面积与内标物峰面积的比值均与质量浓度的比值呈良好的线性关系，相关系数r2>0.999，检出限分别为0.018和0.023 μg/kg，定量限分别为0.059和0.076 μg/kg，3个浓度梯度添加平均回收率分别在68.67%~80.30%、62.67%~83.40%之间，相对标准偏差分别在2.35%~6.53%、3.16%~6.80%之间，该方法灵敏度高、重复性好，可用于批量鱼肉样品中土臭味素和2-甲基异莰醇的定量测定。 |
| 关键词: 顶空固相微萃取 气相色谱质谱法 鱼肉 土臭味素 2-甲基异莰醇 |
| DOI：10.19663/j.issn2095-9869.20200315001 |
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| Determination of geosmin and 2-methylisoborneol in fish muscle by gas chromatography-mass spectrometry |
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ZHANG Yanhong1,2,3, LI Dexiang1,2,3, ZHANG Fengping1,2,3, ZOU Changjian1,2,3
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1.Sichuan Willtest Technology Co. Ltd., Chengdu, Sichuan 610041, China;2.Key Laboratory of Aquatic, Livestock, Poultry Nutrition and Healthy Culturing, Ministry of Agriculture and Rural Affairs, Tongwei Co. Ltd., Chengdu, Sichuan 610093, China;3.Key Laboratory of Aquatic Healthy Aquaculture of Sichuan Province, Tongwei Co., Ltd., Chengdu, Sichuan 610093, China
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| Abstract: |
| Geosmin and 2-methylisoborneol are semi-volatile, off-flavor compounds with similar chemical structures that are produced by certain species of actinomycetes, fungi, and blue-green algae. These off-flavor compounds tend to bio-accumulate within fish, depending on the concentrations in the water, the water temperature, the fat content and mass of the fish, and other abiotic and biotic factors. It is necessary to develop an accurate test of geosmin and 2-methylisoborneol in fish muscle to improve the quality of aquaculture products. A novel qualitative and quantitative determination method for geosmin and 2-methylisoborneol in fish meat was established, using cis-decahydro-1-naphthol as an internal standard and headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry. The method of geosmin and 2-methylisoborneol extraction and quantification in fish meat was investigated, the conditions of headspace solid phase microextraction were optimized, and the adaptability of the method was examined through the measurement of actual samples. In the range of 0.1~10.0 μg/L, the ratio of the peak area of geosmin and 2-methylisoborneol to the peak area of the internal standard was linearly related to the ratio of the mass concentration. The correlation coefficient (r2) was > 0.999, the detection limits were 0.018 μg/kg and 0.023 μg/kg, respectively, the limits of quantification were 0.059 μg/kg and 0.076 μg/kg, the average recovery of the three concentration gradients was 68.67%~80.30% and 62.67%~83.40%, and the relative standard deviations were between 2.35%~6.53% and 3.16%~6.80%. This method is highly sensitive, has good repeatability, and can be used to determine the geosmin and 2-methylisoborneol contents of fish. |
| Key words: Headspace solid-phase microextraction Gas chromatography-mass spectrometry Fish muscle Geosmin 2-Methylisoborneol |