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建立并验证一种基于 UPLC-MS 的柱端萃取方法,用于鱼类生物胺分析。

Developing and Validating a UPLC-MS Method with a StageTip-Based Extraction for the Biogenic Amines Analysis in Fish.

机构信息

School of Food Science and Technology, Dalian Polytechnic Univ., Natl. Engineering Research Center of Seafood, 1 Qinggongyuan, Ganjingzi District, Dalian, 116034, PR China.

Dept. of Agricultural and Biosystems Engineering, Iowa State Univ., Ames, IA, 50011, U.S.A.

出版信息

J Food Sci. 2019 May;84(5):1138-1144. doi: 10.1111/1750-3841.14597. Epub 2019 Apr 16.

DOI:10.1111/1750-3841.14597
PMID:30990887
Abstract

To effectively extract biogenic amines (BAs) from complex food matrices is an important issue. In this study, a stop-and-go-extraction tip (StageTip)-based method for simultaneous enrichment of six BAs including histamine, tyramine, putrescine, cadaverine, tryptamine, and β-phenylethylamine in fish samples was developed and optimized. This StageTip-based BAs extraction method required short extraction time, small sample size, and minimal consumption of organic solvents. In addition, an ultrahigh-performance liquid chromatography coupled with triple quadrupole mass spectrometer was used to identify and quantify BAs without derivatization. Target recovery efficiencies of BAs from spiked fish samples ranged from 84% to 110%. Linear regression models were established to determine BAs in the range of 0.4 to 3.0 mg/L (R > 0.995). Good repeatability was obtained with relative standard deviation of peak areas (1.17 to 5.61%) and retention time (0.09 to 0.20%). High sensitivity was achieved for the detection of six BAs (0.064 to 1.00 ng/L for the limit of detection, 0.10 to 5 ng/L for the limit of quantification). The proposed method had an obvious advantage in the analysis of BAs in complex food matrices such as fish tissues since it could reflect the subtle distribution of BAs from one fish fillet. PRACTICAL APPLICATION: A StageTip-based BAs enrichment combined with UPLC-MS analysis method was developed and optimized, which was low-cost, environmentally friendly, and with good analytical performances. As such, it has the potential to become a powerful tool for the analysis of BAs in different complex food matrices.

摘要

从复杂的食物基质中有效地提取生物胺(BAs)是一个重要的问题。在这项研究中,开发并优化了一种基于停走萃取尖端(StageTip)的方法,用于同时富集六种 BAs,包括组胺、酪胺、腐胺、尸胺、色胺和β-苯乙胺在鱼类样本中。这种基于 StageTip 的 BAs 提取方法需要短的提取时间、小的样品量和最小的有机溶剂消耗。此外,还使用超高效液相色谱-三重四极杆质谱联用仪对 BAs 进行了鉴定和定量,无需衍生化。从加标鱼样中回收 BAs 的目标回收率在 84%到 110%之间。建立了线性回归模型,用于在 0.4 到 3.0 mg/L 范围内测定 BAs(R > 0.995)。通过峰面积(1.17 到 5.61%)和保留时间(0.09 到 0.20%)的相对标准偏差得到了良好的重复性。对于六种 BAs 的检测,灵敏度很高(检出限为 0.064 到 1.00 ng/L,定量限为 0.10 到 5 ng/L)。该方法在分析鱼类组织等复杂食物基质中的 BAs 方面具有明显的优势,因为它可以反映一条鱼片中 BAs 的细微分布。实际应用:开发并优化了一种基于 StageTip 的 BAs 富集与 UPLC-MS 分析方法,该方法具有成本低、环保、分析性能良好等优点。因此,它有可能成为分析不同复杂食物基质中 BAs 的有力工具。

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