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利用顶空固相微萃取-气相色谱串联质谱法测定养殖水体及水产品中土臭素和二甲基异莰醇的残留量

Residues of Geosmin and 2-Mathylisoborneol in Aquaculture Water and Aquatic Products Determined by Headspace Solid-phase Microextraction-Gas Chromatography Mass Spectrometry

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【作者】 邹剑敏; 卢奇; 桂源; 宋超; 陈家长;

【Author】 ZOU Jianmin;LU Qi;GUI Yuan;SONG Chao;CHEN Jiazhang;Freshwater Fisheries Research Center of Chinese Academy of Fishery Science;Laboratory of Quality & Safety Risk Assessment for Aquatic Products on Environmental Factors (Wuxi), Ministry of Agriculture and Rural Affairs;Key Laboratory of Control of Quality and Safety for Aquatic Products, Ministry of Agriculture and Rural Affairs;Wuxi Fishery College of Nanjing Agricultural University;

【通讯作者】 宋超;陈家长;

【机构】 中国水产科学研究院淡水渔业研究中心; 农业农村部水产品质量安全环境因子风险评估实验室(无锡); 农业农村部水产品质量安全控制重点实验室; 南京农业大学无锡渔业学院;

【摘要】 本文旨在优化微波蒸馏-固相微萃取-气质联用法(Microwave Distillation-Solid Phase Micro extraction-Gas Chromatographic Mass Spectrometry,MD-SPME-GC-MS)测定养殖水体及水产品中土臭素(Geosmin,GSM)和二甲基异莰醇(2-mathylisoborneo1,2-MIB)的检测方法。主要从微波蒸馏前处理过程的载气流速、微波功率、蒸馏时间和收集方式等4个参数进行了优化,最终确定最佳实验条件:载气流速60 mL/min、微波功率400 W、蒸馏时间6 min并定容于250 mL进行馏分收集定量。在养殖水体检测中,该方法对于GSM和2-MIB的检测限分别达到了1 ng/L和10 ng/L;而在水产品中检测限则分别为0.025μg/kg和0.25μg/kg。该方法的标准曲线在1~200 ng/L和10~200 ng/L的范围内线性关系良好,R~2分别为0.9997和0.9982。在水产品样品不同加标浓度(1、5、7、10、20μg/kg)的回收率实验中,GSM和2-MIB的平均回收率范围分别为45.28%~49.92%、82.15%~87.36%。本实验通过该方法对无锡地区的养殖池塘水样以及水产品进行了检测,发现水样中GSM和2-MIB的浓度均值为分别为19.58 ng/L和58.29 ng/L。而在水产品中,仅检出GSM,其浓度均值为0.61μg/kg。该方法能够广泛应用于养殖水体以及水产品土腥味物质的检测。

【Abstract】 In this paper,we optimized the determination method for geosmin (GSM) and 2-mathylisoborneo(2-MIB) in aquaculture water and aquatic products by using the method of microwave distillation-solidphase microextraction-gas chromatographic-mass spectrometry (MD-SPME-GC-MS).We optimized the four pre-treatment processing parameters,including carrier gas rate,microwave power,distillation time and collection method,and determined the experimental conditions as follows:carrier gas rate of 60 mL/min microwave power of 400 W,distillation time of 6 min,and constant of 250 mL.In aquaculture water,the detection limit of GSM and 2-MIB reached 1 ng/L and 10 ng/L,respectively.In aquatic products,the detection limit of GSM and 2-MIB reached 0.025μg/kg and 0.25μg/kg,respectively.The standard curve of this method had good liner relation in the range of 1-200 ng/L and 10-200 ng/L (R~2 was 0.9997 and 0.9982,respectively)The average recovery rate of GSM and 2-MIB at different concentrations (1,5,7,10,and 20μg/kg) was 45.28%-49.92% and 82.15%-87.36%,respectively.In this experiment,the water samples and aquatic product samples from Wuxi were detected by this method.The result showed that the average concentration of GSM and 2-MIB in the water samples was 19.58 ng/L and 58.29 ng/L,respectively.In aquatic products,only GSM was detected,and the average concentration was 0.61μg/kg.This method can be widely used to detect fishy substances in aquaculture water and aquatic products.

【基金】 中国水产科学研究院淡水渔业研究中心基本科研业务费资助“饵料代替政策对鲈鱼质量安全风险的影响评估”(2021JBFM18)
  • 【文献出处】 中国农学通报 ,Chinese Agricultural Science Bulletin , 编辑部邮箱 ,2022年35期
  • 【分类号】O657.63;TS254.7
  • 【下载频次】20
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