This work describes a simple screening protocol for quantification of carbasalate calcium derived metabolites, acetylsalicylic acid (ASA) and salicylic acid (SA), in animal and aquatic food matrices using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The analytes were extracted from porcine muscle, milk, egg, shrimp, eel, and flatfish using acetonitrile, with the addition of formic acid as well as trifluoroacetic acid, followed by liquid-liquid purification with saturated n-hexane. A reverse-phase analytical column was employed with a mobile phase comprising (A) 1 mM ammonium acetate in distilled water and (B) methanol to achieve the best chromatographic separation. Matrix-matched calibration curves (R² ≥ 0.9817) were constructed using six concentrations of 5, 10, 20, 30, 40, and 50 µg/kg in porcine muscle, milk, egg, shrimp, eel, and flatfish matrices. The calculated limits of quantification (LOQ) were 10 and 7 µg/kg, for ASA and SA, respectively. Recoveries of 67 to 102% with relative standard deviations (RSDs) of ≤9.0% (intra-day and inter-day) were obtained for all matrices at four spiking concentrations (5, 10, 20, and 50 µg/kg). The method was feasibly applied for monitoring market samples. In conclusion, the developed method is versatile, accurate, and precise for detecting and quantifying acetylsalicylic acid and salicylic acid residues in animal-derived foods meant for human consumption.

这项工作描述了一种简单的筛选方案，用于使用液相色谱-串联质谱法（LC-MS / MS）在动物和水生食品基质中定量测定氨基甲酸钙衍生的代谢物，乙酰水杨酸（ASA）和水杨酸（SA）。将分析物从猪肌肉，牛奶，鸡蛋，虾，鳗鱼，并使用乙腈比目鱼萃取，用加入甲酸以及三氟乙酸，接着通过液-液纯化用饱和Ñ正己烷。使用反相分析柱，其流动相包含（A）在蒸馏水中的1 mM乙酸铵和（B）甲醇，以实现最佳色谱分离。基质匹配的校准曲线（R ² ≥0.9817）是在猪肌肉，牛奶，鸡蛋，虾，鳗鱼和比目鱼基质中使用六种浓度分别为5、10、20、30、40和50 µg / kg的溶液构建的。ASA和SA的定量限（LOQ）分别为10和7 µg / kg。在四种加标浓度（5、10、20和50 µg / kg）下，所有基质的回收率均达到67％至102％，相对标准偏差（RSD）≤9.0％（日内和日间）。该方法可行地用于监测市场样本。总之，所开发的方法用途广泛，准确且精确，可用于检测和定量供人食用的动物源性食品中的乙酰水杨酸和水杨酸残留。