通过式固相萃取-超高效液相色谱-串联质谱法测定动物源性食品中30种食源性兴奋剂

Simultaneous Determination of 30 Foodborne Stimulant Drug Residues in Animal-Derived Foods by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry with Pass-Through Solid Phase Extraction

针对不同动物源性食品中多种食源性兴奋剂检测基质效应差异较大、干扰较多等问题,本研究建立通过式固相萃取-超高效液相色谱-串联质谱法测定动物源性食品中10种蛋白同化剂、8种糖皮质激素和12种利尿剂等食源性兴奋剂,试样经5%甲酸-乙腈提取,通过式固相萃取柱净化,采用液相色谱-串联质谱仪测定,同位素内标法定量。结果表明,30种食源性兴奋剂在各自浓度范围内线性关系良好,平均回收率介于67.5%~114.3%,相对标准偏差介于0.7%~16.1%(n=6)。该方法具有灵敏度高、操作简单、检测通量大、检测效率高等特点,提高了不同复杂基质下的检测准确性,能够满足赛事用动物源性食品中30种食源性兴奋剂的检测需求。

In order to solve the problems of the detection of various foodborne stimulants in different animal-derived foods such as significant differences in matrix effects and many types of interference,a method was established for the determination of 10 protein anabolic agents,8 glucocorticoids,and 12 diuretics in animal-derived foods by pass-through solid phase extraction(SPE)and ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The sample was extracted with 5%formic acid in acetonitrile,and the extract was purified by pass-through solid phase extraction before being analyzed by UPLC-MS/MS.The internal standard method was used for quantification.The results showed that good linearity was observed for all analytes within their respective concentration ranges.The average recoveries ranged from 67.5%to 114.3%with relative standard deviations(RSDs)between 0.7%and 16.1%(n=6).This method is characterized by high sensitivity,simple operation,high throughput and high detection efficiency,which improves the measurement accuracy of different complex matrices and can meet the need for the detection of the 30 foodborne stimulants in animal-derived foods used in sports events.