摘要
采用改进的QuEChERS方法,利用液相色谱-串联质谱(RPLC—TMS)检测,建立了几种水产品中生物胺的分析方法。样品用乙腈+甲醇(9+1)提取,无水硫酸钠除去水分,经乙二胺-N-丙基硅烷(PSA)和C18混合粉末净化,采用HILIC柱,以乙腈/1%甲酸水溶液为流动相梯度洗脱进行液相色谱分离。质谱分析采用电喷雾正离子电离,多反应监测模式,外标法定量。结果显示6种生物胺在10~200ng/mL范围线性关系良好。方法的定量限(LOQ,信噪比为10)为0.10mg/kg。加标水平在0.10mg/kg时,鱼、虾、蟹及鱿鱼四种阴性基质中加标的回收率在74.18%~90.15%之间,相对标准偏差(RSD,11=6)在2.22%~8.04%之间。结果表明本方法简便、快速、安全、适用于水产品中生物胺含量的定性和定量检测。
A modified QuEChERS method followed by liquid chromatography-tandem mass spectrometric analysis was developed for the determination of biogenic amines in aquatic products. The samples was diluted with acetonitrile/methanol solution (9/1)and cleaned up with primary secondary amine (PSA)and Octadecylsilane (C18) sorbent.The separation of biogenic amines was performed by hydrophilic interaction liquid chromatography (HILIC) column and gradiently eluting with acetonitrile/formic acid- water (1%) without derivatization. Biogenic amines were analyzed by positive electrosprary ionization (ESI^+) tandem mass spectrometry under multiple reaction monitoring(MRM)mode.Quantification was achieved using external standard method.The linearities were excellent in the range of 10-200 ng/mL.The limits of quantification( LOQ,S/N = 10)were 0.10 mg/kg.The recoveries of biogenic amines spiked in matrices were between 74.18% and 90.15% at the spiked levels of 0.10 mg/kg.The relative standard deviations ( RSDs, n = 6) were in the range of 2.22% -8.04%.The method ( quick, easy, safe) could meet the requirements of the daily work for the determination of biogenic amines in aquatic products.
出处
《食品工业科技》
CAS
CSCD
北大核心
2016年第22期68-72,79,共6页
Science and Technology of Food Industry
基金
海南省自然科学基金项目(313105)
海南省科技兴海项目(XH201407)