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首页> 外文期刊>Analytical methods >Ultrasound-assisted dispersive liquid-liquid microextraction combined with high performance liquid chromatography for sensitive determination of five biogenic amines in fermented fish samples
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Ultrasound-assisted dispersive liquid-liquid microextraction combined with high performance liquid chromatography for sensitive determination of five biogenic amines in fermented fish samples

机译:超声辅助分散液-液微萃取-高效液相色谱法灵敏测定发酵鱼样品中的五种生物胺

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摘要

Ultrasound-assisted dispersive liquid-liquid microextraction (USADLLME) coupled to high performance liquid chromatography with fluorescence detection was developed for the simultaneous determination of five biogenic amines (histamine, tryptamine, cadaverine, tyramine and spermidine). The biogenic amines were derivatized with 9-fluorenylmethyl chloroformate before analysis. The five biogenic compounds were separated within 30 min using a C18 column and gradient elution with acetonitrile and 1% acetic acid. The parameters affecting extraction efficiency by USADLLME such as type and volume of extraction solvent and disperser were studied. Under the optimum conditions for USADLLME, 200 μL of 1-octanol as extraction solvent, 200 |xL acetonitrile as disperser with the aid of ultrasonication for 1 min, resulted in enrichment factors in the range of 12-42. Good linearity was obtained from 0.2-300 ng mL~(-1) (r~2 >0.992). Limits of detection ranged from 0.02 to 0.5 ng mL~(-1). The proposed method was applied in the analysis of biogenic amines in fermented fish samples, good recoveries were obtained in the range of 77.02-126.38%.
机译:开发了超声辅助分散液-液微萃取(USADLLME)结合高效液相色谱和荧光检测技术,用于同时测定五种生物胺(组胺,色胺,尸胺,酪胺和亚精胺)。在分析之前,用9-芴基甲基氯甲酸酯衍生生物胺。使用C18色谱柱在30分钟内分离出5种生物化合物,并用乙腈和1%乙酸进行梯度洗脱。研究了影响USADLLME萃取效率的参数,例如萃取溶剂和分散剂的种类和体积。在USADLLME的最佳条件下,借助200μL1-辛醇作为萃取溶剂,200μL乙腈作为分散剂,借助超声处理1分钟,得到的富集因子在12-42范围内。从0.2-300 ng mL〜(-1)(r〜2> 0.992)获得良好的线性。检测限范围为0.02至0.5 ng mL〜(-1)。该方法用于发酵鱼样品中生物胺的分析,回收率在77.02-126.38%之间。

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