固相萃取结合超高效液相色谱-串联质谱法测定新疆特色食品中的丙烯酰胺
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作者单位:

克拉玛依市疾病预防控制中心,新疆 克拉玛依 834000

作者简介:

徐曼 女 实验师 研究方向为食品理化检测 E-mail:1182519600@qq.com

通讯作者:

吴德 男 主任医师 研究方向为食品安全检测和质量控制 E-mail:1547755155@qq.com

中图分类号:

R155

基金项目:

新疆维吾尔自治区卫生健康青科项目(WJWY-202307)


Determination of acrylamide in Xinjiang specialty foods by solid phase extraction combined with ultra-high performance liquid chromatography-tandem mass spectrometry
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Karamay City Center for Disease Control and Prevention, Xinjiang Karamay 834000, China

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    摘要:

    目的 建立一种固相萃取结合超高效液相色谱-串联质谱法测定新疆特色食品(馕、馓子、烤包子及油香)中丙烯酰胺的分析方法。方法 以水-乙腈为提取溶剂,正己烷为去脂溶剂,对样品进行涡旋振荡提取,离心后取下层溶液通过MCX固相萃取柱净化,净化液经氮吹浓缩、纯水复溶后测定。采用水-甲醇为流动相梯度洗脱,ACQUITY UPLC HSS T3(100 mm×2.1 mm,1.8 μm)柱分离,串联质谱同位素内标法定性定量。结果 该方法在1.0~200 ng/mL范围内线性良好(r2=0.999 5);在4种食品中,定量限介于0.19~0.31 μg/kg之间;3个浓度水平的加标回收率为89.5%~99.4%,相对标准偏差(n=6)为1.8%~6.4%。结论 本方法提取溶剂消耗量小,操作简便,净化效果好,结果准确,适合新疆特色食品中丙烯酰胺的测定。

    Abstract:

    Objective A method for determination of acrylamide in Xinjiang specialty foods (naan products, rice dumplings, roasted buns and oil incense) by solid phase extraction combined with ultra-high performance liquid chromatography-tandem mass spectrometry was established.Methods Using water-acetonitrile as the extraction solvent and n-hexane as the degreasing solvent, the sample was extracted by vortex oscillation. After centrifugation, remove the layer solution and purify it through MCX solid phase extraction column. The purified liquid was concentrated by nitrogen blowing and measured after resolvation with pure water. Water-methanol was used as the mobile phase for gradient elution, ACQUITY UPLC HSS T3 (100 mm×2.1 mm, 1.8 μm) column separation, and tandem mass spectrometry isotope internal standard method for qualitative quantification.Results The method has good linearity in the range of 1.0-200 ng/mL (r2=0.999 5). Among the four foods, the standard recovery rate of the three concentration levels were 89.5%-99.4%, and the relative standard deviation (n=6) were 1.8%-6.4%.Conclusion This method has low consumption of solvent extraction, easy operation, good purification effect, accurate results, which is suitable for the determination of acrylamide in Xinjiang specialty foods.

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徐曼,王银,宋少龙,胡俊,吴德.固相萃取结合超高效液相色谱-串联质谱法测定新疆特色食品中的丙烯酰胺[J].中国食品卫生杂志,2024,36(11):1226-1233.

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  • 收稿日期:2024-06-27
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  • 在线发布日期: 2025-03-14
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