LC-MS测定火腿肠中4种硝基呋喃类代谢物残留

Determination of Metabolites of Nitrofuran Antibiotics in Sausage by LC-MS

建立同时测定火腿肠中4种硝基呋喃类药物代谢物残留量的液相色谱-质谱方法。火腿肠样品均质后,用0.2 mol/L盐酸水解,经邻硝基苯甲醛衍生后过固相萃取小柱净化,收集洗脱液用氮气吹干定容后,采用多反应监测模式进行检测,同位素内标法定量。添加浓度为0.498 ng/mL^5.070 ng/mL时,4种硝基呋喃类药物代谢物的回收率为76.7%~109.6%,相对标准偏差为3.0%~8.9%。该方法灵敏度高,检出限低,准确性好,可用于火腿肠中硝基呋喃类药物代谢物残留量的测定。

A method was established to determine metabolites of nitrofuran antibiotics in sausage. Homogenized samples were hydrolyzed with 0.2 mol/L hydrochloric acid, and then derivatized by 2-nitrobenzaldehyde. Analytes were cleaned by solid phase extraction （SPE）and reconstituted after dried under nitrogen. LC-MS detection was performed using multiple reaction monitoring module. The quantification was obtained utilizing the homologous internal standards. Recoveries of metabolites of nitrofuran antibiotics were from 76.7%to 109.6%at fortified levels of 0.498 ng/mL-5.070 ng/mL. The RSDs of the method were 3.0%-8.9%. The established method is sensitive, accurate and suitable for the determination of nitrofuran metabolites in sausage.