Applied Technology Center, Pacific Regional Laboratory Northwest, Office of Regulatory Affairs, U.S. Food and Drug Administration, 22201 23rd Drive S.E., Bothell, Washington 98021, USA.
J Agric Food Chem. 2011 Jun 8;59(11):5906-13. doi: 10.1021/jf200455r. Epub 2011 May 10.
A method for the extraction of agmatine, cadaverine, histamine, phenyethylamine, putrescine, tryptamine, tyramine, and urocanic acid from canned tuna and frozen tuna loin matrices by matrix solid-phase dispersion, followed by separation and quantification of these compounds by ultrahigh-performance hydrophilic interaction chromatography (UHPLC-HILIC) with orbitrap mass spectrometric detection, is described. Tuna samples are dispersed in a CN-silica sorbent and eluted with a mixture of aqueous ammonium formate buffer and acetonitrile. Separation and detection are carried out on an Agilent 1200 high-performance liquid chromatograph coupled to a Thermo Exactive orbitrap mass spectrometer, and metformin is used as the internal standard. Spike recoveries are determined across a range of 20-100 ppm for each compound, and the method is validated with respect to linearity, reproducibility, accuracy, and limits of quantitation and detection. The method is demonstrated to be suitable for use in quantifying these target compounds in the studied matrices.
一种从金枪鱼罐头和冷冻金枪鱼腰肉基质中提取腐胺、尸胺、组氨酸、苯乙胺、精胺、色胺、酪胺、尿刊酸的方法，采用基质固相分散法，然后通过超高效亲水相互作用色谱（UHPLC-HILIC）与轨道阱质谱检测对这些化合物进行分离和定量。金枪鱼样品分散在 CN-硅胶吸附剂中，用甲酸铵缓冲液和乙腈的混合物洗脱。分离和检测在安捷伦 1200 高效液相色谱仪与热电 Exactive 轨道阱质谱仪上进行，二甲双胍用作内标。对每种化合物的 20-100ppm 范围内进行了加标回收率的测定，并对该方法进行了线性、重现性、准确性和定量限及检测限的验证。该方法适用于定量分析研究基质中这些目标化合物。
