分子印迹固相萃取/液-质谱联用法测定烟熏鲟鱼中苯并芘
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国家重点研发计划项目(2016YFD0400703-4);浙江省重点研发计划项目(2017C03041)


Determination of Benzo[a]pyrene in Smoked Sturgeon (Acipenser sinensis)Using Molecular-imprinted Solid-phase Extraction Liquid Chromatography Tandem Mass Spectrometry Method
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    摘要:

    目前常规苯并芘检测方法存在着专一性不强、灵敏度低等问题,为精确测定市售烟熏鲟鱼中痕量3,4-苯并芘(3,4-BaP),本试验合成了3,4-BaP分子印迹固相萃取(BISPE)填料,并以此建立了固相萃取-超高效液相色谱串联质谱(SPE-UPLC-MS/MS)的方法。制备的3,4-BaP分子印迹填料为分散的球状颗粒,其外径在20~90μm不等,应用BISPE成功富集了烟熏鲟鱼中的3,4-BaP,并比较了Sep-pak,HLB和Florisil的萃取效率。经方法学验证,该方法线性好(R2=0.9998),检出限(LoD)0.98μg/kg,定量限(LoQ)3.16μg/kg,日内和日间精密度的相对标准偏差分别为3.26%~4.77%和3.78%~5.26%,回收率为89.7%~95.3%,RSD为2.89%~3.44%,符合痕量分析的要求。对市售50个批次烟熏鲟鱼进行测试发现,3,4-BaP阳性检出率为24%。结果表明,该方法适用于烟熏鲟鱼中3,4-BaP的检测,相关数据能为职能部门提供相关依据,进而为消费者食品安全提供保障。

    Abstract:

    The current normal method for the determination of benzo(a)pyrene is not specific, and its sensitivity is not very good. The 3,4-benzo(a)pyrene(3,4-BaP) is an organic compound with the formula C20H12. 3,4-BaP is a harmful compound, because it generates carcinogenic and mutagenic metabolites which can intercalate into DNA and interference with transcription. In this study, the molecular imprinted sorbent was synthesized and packed into a solid-phase extraction (SPE) cartridge for the enrichment of 3,4-BaP in smoked sturgeon (Acipenser sinensis) bought from local market. An analytical method was also developed for accurate determination of 3,4-BaP on the basis of ultra-performance liquid chromatography tandem mass spectrometry. The molecular imprinted sorbents are dispersed spherical particles, with diameter from 20 to 90 μm. It was successfully applied in the enriching of 3,4-BaP, and its performance was compared with Sep-pak, HLB, and Florisil SPE. The method was validated, and the results showed that the calibration curve is linear with R2 = 0.9998. The limit of detection (LoD) and limit of quantitation (LoQ) are 0.98 and 3.16 μg/kg, respectively. The RSDs of intra-day and inter-day accuracy are 3.26%-4.77% and 3.78%-5.26%, respectively. The recovery ranged from 89.7% to 95.3%, with RSD 2.89%-3.44%. Afterwards, the method was successfully applied to determine the 3,4-BaP in 50 batches of smoked sturgeon. The results indicated that 12 positive samples were found. The content of 3,4-BaP in the worst sample reached 21.9 μg/kg. The contents of 3,4-BaP in the other samples are lower than 3.58 μg/kg. In conclusion, this method is good at determining 3,4-BaP in smoked sturgeon. The relevant data could be used as reference for the functional departments for ensuring the food safety for consumers.

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林亚楠;李诗言;崔益玮;戴志远;陈康;王扬;沈清;.分子印迹固相萃取/液-质谱联用法测定烟熏鲟鱼中苯并芘[J].中国食品学报,2020,20(3):251-257

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  • 在线发布日期: 2020-04-14
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