Jin Gaowa, Cai Youqiong, Yu Huijuan, Qian Beilei
East China Sea Fishery Research Institute, Chinese Academy of Fishery Sciences, Fishery Products Quality Inspection and Test Center (Shanghai), Ministry of Agriculture of China, Shanghai 200090, China.
Se Pu. 2010 Nov;28(11):1099-102.
A pre-column derivatization-high performance liquid chromatographic (HPLC) method has been developed for the determination of histamine in canned fish. The homogenated samples were ultrasonically extracted with perchloric acid aqueous solution, derivatized with dansyl chloride and diluted with acetonitrile to a desired volume. The samples were determined by HPLC with ultraviolet detector and quantified by external standard method. Adopting a C18 column with 1.8 microm stationary phase particles, the analysis time for each sample was smaller than 5 min with the flow rate of 0.3 mL/min. It can decrease the consumption of the mobile phase and save the cost. The linear range was 0.08-8.00 mg/L for histamine. The correlation coefficient was 0.999 98. The average recoveries of histamine at different concentration levels in spiked samples were greater than 96% and the relative standard deviations (RSDs) were smaller than 2.5%. The quantitation limit was 5.00 mg/kg for histamine in canned fish by HPLC. The results indicated that this HPLC method is fast, sensitive, reproducible and practical for the routine analysis of histamine in canned fish.
建立了一种柱前衍生-高效液相色谱（HPLC）法测定罐头鱼中的组胺。将匀浆后的样品用高氯酸水溶液超声提取，用丹磺酰氯衍生化，并用乙腈稀释至所需体积。采用配有紫外检测器的HPLC对样品进行测定，并采用外标法进行定量。采用粒径为1.8微米的C18柱，在流速为0.3 mL/min的条件下，每个样品的分析时间小于5分钟。该方法可减少流动相的消耗，节约成本。组胺的线性范围为0.08-8.00 mg/L，相关系数为0.999 98。加标样品中不同浓度水平组胺的平均回收率大于96%，相对标准偏差（RSD）小于2.5%。采用HPLC法测定罐头鱼中组胺的定量限为5.00 mg/kg。结果表明，该HPLC法快速、灵敏、重现性好，适用于罐头鱼中组胺的常规分析。
