摘要
试验采用柱后衍生阳离子交换色谱技术建立同时测定动物源性饲料原料及饲料中组胺、腐胺、尸胺、亚精胺、精胺和酪胺的分析方法。样品以2%磺基水杨酸溶液提取,4%磺基水杨酸溶液和二氯甲烷净化提取样液,采用氨基酸分析仪用阳离子交换色谱柱(LCA K17)、以柠檬酸K液为流动相分离6种生物胺,茚三酮溶液衍生后,可见光检测器于570 nm条件下测定。结果显示,6种生物胺在2~100μmol/L浓度范围内具有良好的线性,相关系数均大于0.999;方法的检出限为5.0 mg/kg,定量限为10.0 mg/kg;3个加标水平的回收率在83.46~111.34%,加标含量范围为25.0~1 000.0 mg/kg,相对标准偏差(RSD,n=6)在0.38%~5.13%。研究表明,此方法的回收率高、选择性好,可应用于动物源性饲料原料及饲料中生物胺的测定。
A method for the determination of histamine, putrescine, cadaverine, spermidine, spermine, tyramine in animal-derived feed ingredients and feeds was established by post-column derivatization with cation exchange chromatography. The samples were extracted with 2% sulfosalicylic acid solution, and purified with 4% sulfosalicylic acid solution and dichloromethane. The six biogenic amines were separated by the amino acid analyzer using cationic exchange column(LCA K17) with the mobile phases of potassium citrate buffers. The separated biogenic amines solutions were derived with ninhydrin solution, and the derivatives were detected by the visible light detector at 570 nm. The results showed that the linearities were excellent in the range of 2~100 μmol/L with the correlation coefficients above 0.999. The limits of detection of method were 5.0 mg/kg, and the limits of quantification were 10.0 mg/kg. The recoveries of biogenic amines were between 83.46% and 111.34% at the spiked levels ranged from 25.0 mg/kg to 1 000.0 mg/kg. The relative standard deviations(RSD, n=6) were in the ranges of 0.38%~5.13%. The experiment indicates that the method has high recovery and good selectivity, which can be applied to the determination of biogenic amines in animal feed materials and feed.
作者
李欣欣
梁玉树
刘尚群
何开蓉
熊安琪
周桂莲
李勇
乔煦玮
LI Xin-xin;LIANG Yu-shu;LIU Shang-qun;HE Kai-rong;XIONG An-qi;ZHOU Gui-lian;LI Yong;QIAO Xu-wei
出处
《饲料研究》
CAS
北大核心
2022年第1期124-129,共6页
Feed Research
关键词
阳离子交换色谱
柱后衍生
生物胺
饲料
cation exchange chromatography
post-column derivatization
biogenic amines
feed
