HPLC-Q-Orbitrap-HRMS方法检测广式烧鹅中7种非极性杂环胺
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(1.仲恺农业工程学院轻工食品学院 广东省岭南特色食品科学与技术重点实验室 现代农业工程创新研究院农业农村部岭南特色食品绿色加工与智能制造重点实验室 广州 510225;2.广州质量监督检测研究院 食品安全预警研发中心 广州 510447)

作者简介:

董浩(1989—),男,博士,副教授

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基金项目:

广东省普通高校重点领域专项(2020ZDZX1015);国家自然科学基金青年科学基金项目(32001729);广东省联合培养研究生示范基地项目(仲恺-广州质量监督检测研究院);广东省重点领域研发计划项目(2020B0202080002)


Determination of 7 Nonpolar Heterocyclic Aromatic Amines in Cantonese Roast Goose by HPLC-Q-Orbitrap-HRMS
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(1.Key Laboratory of Green Processing and Intelligent Manufacturing of Lingnan Specialty Food, Ministry of Agriculture and Rural Affairs, Academy of Contemporary Agricultural Engineering Innovations, Guangdong Provincial Key Laboratory of Lingnan Specialty Food Science and Technology, College of Light Industry and Food Sciences, Zhongkai University of Agriculture and Engineering, Guangzhou 510225;2.Food Safety Early Warning R&D Center, Guangzhou Quality Supervision and Testing Institute, Guangzhou 510447)

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    摘要:

    广式烧鹅在高温烧制过程中极易产生杂环胺,因此对其中杂环胺的检测和含量监控尤为重要。为建立一种基于高效液相色谱-四极轨道高分辨质谱联用技术(HPLC-Q-Orbitrap-HRMS)检测中国传统美食广式烧鹅中7种杂环胺的方法,样品用NaOH-乙腈溶液均质,可实现样品中油脂的皂化水解和目标杂环胺的提取。通过StartaTM-X-C固相萃取小柱净化提取液后,采用C18色谱柱进行分离,以乙腈和含0.05%甲酸的1 mmol/L乙酸铵溶液为流动相梯度洗脱,在电喷雾正离子、全扫描和数据依赖性扫描的模式下检测,以保留时间、一级离子质量准确度、二级碎片与库匹配准确定性,用内标法结合一级离子峰面积进行定量。结果表明:7种杂环胺的质量精确度<3.0×10-6,在0.100~100 μg/L范围有良好的线性关系,相关系数R2>0.997。方法检出限介于0.02~0.15 μg/kg之间,定量限介于0.05~0.5 μg/kg之间。加标回收率结果表明,在3种加标浓度下7种杂环胺的回收率良好。建立的HPLC-Q-Orbitrap-HRMS检测方法灵敏度高,结果准确可靠,可应用于广式烧鹅中非极性杂环胺的检测。

    Abstract:

    It is of significance to detect and monitor the heterocyclic aromatic amines (HAAs) contents in Cantonese roast goose because they are very easy to be formed in the high-temperature processing. In order to develop a method on the basis of high-performance liquid chromatography coupled to quadrupole orbitrap high-resolution mass spectrometry (HPLC-Q-Orbitrap HRMS) for the determination of 7 HAAs in Cantonese roast goose, one of the traditional Chinese food, samples were homogenized with NaOH-acetonitrile solution, which could achieve saponification hydrolysis of oil in the samples and extraction of target HAAs. The extraction solution was purified by StrataTM-X-C solid phase extraction cartridge, separated on a C18 column by gradient elution with mobile phase consisting of acetonitrile and 1 mmol/L ammonium acetate containing 0.05% formic acid, detected by electrospray positive ion, full scan and data-dependent scan modes. Retention time, accuracy of primary ion mass in combination with matching of secondary fragments to the library was used for qualitative analysis, and the internal standard method combined with the peak area of primary ion was used for quantitative analysis of HAAs. Results showed that the mass accuracy of the target HAAs was less than 3×10-6, with good linearity in the range of 0.100-100 μg/L, and the correlation coefficients were greater than 0.997. The limits of detection and limits of quantification were 0.02-0.15 μg/kg and 0.05-0.5 μg/kg, respectively. Recoveries of 7 HAAs were good at three spiked concentrations. The established HPLC-Q-Orbitrap HRMS method has high sensitivity, accurate and reliable results, and can be applied to detecting nonpolar HAAs in Cantonese roast goose.

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董浩,黄俊源,何昀桐,冼燕萍,白卫东,曾晓房. HPLC-Q-Orbitrap-HRMS方法检测广式烧鹅中7种非极性杂环胺[J].中国食品学报,2022,22(10):295-302

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  • 收稿日期:2021-10-31
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  • 在线发布日期: 2022-11-24
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