摘要
建立了通过式固相萃取-超高效液相色谱串联质谱法测定动物源性食品中13种磺胺类药物的检测方法。动物源性食品经1%甲酸乙腈(V/V)或80%乙腈水溶液(含1%甲酸)(V/V)提取,氯化钠饱和,通过式固相萃取净化。使用Phenomenex Luna Omega C18色谱柱(2.1 mm×100 mm,1.6μm)进行分离,0.1%甲酸水溶液(V/V)和乙腈为流动相梯度洗脱。采用电喷雾电离(Electrospray ionization,ESI)和多离子检测模式(Multiple reaction monitoring,MRM)进行检测,基质匹配外标法定量。结果显示13种磺胺类药物在0.0005~0.050 mg/L范围内线性关系良好,r>0.995。在猪肉、鸡肉、鲈鱼、鸡蛋和猪肝5种典型基质中,0.5~100μg/kg添加浓度范围内,平均回收率在78.1%~101.3%,相对标准偏差均<10%。该方法操作简单、灵敏度高,可用于动物源性食品中13种磺胺类药物的测定。
A detection method for 13 sulfonamide drugs in animal-derived foods was established by pass-through solid-phase extraction-ultra high-performance liquid chromatography-tandem mass spectrometry.Animal-derived foods were extracted with 1%formic acid acetonitrile(V/V)or 80%acetonitrile aqueous solution containing 1%formic acid(V/V),saturated with NaCl,and purified by passthrough solid-phase extraction.The Phenomenex Luna Omega C18(2.1 mm×100 mm,1.6μm)column was used for separation,and a gradient elution with 0.1%formic acid water and acetonitrile was applied as the mobile phase.Detection was carried out using electrospray ionization(ESI)and multiple reaction monitoring(MRM)mode,and matrix-matched calibration was used for quantification.The results showed good linearity for the 13 sulfonamide drugs within the range of 0.0005–0.050 mg/L,with an r>0.995.The average recovery rates of the 13 sulfonamide drugs in five typical matrices(pork,chicken,fish,eggs,and pig liver)were in the range of 78.1%to 101.3%at the addition levels of 0.5–100μg/kg,and the relative standard deviations all less than 10%.This method is simple,sensitive,and suitable for the determination of 13 sulfonamide drugs in animal-derived foods.
作者
李丹娜
王建山
LI Danna;WANG Jianshan(Henan Techenical Institute,Zhengzhou 450042,China;Shaanxi Key Laboratory of Food and Drug Safety Monitoring,Shaanxi Institute for Food and Drug Control,Xi’an 710065,China)
出处
《食品科技》
北大核心
2023年第11期305-311,共7页
Food Science and Technology
基金
2019年陕西省创新能力支撑计划项目(2019PT-22)。
关键词
通过式固相萃取
超高效液相色谱串联质谱法
动物源性食品
磺胺类药物
pass-through solid-phase extraction
ultra high-performance liquid chromatography-tandem mass spectrometry
animal-derived foods
sulfonamide drugs
