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目的建立鱼类胶原肽中精胺(Spm)、亚精胺(Spd)和腐胺(Put)的柱前衍生-高效液相色谱测定方法。方法样品经6 mol/L盐酸消化前处理,以10 mg/ml丹磺酰氯为衍生剂,在60℃下衍生,使用C18(4.6 mm×250 mm,5μm)色谱柱,以甲醇和水为流动相,梯度洗脱。结果 3种生物胺在浓度范围内线性相关系数均≥0.999 1,方法的检出限(LOD)为0.028 3 mg/L~0.125 0 mg/L,定量限(LOQ)为0.094 5 mg/L~0.500 0 mg/L,加标回收率为87.1%~102.6%,RSD为0.11%~4.90%。结论该方法操作简单、准确灵敏,可用于鱼类胶原肽中生物胺含量的测定。
Objective To establish a pre-column derivatization-high performance liquid chromatographic method for the determination of spermine (Spm), spermidine (Spd) and putrescine in fish collagen peptides. Methods The samples were pretreated with 6 mol / L hydrochloric acid and derivatized with 10 mg / ml Dansyl chloride at 60 ℃ using a C18 (4.6 mm × 250 mm, 5 μm) column with methanol and water as the mobile phase Phase, gradient elution. Results The linear correlation coefficients of three biogenic amines in the range of concentration were all ≥0.999 1. The limits of detection (LOD) of the three biogenic amines were 0.028 3 mg / L ~ 0.125 0 mg / L and the LOQ was 0.094 5 mg / L ~ 0.500 0 mg / L, the spiked recoveries ranged from 87.1% to 102.6%, and the RSDs ranged from 0.11% to 4.90%. Conclusion The method is simple, accurate and sensitive and can be used for the determination of biogenic amines in fish collagen peptides.