高效液相色谱-串联质谱法检测水产品中硝基呋喃类代谢物的优化研究

Optimization of determination of nitrofuran metabolites in aquatic products by liquid chromatography tandem mass spectrometry

研究了利用高效液相色谱-串联质谱法（LC—MS／MS）检测水产品中残留的5-吗啉甲基-3-氨基-2-嗯唑烷基酮（AMOZ）、氨基脲（SEM）、1-氨基-2-内酸脲（AHD）和3-氨基-2-噁唑烷基酮（AOZ）等4种硝基呋喃类代谢物，优化了前处理方法及液相色谱条件。硝基呋喃类代谢物经衍生化后，调节样品pH至7．0～7．5，加入8mL乙酸乙酯，离心并转移上清液，氮气吹干后，用乙腈-0．1％的甲酸水（5／95，V/V）溶液定容，4℃高速离心后上机测定。采用梯度洗脱法，4种代谢物在C18柱中分离良好。该法有效地提高硝基呋喃类代谢物的检测效率，且检测结果准确，适用于批量水产品的检测。

The nitrofuran metabolites （AMOZ, SEM, AHD and AOZ） were determined by liquid chromatography tandem mass spectrometry （LC-MS/MS） in aquatic products. The sample pretreatment method and chromatographic conditions were optimized. The sample pH value was adjusted to 7. 0 - 7.5 after derivation. Then the analytes were extracted by 8 mL ethyl acetate. Following centrifugation, the supernatant was transferred and evaporated to dryness under a gentle stream of nitrogen at 40 ℃. The residues were redissolved in 1 mL mobile phase of acetonitrile and 0. 1% formic acid （5/95, V/V）, and then centrifuged at 20 000 × g for 10 min at 4 ℃. Gradient elution for LC separation was performed by using acetonitrile and 0. 1% formic acid in water solution, and four nitrofuran metabolites were excellently separated with a C18 column. This accurate optimized method can promote efficiency greatly and is suitable for lot determination of nitrofuran metabolites in aquatic products.