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

October 2024

Article Contents

LI Min, HE Shanshan and YANG Yuwen. Determination of heterocyclic aromatic amines in ham sausage by modified quEChERS method combined with ultra-high performance liquid chromatography[J]. Journal of Light Industry, 2024, 39(5): 60-70. doi: 10.12187/2024.05.007

Citation: LI Min, HE Shanshan and YANG Yuwen. Determination of heterocyclic aromatic amines in ham sausage by modified quEChERS method combined with ultra-high performance liquid chromatography[J]. Journal of Light Industry, 2024, 39(5): 60-70. doi: 10.12187/2024.05.007 shu

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

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

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