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采用稳定同位素稀释法和固相萃取-气相色谱-三重四极杆质谱联用技术测定鱼虾肌肉组织中的丁香酚。

Determination of eugenol in fish and shrimp muscle tissue by stable isotope dilution assay and solid-phase extraction coupled gas chromatography-triple quadrupole mass spectrometry.

作者信息

Li Jincheng, Liu Huan, Wang Chaoying, Wu Lidong, Liu Dan

机构信息

Chinese Academy of Fishery Sciences, No. 150 Qingta, Yongding Road, Beijing, 100141, China.

Beijing University of Agriculture, Beinong Road 7, Huilongguan, Changping District, Beijing, 102206, China.

出版信息

Anal Bioanal Chem. 2016 Sep;408(24):6537-44. doi: 10.1007/s00216-016-9850-z. Epub 2016 Aug 16.

Abstract

In this study, we developed a new method for the accurate quantification of eugenol in fish samples based on stable isotope dilution assay (SIDA) and solid-phase extraction (SPE) coupled gas chromatography-triple quadrupole mass spectrometry (SIDA-SPE-GC-MS/MS). Due to the difference of matrix effect (ME), it was difficult to determine accurately the level of eugenol residue in different fish and shrimp samples based on external standard calibration method. SIDA was applied to compensate matrix effect (ME) that eugenol-d3 was used as internal standard (IS). Freshwater fish (carp, channel catfish), marine fish (turbot), and shrimp (Penaeus vannawei) were used for the method validation. The average recoveries of eugenol were in the range of 94.7 to 109.78 % when the spiking levels were 10, 50, and 200 μg kg(-1). The inter-day and intra-day precisions were in the range of 1.15-8.19 and 0.71-8.45 %. The limit of detection (LOD) and the limit of quantification (LOQ) were approximately 2.5 and 5.0 μg kg(-1). This method was applied to the real fish samples assay obtained from aquaculture markets in Beijing, China. Eugenol residue was found in two fish samples with the levels at 6.2 and 7.7 μg kg(-1), respectively. Graphical abstract Determination of eugenol in fish and shrimp muscle tissue.

摘要

在本研究中,我们基于稳定同位素稀释法(SIDA)和固相萃取(SPE)结合气相色谱-三重四极杆质谱联用技术(SIDA-SPE-GC-MS/MS),开发了一种准确测定鱼类样品中丁香酚含量的新方法。由于基质效应(ME)的差异,基于外标校准法难以准确测定不同鱼虾样品中丁香酚残留水平。采用SIDA补偿基质效应,以丁香酚-d3作为内标(IS)。使用淡水鱼(鲤鱼、斑点叉尾鮰)、海水鱼(大菱鲆)和虾(凡纳滨对虾)进行方法验证。当加标水平为10、50和200 μg kg⁻¹时,丁香酚的平均回收率在94.7%至109.78%之间。日间和日内精密度分别在1.15 - 8.19%和0.71 - 8.45%之间。检测限(LOD)和定量限(LOQ)分别约为2.5和5.0 μg kg⁻¹。该方法应用于从中国北京水产市场采集的实际鱼类样品分析。在两个鱼类样品中检测到丁香酚残留,含量分别为6.2和7.7 μg kg⁻¹。图形摘要 鱼虾肌肉组织中丁香酚的测定

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