Method Development And Application For Determination Of Estrogens In Animal-derived Food With UPLC/QTOFMS

Objective To develop a method for determinate estrogens in animal-derived food withultra UPLC/QTOF. To optimize the pretreatment method. To determinate the sample realsample and evaluate the results. Method Optimize the condition of UPLC separation.Optimize the MS condition and collision energy. Optimize the two methods of pretreatmentand chose the optimizing pretreatment according to the removing influencing factors andextractability. Determinate real samples and evaluate the results. Results Estrogens wereseparated by Agilent SB-C18column with one simple elution, water/acetonitrile52/48(V/V).The minimum resolution was4.0139. Six estrogens have been chosen for rapid determinationwith UPLC/QTOFMS at205nm. The experiment was accomplished under target MS/MS,ESI-mode. With the optimized collision energy, the MS/MS has been performed to avoidfalse positives. The LOD was0.1-0.8μg/L, the LOQ was3.5-7.3μg/L. At the spiked levels of10，20，50，100，500μg/L, the recoveries were59.6-128.5%, with a relative standard deviation(RSD) between1.2%–23.1%, The linear relation is0.9922～0.9989. MSPD were used in thepretreatment, the complication of classical pretreatment were eliminated. The results of thereal sample show that the estrogens were broadly detected. Milk contains more DES thanmeat. Pork and condensed milk contains more estrogens than other specimens. ConclusionA novel UPLC/QTOFMS method was developed for rapidly and simultaneously determinedsix estrogens in animal-derived food with good sensitivity. The method was successfullyapplied to real samples, provided a method for scientific guidance.