丹磺酰氯柱前衍生-反相高效液相色谱法同时测定水产品中9种生物胺  

Simultaneous determination of 9 kinds of biogenic amines in aquatic products by dansyl chloride precolumn derivatization-reverse phase high performance liquid chromatography

作　　者：周朗君 陈钦 李秀英 ZHOU Lang-Jun;CHEN Qin;LI Xiu-Ying(Guangzhou Inspection Testing and Certification Group Co.,Ltd.,Guangzhou 511447,China;National Quality Testing Center for Processed Food(Guangdong),Guangzhou 511447,China)

机构地区：[1]广州检验检测认证集团有限公司,广州511447 [2]国家加工食品质量检验检测中心(广东),广州511447

出　　处：《食品安全质量检测学报》2025年第5期24-31,共8页Journal of Food Safety and Quality

基　　金：广州检验检测认证集团有限公司科技项目(2019kj07GZ)。

摘　　要：目的建立丹磺酰氯柱前衍生-反相高效液相色谱法同时检测水产品中9种生物胺的检测方法。方法采用5%三氯乙酸水溶液提取,10mg/mL丹磺酰氯丙酮溶液衍生,氨水终止衍生反应,乙腈定容获得9种生物胺的丹磺酰氯衍生物待测溶液。试样溶液通过反相液相色谱检测,以乙腈和水为流动相梯度洗脱,采用C_(18)色谱柱分离,紫外检测器在254 nm下检测。结果水产品中9种生物胺的定量限在1.08~7.59 mg/kg,加标回收率在85.2%~106.7%,精密度在1.5%~4.9%。采用所建立的方法测定广州市售的50批次高组胺鱼类,结果发现,广州市售的高组胺鱼类质量整体较好,β-苯乙胺和尸胺相对其他生物胺有较高检出率,但含量均低于35mg/kg,色胺、组胺、章鱼胺、亚精胺、精氨均为未检出。结论该方法快速、简便、灵敏度高,适用于水产品中9种生物胺的批量样品测定。Objective To establish a detection method for simultaneously detecting 9 kinds of biogenic amines in aquatic products using the dansyl chloride precolumn derivazation-reverse phase high performance liquid chromatography.Methods The samples were extracted with a 5%trichloroacetic acid solution and derivatized with a 10 mg/mL dansyl chloride acetone solution.The derivatization reaction was terminated with ammonia,and the resulting solution containing the dansyl chloride derivatives of the 9 kinds of biogenic amines was made up to volume with acetonitrile.The sample solution was analyzed by reverse phase liquid chromatography using a C_(18) column,with a mobile phase gradient of acetonitrile and water,and detected at 254 nm using a ultraviolet detector.Results The limits of quantitation of the 9 kinds of biogenic amines in aquatic products ranged from 1.08 to 7.59 mg/kg,with recovery rates ranging from 85.2%to 106.7%and precision ranging from 1.5%to 4.9%.The established method was used to analyze 50 batches of high-histamine fish sold in Guangzhou.The results revealed that the overall quality of the high-histamine fish in Guangzhou was good.β-phenylethylamine and cadaverine had relatively higher detection rates compared to other biogenic amines,but their content was all below 35 mg/kg.Histamine,putrescine,spermidine,agmatine,and arginine were not detected.Conclusion The method is fast,simple,and highly sensitive,making it suitable for batch sample determination of the 9 kinds of biogenic amines in aquatic products.

关 键 词：丹磺酰氯 柱前衍生 反相高效液相色谱法 水产品 生物胺 

分 类 号：O657.72[理学—分析化学] TS254.7[理学—化学]