Huang Ke-Jing, Wei Cai-Yun, Liu Wei-Li, Xie Wan-Zhen, Zhang Jun-Feng, Wang Wei
College of Chemistry and Chemical Engineering, Xinyang Normal University, Xinyang 464000, China.
J Chromatogr A. 2009 Sep 18;1216(38):6636-41. doi: 10.1016/j.chroma.2009.07.070. Epub 2009 Aug 5.
Ultrasound-assisted dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography-fluorescence detection was used for the extraction and determination of three biogenic amines including octopamine, tyramine and phenethylamine in rice wine samples. Fluorescence probe 2,6-dimethyl-4-quinolinecarboxylic acid N-hydroxysuccinimide ester was applied for derivatization of biogenic amines. Acetonitrile and 1-octanol were used as disperser solvent and extraction solvent, respectively. Extraction conditions including the type of extraction solvent, the volume of extraction solvent, ultrasonication time and centrifuging time were optimized. After extraction and centrifuging, analyte was injected rapidly into high-performance liquid chromatography and then detected with fluorescence. The calibration graph of the proposed method was linear in the range of 5-500 microg mL(-1) (octopamine and tyramine) and 0.025-2.5 microg mL(-1) (phenethylamine). The relative standard deviations were 2.4-3.2% (n=6) and the limits of detection were in the range of 0.02-5 ng mL(-1). The method was applied to analyze the rice wine samples and spiked recoveries in the range of 95.42-104.56% were obtained. The results showed that ultrasound-assisted dispersive liquid-liquid microextraction was a very simple, rapid, sensitive and efficient analytical method for the determination of trace amount of biogenic amines.
采用超声辅助分散液液微萃取结合高效液相色谱-荧光检测法,用于提取和测定米酒样品中的3种生物胺,包括章鱼胺、酪胺和苯乙胺。荧光探针2,6-二甲基-4-喹啉羧酸N-羟基琥珀酰亚胺酯用于生物胺的衍生化。分别以乙腈和1-辛醇作为分散剂溶剂和萃取溶剂。对萃取溶剂类型、萃取溶剂体积、超声时间和离心时间等萃取条件进行了优化。萃取和离心后,将分析物快速注入高效液相色谱仪,然后用荧光进行检测。该方法的校准曲线在5-500 μg mL⁻¹(章鱼胺和酪胺)和0.025-2.5 μg mL⁻¹(苯乙胺)范围内呈线性。相对标准偏差为2.4-3.2%(n=6),检测限在0.02-5 ng mL⁻¹范围内。该方法应用于米酒样品分析,加标回收率在95.42-104.56%之间。结果表明,超声辅助分散液液微萃取是一种测定痕量生物胺的非常简单、快速、灵敏且高效的分析方法。