Institute of Quality Standards and Testing Technology for Agricultural Product, Chinese Academy of Agricultural Science, Beijing 100081, China.
Institute of Quality Standards and Testing Technology for Agricultural Product, Chinese Academy of Agricultural Science, Beijing 100081, China.
Food Chem. 2021 Nov 1;361:130115. doi: 10.1016/j.foodchem.2021.130115. Epub 2021 May 15.
A method for rapid screening and quantification of progesterone and progestins in milks by ultrahigh-performance liquid chromatography coupled with quadrupole-high field Orbitrap high-resolution mass spectrometry (UHPLC QE HF HRMS) was established. Milks samples were extracted by acetonitrile + hexane (80 + 20), purified by prime HLB SPE and analyzed by UHPLC QE HF HRMS. The detection limit of progesterone and 21 progestins in milk is between 0.05 µg/kg -0.3 μg /kg, the correlation coefficient of progesterone and progestins in the corresponding concentration range is more than 0.99, recoveries for milk samples are between 80.7% and 108.3% with the relative deviation is less than 15%.The method fulfils the requirements of veterinary drug residue detection validation of EU and China, and successfully applied to detecting the μg/kg level of progesterone and monitoring residual of progestins in real milk.
建立了一种超高效液相色谱-四极杆-高场轨道阱高分辨质谱法（UHPLC-QE-HF-HRMS）快速筛选和定量牛奶中孕酮和孕激素的方法。采用乙腈+正己烷（80+20）提取牛奶样品，经 prime HLB SPE 净化，用 UHPLC-QE-HF-HRMS 分析。牛奶中孕酮和 21 种孕激素的检测限为 0.05μg/kg-0.3μg/kg，相应浓度范围内孕酮和孕激素的相关系数均大于 0.99，牛奶样品的回收率在 80.7%至 108.3%之间，相对偏差小于 15%。该方法符合中、欧兽药残留检测验证要求，成功应用于检测牛奶中μg/kg 水平的孕酮和监测实际牛奶中孕激素的残留。
