摘要:
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C18(2.1 mm×100 mm,1.7 μm)色谱柱;以乙腈-10 mmol/L乙酸铵为流动相;流速:0.3 mL/min;检测波长为245 nm,柱温:35 ℃;进样量3.0 μL。结果:在该色谱条件下,9种生物胺在5.0~100.0 μg/mL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。
Abstract:
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 mL/min.The detection wavelength was at 245 nm and the column temperature was 35 ℃.The injection volume was 3.0 μL.Results:The linear range of 9 biogenic amines was from 5.0 to 100.0 μg/mL(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.
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