改良QuEChERS方法结合超高效液相色谱测定火腿肠中杂环胺类化合物

李敏; 贺姗姗; 杨钰雯

doi:10.12187/2024.05.007

改良QuEChERS方法结合超高效液相色谱测定火腿肠中杂环胺类化合物

郑州轻工业大学食品与生物工程学院, 河南郑州 450001

作者简介: 李敏(1989—),女,河南省宁陵县人,郑州轻工业大学讲师,博士,主要研究方向为食品安全检测与控制。E-mail:2017074@zzuli.edu.cn;

基金项目: 河南省科技攻关项目(242102111066)
中图分类号: TS262.6

Determination of heterocyclic aromatic amines in ham sausage by modified quEChERS method combined with ultra-high performance liquid chromatography

College of Food and Bioengineering, Zhengzhou University of Light Industry, Zhengzhou 450001, China
Received Date: 2024-01-13
Accepted Date: 2024-03-22
Available Online: 2024-10-15
CLC number: TS262.6

摘要: 以火腿肠为研究对象,建立以磁性氧化石墨烯为基质净化材料的改良QuEChERS方法,结合超高效液相色谱(UPLC)技术快速测定火腿肠中4种杂环胺(IQ、Harman、Norharman和Phe-P-1)含量,利用方法学考查该方法的分析性能,并将其用于实际样品的检测。结果表明,与传统净化材料相比,所合成的磁性氧化石墨烯材料具有更高或相当的杂环胺回收效果和基质净化能力,可用作改良QuEChERS方法的净化材料。改良QuEChERS方法的适宜条件为:提取溶剂为碱化乙腈(含体积分数1%的氨水)、用水量1 mL、涡旋萃取时间5 min、萃取盐为无水Na₂SO₄/NaCl(用量0.50 g/0.13 g)、离心时间3 min,磁性氧化石墨烯用量7.5 mg、净化时间1 min。该条件下,4种杂环胺的R²均大于0.999 5,在低、中、高浓度3个加标水平下杂环胺的回收率分别为99.9%~104.3%、101.2%~106.7%和85.7%~101.2%,检出限和定量限分别为0.71~1.52 ng/g和1.00~2.53 ng/g,日内及日间精密度分别低于4.4%和4.9%,精确度和精密度均良好。11种市售火腿肠均未检出4种HAAs,但检测到多种未知物质,且其含量均高于本文方法的定量限。与其他常用前处理技术相比,本文方法具有快速、简便、单样品成本低、有机溶剂用量少等特点,可用于火腿肠中杂环胺的检测。
- QuEChERS /
- UPLC /
- 磁性氧化石墨烯 /
- 火腿肠 /
- 杂环胺
Abstract: A modified QuEChERS method using magnetic graphene oxide as purification material was developed to determine four heterocyclic aromatic amines (IQ, Harman, Norharman and Phe-P-1) in ham sausage by ultra-high performance liquid chromatography (UPLC). Analytical performance of this method was evaluated through methodological validation and applied to the detection of real samples. The results showed that compared with traditional purification materials, the prepared magnetic graphene oxide displayed considerable abilities of matrix purification and achieved satisfactory HAAs recoveries, which could be used as the purification material in the modified QuEChERS method. The optimal conditions for the modified QuEChERS method were as follows: alkaline acetonitrile (containing ammonium hydroxide with volume fraction of 1%) was used as the extraction solvent, the volume of water was 1 mL, the vortex extraction time was 5 min, the combination of anhydrous sodium sulfate/sodium chloride was chosen as the extraction salt with the dosage of 0.50 g/0.13 g, the centrifugation time was 3 min, the dosage of magnetic graphene oxide was 7.5 mg and the purification time was 1 min. Under these conditions, all the correlation coefficients (R²) for the targeted HAAs were greater than 0.9995. The recoveries of four HAAs at three spiked levels (low, medium and high) were 99.9%~104.3%, 101.2%~106.7% and 85.7%~101.2%, respectively. The limit of detection (LOD) was 0.71~1.52 ng/g. The limit of quantification (LOQ) ranged from 1.00 ng/g to 2.53 ng/g. The intra-day and inter-day precisions were less than 4.4% and 4.9% with good accuracy and precision. The four HAAs were not detected in any of the tested ham sausages. However, some unknown substances were found and their contents were higher than the LOQ of the established QuEChERS method. Compared with other commonly used sample pretreatment techniques, this method had advantages of speed, simplicity, low cost per sample and less organic solvents, which was suitable for the determination of HAAs in ham sausage.
- QuEChERS /
- UPLC /
- magnetic graphene oxide /
- ham sausage /
- heterocyclic aromatic amines
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沈阳化工大学材料科学与工程学院沈阳 110142

改良QuEChERS方法结合超高效液相色谱测定火腿肠中杂环胺类化合物

作者简介: 李敏(1989—),女,河南省宁陵县人,郑州轻工业大学讲师,博士,主要研究方向为食品安全检测与控制。E-mail:2017074@zzuli.edu.cn;

Determination of heterocyclic aromatic amines in ham sausage by modified quEChERS method combined with ultra-high performance liquid chromatography

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通讯作者: 陈斌, bchen63@163.com

改良QuEChERS方法结合超高效液相色谱测定火腿肠中杂环胺类化合物

作者简介:李敏(1989—),女,河南省宁陵县人,郑州轻工业大学讲师,博士,主要研究方向为食品安全检测与控制。E-mail:2017074@zzuli.edu.cn

English Abstract

Determination of heterocyclic aromatic amines in ham sausage by modified quEChERS method combined with ultra-high performance liquid chromatography

目录

改良QuEChERS方法结合超高效液相色谱测定火腿肠中杂环胺类化合物

作者简介: 李敏(1989—),女,河南省宁陵县人,郑州轻工业大学讲师,博士,主要研究方向为食品安全检测与控制。E-mail:2017074@zzuli.edu.cn;

Determination of heterocyclic aromatic amines in ham sausage by modified quEChERS method combined with ultra-high performance liquid chromatography

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通讯作者: 陈斌, bchen63@163.com

改良QuEChERS方法结合超高效液相色谱测定火腿肠中杂环胺类化合物

作者简介:李敏(1989—),女,河南省宁陵县人,郑州轻工业大学讲师,博士,主要研究方向为食品安全检测与控制。E-mail:2017074@zzuli.edu.cn

English Abstract

Determination of heterocyclic aromatic amines in ham sausage by modified quEChERS method combined with ultra-high performance liquid chromatography

目录