摘要
目的建立高效液相色谱-荧光检测法(HPLC-FLD)检测黄酒中色胺、苯乙胺、腐胺、尸胺、酪胺、章鱼胺、组胺、亚精胺及精胺。方法生物胺与内标1,7-二氨基庚烷与衍生试剂丹磺酰氯在特定条件下进行衍生,衍生物用乙醚萃取、N2吹干,再用乙腈定容、混匀,过膜后进HPLC分析。以C18色谱柱为分离柱,FLD检测器检测,流动相为乙腈和水,梯度洗脱,流速为1 ml/min,柱温30℃,以保留时间定性,内标法定量。结果 9种生物胺在1.0 mg/L^75.0 mg/L范围内呈良好的线性关系,加标回收率在80%~121%,该法各组分检测限为0.06 mg/kg^0.71 mg/kg,回收率RSD值在0.69%~2.36%之间。结论本法操作简便、准确可靠,能够同时测定黄酒中9种生物胺的含量。
Objective To establish HPLC - FLD method for determiantion of 9 biogenic amine including tryptamine, phenyleth- ylamine, putrescine, cadaverine, tyramine, octopamine, histamine, spermidine and spermine in rice wine. Methods Biogen- ic amines and internal standard 1,7 - Diaminoheptane reacted with dansyl chloride under certain conditions to form derivatives which were then extracted with ether. Then the extracts were blown to dryness by N2, dissolved with 1 ml acetonitrile, filtered through 0.45 μm microporous membrane, separated on C18 column at 30℃with acetonitrile- water as mobile phase at a flow rate of 1 ml/min for gradient elution, and detected by FLD. The sample quantification was carried out by internal standard method, while the qualitative analysis was carried out by retention time. Results The 9 biogenic amines showed good linearity in range of 1 ..0 mg/L ~ 75.0 mg/L. The detection limit was 0.06 mg/kg ~ 0.71 mg/kg, the recoveries were between 80% ~ 121%, the RSDs were between 0.69% - 2.36%. Conclusion This method is simple, accurate, reliable and it can simulta- neously determine the content of nine biogenic amines in yellow rice wine.
出处
《中国卫生检验杂志》
CAS
北大核心
2014年第6期761-764,共4页
Chinese Journal of Health Laboratory Technology
基金
福建省疾病预防控制中心青年科研课题(2011-10)
