高效液相色谱-四极杆-飞行时间质谱法高通量筛查功能食品中48种镇静助眠类化合物

High-throughput screening of 48 kinds of sedative-hypnotic compounds in functional foods by high performance liquid chromatography- quadrupole-time-of-flight mass spectrometry

中文关键词:  镇静助眠化合物  高效液相色谱-四级杆-飞行时间质谱  功能食品  高通量

英文关键词:sedative-hypnotic compounds  high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry  functional foods  high-throughput

中文摘要:

      目的 建立高效液相色谱-四极杆-飞行时间质谱法筛查功能食品中非法添加的镇静助眠类化合物的方法。方法 样品经乙腈或1%氨水乙腈(体积分数)提取, 使用50 mg N-丙基乙二胺和150 mg 无水硫酸镁净化处理, 通过Waters BEH C18色谱柱(2.1 mm×100 mm, 1.7 μm)分离。质谱采用正负离子切换扫描模式, 结合一级全扫描/数据依赖的二级扫描策略, 并基于建立的镇静助眠类化合物多级数据库, 实现对目标化合物的高通量定性筛查和分析。结果 镇静助眠类化合物在10~600 μg/kg的浓度范围内线性关系良好, 相关系数均大于等于0.99, 定量限为20~50 μg/kg。在压片糖果、液体饮料和混合乳粉中, 平均加标回收率(质量分数)分别为51.03%~119.92%、53.36%~115.46%和51.89%~116.79%; 相对标准偏差为1.19%~9.75%、1.27%~9.93%和1.24%~9.52%。实际样品筛查中, 褪黑素的检出率为22%。结论 该方法操作便捷、灵敏度高, 适用于不同种类食品中非法添加的镇静助眠类化合物的测定, 为食品安全监管提供了有力的技术支持。

英文摘要:

      Objective To establish a method for screening illegally added sedative-hypnotic compounds in functional foods by high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry. Methods Samples were extracted with acetonitrile or 1% ammonia-acetonitrile (by volume fraction), purified with 50 mg N-propylethylenediamine and 150 mg anhydrous magnesium sulfate, and separated using a Waters BEH C18 column (2.1 mm×100 mm, 1.7 μm). The mass spectrometry analysis was performed in positive and negative ion switching scan mode, combined with full-scan primary mass spectrometry and data-dependent tandem mass spectrometry acquisition. Based on the established multilevel database of sedative-hypnotic compounds, high-throughput qualitative screenings and analysis of the target compounds were achieved. Results All sedative-hypnotic compounds showed good linear relationships in the concentration range of 10–600 μg/kg, with correlation coefficients all greater than 0.99, and the limits of quantitation ranged from 20 to 50 μg/kg. In compressed candies, liquid beverages and mixed milk powders, the average spiked recoveries (mass fraction) were 51.03%–119.92%, 53.36%–115.46% and 51.89%–116.79%, respectively; the relative standard deviations were 1.19%–9.75%, 1.27%–9.93% and 1.24%–9.52%, respectively. In the screening of actual samples, the detection rate of melatonin was 22%. Conclusion The proposed method is simple to operate, highly sensitive, and it is applicable for determining illegally added sedative-hypnotic compounds in diverse food matrices, providing robust technical support for food safety supervision.