HPLC-MS/MS法分析乙酰甲喹在海参中的主要代谢物

Study on Metabolites of Mequindox in Apostichopusjaponicus by HPLC-MS/MS

建立了高效液相色谱-串联质谱(HPLC-MS/MS)法分析乙酰甲喹在海参体壁中可能的代谢产物。采用沉淀法和固相萃取法(SPE)对不同种类的代谢物进行净化和浓缩。以含0.1%甲酸的乙腈和含0.1%甲酸的水为流动相,选取AcquityTMUPLCBEH C18(2.1mm×50mm×1.7μm)色谱柱对代谢物进行梯度洗脱,以电喷雾离子源(ESI)正离子全扫描模式进行检测。通过将样品的一级和二级子离子与标准品比对,确定乙酰甲喹在海参体壁的代谢物中含有3-甲基喹噁啉-2-羧酸(MQCA),同时检测出3种未知代谢物D2、D3、D4,并推测了代谢物可能的裂解途径。

Mequindox and its possible metabolites in body wall of Apostichopusjaponi- cus were identified by high performance liquid chromatography-tandem mass spectrome-try （HPLC-MS/MS）. Acetonitrile extraction and hydrochloric acid hydrolysis-SPE extraction were conducted to extract different kinds of metabolites. Metabolites were separated on an AcquityrMUPLC BEH C18（2.1 mm×50 mm×1.7μm）column by gradient elution with acetonitrile-water （containing 0.1% formic acid） as mobile phase, and detected by positive ions electrospray ionization （ESI） mass spectrometry with fullscan data dependent scan. Through comparison of MS1 and MS2 ions with the refer- ence standard, 3-methyl-quinoxaline-2-carbosylic acid （MQCA） is identified as a metab- olite of mequindox in Apostichopusjaponicus. The other identified metabolites include D2, D3, D4, and which the fragmentation pathways are deduced.