超高效液相色谱法(UPLC)测定猪肉中9种生物胺含量

Determination of 9 Biogenic Amines in Pork by Using Ultra-high Performance Liquid Chromatography

目的:建立了超高效液相色谱法(UPLC)测定猪肉中色胺、β-苯乙胺、腐胺、尸胺、组胺、章鱼胺、酪胺、亚精胺、精胺含量的方法,并对该检测方法进行优化。方法:样品用5%TCA提取,经丹磺酰氯衍生后,采用C_(18)(2.1 mm×100 mm,1.7μm)色谱柱;以乙腈-10 mmol/L乙酸铵为流动相;流速:0.3 m L/min;检测波长为245 nm,柱温:35℃;进样量3.0μL。结果:在该色谱条件下,9种生物胺在5.0～100.0μg/m L范围内呈良好的线性关系,r≥0.999,最低检测限为0.028～0.29 mg/kg;仪器精密度较好,RSD(n=6)≤3.72%,其平均回收率为70.70%～111.80%。结论:所建立的方法灵敏、准确、简便、重现性好,出峰时间短,对于批量快速准确检测猪肉中生物胺具有很好的应用前景。

Objective: To develop and optimized ultra high pressure liquid chromatography( UPLC) methods for the quantitative determination of tryptamine,β-phenylethylamine,putrescine,cadaverive,histamine,octopamine,tyramine,spermidine and spermine in pork. Methods: The samples were extracted with 5% TCA and derived with dansyl chloride.( 2.1 × 100 mm,1.7 μm) C18 column was used.The mobile phase consisted of acetonitrile-10 mmol/L ammonium acetate solution at the flow rate of 0.3 m L/min. The detection wavelength was at 245 nm and the column temperature was 35 ℃.The injection volume was3.0 μL. Results: The linear range of 9 biogenic amines was from 5.0 to 100.0 μg/m L( r≥0.999).The limits of detection were in the range of 0.028~0.29 mg/kg.The relative standard deviation( RSD) of precision was lower than 3.72%.The average recovery was 70.70%~ 111.80%. Conclusions: The method was simple,accurate,sensitive,reproducible and short peak time. It would have a nice application foreground in a quick,accurate and batch quantity analysis methods of biogenic amines in pork.