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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AcquityTMUPLCBEH 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。
A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method was developed to analyze the possible metabolites of mequindox in the body wall of sea cucumber. Different types of metabolites are purified and concentrated by precipitation and solid-phase extraction (SPE). The mobile phase consisted of acetonitrile with 0.1% formic acid and water with 0.1% formic acid, and the metabolites were eluted with a gradient of Acquity TM UPLC BEH C18 (2.1 mm × 50 mm × 1.7 μm). Electrospray ionization (ESI) Positive ion full scan mode to detect. By comparing the primary and secondary ion of the sample with the standard, it was confirmed that mequindox contained 3-methylquinoxaline-2-carboxylic acid (MQCA) in the metabolites of the sea cucumber body wall, and at the same time, 3 Unknown metabolites D2, D3, D4, and speculated possible metabolite cleavage pathways.