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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Determination of biogenic amines in chocolate by ion chromatographic separation and pulsed integrated amperometric detection with implemented wave-form at Au disposable electrode
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Determination of biogenic amines in chocolate by ion chromatographic separation and pulsed integrated amperometric detection with implemented wave-form at Au disposable electrode

机译:离子色谱分离-脉冲积分安培检测法在Au一次性电极上实现波形测定巧克力中的生物胺

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A rapid and selective cation exchange chromatographic method coupled to integrated pulsed amperometric detection (PAD) has been developed to quantify biogenic amines in chocolate. The method is based on gradient elution of aqueous methanesulfonic acid with post column addition of strong base to obtain suitable conditions for amperometric detection. A potential waveform able to keep long time performance of the Au disposable electrode was set up. Total analysis time is less than 20 min. Concentration levels of dopamine, serotonin, tyramine, histamine and 2-phenylethylamine were measured, after extraction with perchloric acid from 2 g samples previously defatted twice with petroleum ether. The method was used to determine the analytes in chocolate real matrices and their quantification was made with standard addition method. Only dopamine, histamine and serotonin were found in the analysed real samples. Repeatabilities of their signals, computed on their amounts in the real samples, were 5% for all of them. Repeatabilities of tyramine and phenethylamine were relative to standard additions to real samples (close to 1 mg/1 in the extract) and were 7 and 3%, respectively. Detection limits were computed with the 3 s of the baseline noise combined with the calibration plot regression parameters. They were satisfactorily low for all amines: 3 mg/kg for dopamine, 2 mg/kg for tyramine, I mg/kg for histamine, 2 mg/kg for serotonin, 3 mg/kg for 2-phenylethylamine. (c) 2005 Elsevier B.V. All rights reserved.
机译:已经开发了一种快速,选择性的阳离子交换色谱方法,并结合了集成脉冲安培检测(PAD)来量化巧克力中的生物胺。该方法基于在柱后加入强碱的甲磺酸水溶液的梯度洗脱,以获得用于安培检测的合适条件。建立了能够长期保持Au一次性电极性能的电势波形。总分析时间少于20分钟。用高氯酸从2 g先前用石油醚脱脂的样品中提取高氯酸后,测量多巴胺,5-羟色胺,酪胺,组胺和2-苯乙胺的浓度水平。该方法用于测定巧克力真实基质中的分析物,并使用标准添加方法进行定量。在分析的真实样品中仅发现多巴胺,组胺和5-羟色胺。根据真实样本中信号的数量计算,所有信号的重复性均为5%。酪胺和苯乙胺的重复性与相对于真实样品的标准添加量(提取物中接近1 mg / 1)相对,分别为7%和3%。用3 s基线噪声结合校准图回归参数计算检测极限。它们对所有胺均令人满意地低:多巴胺3 mg / kg,酪胺2 mg / kg,组胺1 mg / kg,5-羟色胺2 mg / kg,2-苯基乙胺3 mg / kg。 (c)2005 Elsevier B.V.保留所有权利。

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