红烧乳鸽中11种极性杂环胺的UHPLC-Q-Orbitrap HRMS检测

Determination of 11 polar heterocyclic aromatic amines in braised squab By UHPLC-Q-Orbitrap HRMS

以市售红烧乳鸽为研究对象,建立超高效液相色谱-四极轨道高分辨质谱(UHPLC-Q-Orbitrap HRMS)联用法,并对红烧乳鸽样品中不同部位11种极性杂环胺含量进行检测。结果表明:建立的方法线性关系良好、灵敏度较高,11种杂环胺的质量准确度均<3×10^(-6),决定系数R^(2)≥0.9972,方法的检出限为0.03~0.60μg/kg,方法的定量限为0.10~2.00μg/kg;该方法具有稳定的回收率和一定的精确性,11种杂环胺的回收率分布在为83.40%~114.80%,精密度为1.40%~7.20%之间,结果良好;红烧乳鸽中主要检出MeIQx(0.10~0.46μg/kg)、PhIP(0.10~0.53μg/kg)和DMIP(0.10~0.25μg/kg)3种杂环胺,乳鸽部位中HAAs总含量由多到少依次为鸽跟>鸽胸>鸽翅>鸽腿。

With commericially available braised squab as research object,UHPLC-Q-Orbitrap HRMS was established.Eleven polar heterocyclic aromatic amines in braised squab were detected by UHPLC-Q-Orbitrap HRMS.The results showed that the method had good linearity and high mass accuracy.The mass accuracy of 11 heterocyclic aromatic amines was<3×10^(-6).Linearities of IQ and MeIQ in 0.5~50μg/L,of IFP in 2.0~100μg/L,and of the other eight heterocyclic aromatic amines in of 0.5~100μg/L and 0.1~100μg/L were good,respectively.The determination coefficients were greater than 0.9972.The limit of detection was 0.03~0.60μg/kg,and the limit of quantification was 0.10~2.00μg/kg.This method had stable recovery and certain accuracy.The recovery of 11 HAAs heterocyclic aromatic amines at 3 spiked concentrations ranged from 83.40%to 114.80%,and the precision ranged from 1.40%to 7.20%.The main heterocyclic aromatic amines detected in braised squab were MeIQx(0.10~0.46μg/kg),PhIP(0.10~0.53μg/kg)and DMIP(0.10~0.25μg/kg).The total content of heterocyclic aromatic amines in squab’s skin was significantly higher than that in squab’s meat and the content of heterocyclic aromatic amines in squab’s heel was highest.The established SPE-UHPLC-Q-Orbitrap HRMS method is in high sensitivity,being accurate and reliable in results,and can be used for the determination of HAAs in braised squab.4 parts of braised squab was the heel,breast,wing and leg in descending oder.