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柱前衍生-反相高效液相色谱法测定草鱼肌肉中生物胺 被引量:2

Detection of biogenic amines in grass carp muscle by reversed phase high performance liquid chromatography with precolumn derivatization
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摘要 建立同时测定草鱼肌肉中7种生物胺的柱前衍生-反相高效液相色谱方法,并测定4℃贮藏条件下草鱼肌肉中生物胺含量的变化。以1,6-二氨基己烷为内标试剂,丹磺酰氯为柱前衍生试剂;CAPCELLPAKC18反相柱为固定相,甲醇和水为流动相,采用梯度洗脱,荧光检测器检测。以0.4mol/L高氯酸溶液为样品提取溶剂,正丁醇:氯仿=1:1(v:v)为萃取溶剂。7种生物胺在35min内得到良好的分离。在给定的浓度范围内,各生物胺呈现良好的线性相关(R2〉0.9991),精密度RSD〈2%,回收率在89.87%~103.43%之间,重现性RSD〈10%(精胺为10.02%)。4℃贮藏8d时间之内,草鱼肌肉中组胺含量增加最为显著,可以作为草鱼肌肉质量变化的指标之一。该方法灵敏度高,重现性好,是测定草鱼肌肉中生物胺含量的有效方法。 A method of reversed phase high performance liquid chromatography with precolumn derivatization was developed for the simultaneous determination of seven kinds of biogenic amines (BAs) in grass carp muscle.And the change of biogenic amines amount in grass carp muscle was determined during the storage at 4 ℃.1,6-diamino hexane was used as the internal standard,while the dansyl chloride the reagent of precolumn derivatization.As the CAPCELL PAK C18 reversed-phase column the stationary phase and methanol and water the mobile phase,the detection was conducted by gradient elution system with fluorescence detector.Biogenic amines were extracted by 0.4 mol/L perchloric acid,and then the extraction solvent of normal butanol and chloroform with the volume ratio 1:1.Seven kindsof biogenic amines had a good resolution within 35 minutes.In the given concentration range,the biogenic amines present good linear correlation (R20.9991) with the RSD of precision lower than 2%,the recovery rate between 89.87%~103.43%,and the RSD of repeatability lower than 10%.The content of histamine increased most significantly in grass carp muscle during the storage at 4 ℃ within 8 days.It could be used as one of the indicators of the quality of grass carp muscle.With the merits of high sensitivity and good repeatability,the method was feasible for the determination of biogenic amines in grass carp muscle.
出处 《食品科技》 CAS 北大核心 2013年第5期330-334,共5页 Food Science and Technology
基金 济南市科技发展计划项目(201102036) 武汉市科技计划供需对接项目(200951624512)
关键词 生物胺 反相高效液相色谱 草鱼 biogenic amines reversed phase high performance liquid chromatography grass carp
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参考文献14

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