【摘要】 目的 基于在线固相萃取与液相色谱-串联质谱技术，以在线SPE柱净化、C18色谱柱分离、三重四极杆质谱检测为核心，构建一种婴幼儿配方乳粉及其花生四烯酸原料中蜡样芽胞杆菌呕吐毒素的分析方法，并将其应用于实际样品中目标毒素的定量测定。方法 称取1.00 g试样，加入同位素内标，加入10 mL 70%乙腈溶液，经振荡提取、低温离心处理，取上清液经滤膜过滤，将滤液进行在线SPE净化。以0.1%甲酸的水溶液和0.1%甲酸乙腈为流动相实施梯度洗脱，选用NanoChrom ChromCore 300 C18(3.0 mm×100 mm,3??m)作为色谱分析柱，在电喷雾正离子（ESI~+）多反应监测模式下进行检测，采用内标法定量分析。结果 在0.010～5.0??g/L浓度范围内线性关系良好，相关系数达0.999 9，检出限为0.030??g/kg，定量限为0.10??g/kg，加标回收率为98.5%～106.0%，相对标准偏差为0.96%～2.73%，测定结果与传统离线固相萃取法无显著性差异。结论 方法操作简便、灵敏度高、抗基质干扰能力强，可作为高效检测手段用于婴幼儿配方乳粉及其原辅料中蜡样芽胞杆菌呕吐毒素的食品安全风险监测与质量管控。更多还原

【Abstract】 Objective A analytical method for the determination of cereulide produced by Bacillus cereus in infant formula and its arachidonic acid raw materials was developed based on online solid-phase extraction(SPE) coupled with liquid chromatography-tandem mass spectrometry. The method utilized online SPE column for purification, C18 chromatographic column for separation, and triple quadrupole mass spectrometry for detection. It was subsequently applied to the quantitative determination of the target toxin in real samples.Methods A 1. 00 g test portion was weighed, and isotope-labeled internal standards were added. After the addition of 10 mL of 70% acetonitrile solution, the mixture was extracted by shaking and subjected to low-temperature centrifugation. The supernatant was filtered through a membrane, and the filtrate was purified by online SPE. Gradient elution was carried out using mobile phases consisting of 0. 1% formic acid in water and 0. 1% formic acid in acetonitrile. Chromatographic separation was performed on a NanoChrom ChromCore 300 C18 column(3. 0 mm×100 mm, 3 ??m). Detection was conducted in electrospray positive ionization(ESI~+) mode under multiple reaction monitoring(MRM), and quantification was achieved using the internal standard method.Results Excellent linearity was observed over the concentration range of 0. 010-5. 0 ??g/L, with a correlation coefficient of 0. 999 9. The limit of detection and quantification were 0. 030 ??g/kg and 0. 10 ??g/kg, respectively. The average recoveries ranged from 98. 5% to 106. 0%, with relative standard deviations between 0. 96% and 2. 73%. No significant difference was observed between this method and conventional offline solid-phase extraction method.Conclusion This method is simple, sensitive, and demonstrates strong resistance to matrix interference. It can be employed as an efficient analytical tool for the food safety risk monitoring and quality control of B. cereus emetic toxin in infant formula and its raw and auxiliary materials.更多还原