Study On Ten Biogenic Amines Determination In Food By Capillary Liquid Chromatography

Biogenic amines (BAs), existing in plants, animals and microorganisms at low levels, are one kind of organic compounds with low molecular weight. High levels of BAs can cause some harmful effects such as headache, nausea, hypertension, cardiac palpitations and renal intoxication. Therefore, establishing a method for BAs content detection with high accuracy and sensitivity has great significance.In this research, we optimized relative experimental parameters including the BAs derivation procedure, separation procedure of capillary liquid chromatography (CLC) and the purification and extraction conditions of ten BAs in food matrix and established a method for BAs detection by combining solid phase extraction with CLC using cigarette filter as SPE adsorbent material.The results showed that the employed cigarette filter fibers had good adsorption ability for BAs dansylamides. Through single factor variable test, the parameters affecting SPE extraction efficiency were optimized and established as follows:sample loading solution pH:7.0; washing solution:acetone/water (1:9, v/v); the eluent:mixed methanol and ethyl acetate solution (8:2, v/v); eluent volume:6.0mL. Furthermore, an optimal gradient elution procedure of CLC separation to separate the amines under the flow rate of10.0uL/min was analyzed. A ZORBAX XDB-C18column (150×0.5mm,3.5μm) was chose to separate the analytes using a mobile phase of water (A) and acetonitrile (B) with the gradient elute. The injection volume and column temperature were set up at1μL and35℃, respectively. All analytes were baseline separated with better peak symmetry. Good linearity of ten BAs was obtained with r2>0.999in the range of0.01-40mg/L with the instrumental LODs of0.001-0.03mg/L. The established method was applied to evaluate meat and aquatic samples (pork, beef, codfish and squid) with the methodology LODs of0.002-0.05mg/L. The recoveries of the ten BAs at three levels of0.5,1.0,5.0mg/kg achieved to71.3%-128.3%with relative standard deviations (RSDs) of1.9%-20.1%, indicating the developed method can offer an accurate and sensitive quantification analysis of ten BAs in complex biological samples.