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目的建立一种可同时快速测定海产品中8种生物胺的丹磺酰氯柱前衍生反相高效液相色谱法。方法样品经5%三氯乙酸提取,丹磺酰氯柱前衍生后,采用Agilent zorbax SB-C_(18)色谱柱(4.6 mm×150 mm,5μm),以甲醇和水作为流动相,进行梯度洗脱。柱温30℃,流速为1.5 m L/min,采用UV紫外检测器,检测波长254 nm,对8种生物胺进行分离分析。结果结果显示,色胺、2-苯乙胺、腐胺、尸胺、组胺、酪胺、亚精胺和精胺在15 min内得到有效分离,在1~100 mg/L范围内线性系数r~2﹥0.999,8种生物胺测定方法的检出限范围为0.02~0.17 mg/L,定量限范围为0.067~0.57 mg/L,且重复性良好,向秋刀鱼中分别添加生物胺标准品20.0、50.0、100.0 mg/L 3个含量水平,8种生物胺平均回收率介于79%~117%之间,相对标准偏差为0.84%~12.57%。采用该方法测定了秋刀鱼等5类海产品中8种生物胺的含量,结果显示生物胺总含量在23~208 mg/kg之间。结论该方法简单、快速,灵敏度和准确度符合要求,适用于海产品中多种生物胺的同时检测。
Objective To establish a Dansyl chloride pre-column derivatization RP-HPLC method capable of simultaneous determination of eight biogenic amines in seafood. Methods The sample was extracted with 5% trichloroacetic acid and the Dansyl chloride was pre-column derivatized with an Agilent Zorbax SB-C 18 column (4.6 mm × 150 mm, 5 μm) using methanol and water as mobile phases. Off The column temperature was 30 ℃ and the flow rate was 1.5 m L / min. UV ultraviolet detector was used to detect the wavelength of 254 nm. Eight biogenic amines were separated and analyzed. The results showed that tryptamine, 2-phenylethylamine, putrescine, cadaverine, histamine, tyramine, spermidine and spermine were effectively separated within 15 min, linear coefficients in the range of 1 to 100 mg / L r ~ 2> 0.999, the detection limits of 8 biogenic amines ranged from 0.02 to 0.17 mg / L, the limits of quantification ranged from 0.067 to 0.57 mg / L, and the reproducibility was good. Biogenic amine standards 20.0,50.0,100.0 mg / L, the average recoveries of eight biogenic amines ranged from 79% to 117% with relative standard deviations of 0.84% to 12.57%. The method was used to determine the contents of 8 biogenic amines in 5 species of saury, including the total biogenic amines ranging from 23 to 208 mg / kg. Conclusion The method is simple, rapid, sensitive and accurate to meet the requirements, suitable for simultaneous detection of a variety of biogenic amines in seafood.