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

中文关键词:  丹磺酰氯  柱前衍生  反相高效液相色谱法  水产品  生物胺

英文关键词:dansyl chloride  precolumn derivazation  reverse phase high performance liquid chromatography  aquatic product  biogenic amine

中文摘要:

      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, 10 mg/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C18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35 mg/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。

英文摘要:

      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 C18 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.