食品科学 ›› 2025, Vol. 46 ›› Issue (15): 346-324.doi: 10.7506/spkx1002-6630-20250311-080

• 安全检测 • 上一篇    下一篇

全自动分散固相萃取-超高效液相色谱-串联质谱法测定方便食品中28 种食源性代谢调节剂

黄芊,冯丽凤,叶梦薇,王春,黄力群,潘城   

  1. (福建省产品质量检验研究院,国家加工食品质量检验检测中心,福建 福州 350002)
  • 出版日期:2025-08-15 发布日期:2025-07-22
  • 基金资助:
    福建省产品质量检验研究院科技项目(KY202317A)

Simultaneous Determination of 28 Food-Derived Metabolic Modulators in Instant Foods by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry with Automatic Dispersive Solid Phase Extraction

HUANG Qian, FENG Lifeng, YE Mengwei, WANG Chun, HUANG Liqun, PAN Cheng   

  1. (National Quality Supervision and Testing Center for Processed Food, Fujian Inspection and Research Institute for Product Quality, Fuzhou 350002, China)
  • Online:2025-08-15 Published:2025-07-22

摘要: 针对方便食品中原料残留、非法添加等因素导致的食源性代谢调节剂污染风险与现有检测技术基质不匹配、风险覆盖面小、分析过程复杂等局限,建立全自动分散固相萃取法净化-超高效液相色谱-串联质谱快速测定方便食品中28 种食源性代谢调节剂的分析方法。样品经全自动QuEChERS实验仪以0.1%甲酸乙腈提取,基质分散固相萃取法净化前处理后,Shimadzu Shim-pack GIST C18-AQ色谱柱(2.1 mm×100 mm,1.9 μm)分离,电喷雾离子源正、负离子同时扫描,多反应监测模式采集,外标法定量。在优化的条件下,28 种食源性代谢调节剂在各自的线性范围内线性关系良好,决定系数(R2)均大于0.994,方法检出限在0.05~2.0 μg/kg之间,方法定量限为0.1~5.0 μg/kg。在谷物蛋白棒和面包2 种基质中的平均回收率为63.4%~112.0%,相对标准偏差为1.4%~17.7%(n=6)。该方法具有自动化程度高、分析速度快、高灵敏度、准确、稳定等特点,可满足方便食品中28 种食源性代谢调节剂的快速筛查需求。

关键词: 食源性代谢调节剂;方便食品;全自动分散固相萃取;超高效液相色谱-串联质谱法

Abstract: In view of the contamination risk of food-derived metabolic modulators caused by factors such as their residues in food raw materials and their illegal addition in instant foods, as well as the limitations of existing detection technologies such as mismatched matrix, small risk coverage, and complex analysis processes, an analytical method for the rapid determination of 28 food-derived metabolic modulators in instant foods was developed using automatic dispersive solid phase extraction (auto-dSPE) coupled with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were extracted with 0.1% formic acid in acetonitrile, purified by matrix solid-phase dispersion extraction (MSPD), and separated by on a Shimadzu Shim-pack GIST C18-AQ column (2.1 mm × 100 mm, 1.9 μm). Detection was performed using electrospray ionization (ESI) in both positive and negative ion modes. Data acquisition was performed using multiple reaction monitoring (MRM) and quantitation of each analyte was carried out using an external standard method. Under the optimal conditions, the 28 metabolic modulators had good linear relationship in their respective concentration ranges, with determination coefficients (R2) greater than 0.994. The detection limit of the developed method was between 0.05 and 2.0 μg/kg, and the quantification limit was between 0.1 and 5.0 μg/kg. The average recoveries from cereal protein bar and bread ranged from 63.4% to 112.0%, with relative standard deviations (RSDs) ranging from 1.4% to 17.7% (n = 6). This method was characterized by high automation, fast analysis speed, high sensitivity, accuracy and stability, and could meet the demand for rapid screening of the 28 food-derived metabolic modulators in instant foods.

Key words: food-derived metabolic regulators; instant foods; fully automatic dispersive solid phase extraction; ultra-high performance liquid chromatography-tandem mass spectrometry

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