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
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摘要: 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R2≥0.997 2,方法的检出限为0.03~0.60 μg/kg,定量限为0.10~2.00 μg/kg;该方法具有稳定的回收率和一定的精确性,11种杂环胺的回收率为83.40%~114.80%,精密度为1.40%~7.20%,结果良好;红烧乳鸽中主要检出MeIQx(0.10~0.46 μg/kg)、PhIP(0.10~0.53 μg/kg)和DMIP(0.10~0.25 μg/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。
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关键词:
- 杂环胺 /
- 红烧乳鸽 /
- 超高效液相色谱-四极轨道高分辨质谱联用法
Abstract: 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. The determination coefficients were greater than 0.997 2. The limit of detection was 0.03~0.60 μg/kg, and the limit of quantification was 0.10~2.00 μg/kg. This method had stable recovery and certain accuracy. The recovery of 11 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 (0.10~0.46 μg/kg), PhIP (0.10~0.53 μg/kg) and DMIP (0.10~0.25 μg/kg). The total content of heterocyclic aromatic amines in 4 parts of braised squab was the heel, breast, wing and leg in descending oder. -
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