论文部分内容阅读
目的建立一种快速、灵敏、准确的鸡蛋中5-吗啉甲基-3-氨基-2-恶唑烷基酮(AMOZ)、氨基脲(SEM)、1-氨基-乙内酰脲(AHD)和3-氨基-2-恶唑酮(AOZ)等4种硝基呋喃代谢物残留的固相萃取-超快速液相色谱-串联质谱(UFLC-MS/MS)测定方法。方法样品经盐酸水解、衍生化、磷酸盐缓冲液(pH=7.4)提取、HLB固相萃取小柱净化,在Shim-pack XR-ODS III C18反相色谱柱(2.0 mm×150 mm i.d.,3.0μm)上分离,采用电喷雾离子源(ESI)在多反应监测(MRM)模式下检测,同位素内标法定量。结果 4种硝基呋喃代谢物在0.25μg/kg~25.0μg/kg(相当于0.5μg/L~50.0μg/L)范围内呈现良好的线性(R2>0.999),检出限在0.04μg/kg~0.05μg/kg范围,定量限在0.13μg/kg~0.16μg/kg范围,当加标水平为0.25μg/kg、10.0μg/kg、20.0μg/kg时,4种硝基呋喃代谢物在鸡蛋中的加标回收率分别为92%~106%、93%~107%和91%~110%,相对标准偏差(RSD)为2.8%~7.7%。结论本方法可用于鸡蛋中残留AMOZ、SEM、AHD和AOZ的快速筛查和确证。
Objective To establish a rapid, sensitive and accurate method for the determination of 5-morpholinomethyl-3-amino-2-oxazolidinone (AMOZ), semicarbazide (SEM), 1-amino-hydantoin ) And 3-amino-2-oxazolidone (AOZ) were determined by UFLC-MS / MS. Methods The samples were extracted with hydrochloric acid, derivatized with phosphate buffer (pH = 7.4) and HLB solid phase extraction cartridges were purified on a Shim-pack XR-ODS III C18 column (2.0 mm × 150 mm id, 3.0 μm), detected by electrospray ionization (ESI) in multiple reaction monitoring (MRM) mode, and quantified by isotope internal standard method. Results Four kinds of nitrofuran metabolites showed good linearity (R2> 0.999) in the range of 0.25μg / kg ~ 25.0μg / kg (equivalent to 0.5μg / L ~ 50.0μg / L) kg to 0.05μg / kg, and the limit of quantification was in the range of 0.13μg / kg ~ 0.16μg / kg. When the spiked levels were 0.25μg / kg, 10.0μg / kg and 20.0μg / kg, The spiked recoveries in eggs ranged from 92% to 106%, from 93% to 107% and from 91% to 110%, respectively. The relative standard deviations (RSDs) ranged from 2.8% to 7.7%. Conclusion This method can be used for rapid screening and confirmation of residual AMOZ, SEM, AHD and AOZ in eggs.