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.
J Chromatogr A. 2022 May 10;1670:462979. doi: 10.1016/j.chroma.2022.462979. Epub 2022 Mar 18.
A simple and accurate method of ultra high performance liquid chromatography (UHPLC) coupled with quadrupole-high field Orbitrap high-resolution mass spectrometry (QE HF HRMS) has been developed for analyzing 8 trace-level (µg/L) carbapenems in milk. Mass spectrometry conditions, chromatographic conditions, extraction solvent and QuEChERS procedures were optimized for determination of 8 carbapenems in milk. Samples were extracted and purified by modified QuEChERS procedure. Good separation for 8 carbapenems s was achieved with a PFP column at 8 min. Method validation results showed the linear ranges are 1-100 µg/L to 10-1,000 µg/L, the correlation coefficients are more than 0.995, and the recoveries of spiked samples are 79.3%-104% with a relative standard deviation less than 15%. This method successfully applied to monitor residue of carbapenems in real milk, four kinds of carbapenems have been detected in 8 sample of 79 collected milks with concentration ranged between 15 µg/L∼3,325 µg/L.
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联用(UHPLC-QE HF HRMS)测定牛奶中 8 种痕量(μg/L)碳青霉烯类抗生素的简单、准确方法。对质谱条件、色谱条件、提取溶剂和 QuEChERS 步骤进行了优化,以测定牛奶中的 8 种碳青霉烯类抗生素。采用改良的 QuEChERS 法提取和净化样品。在 8 min 内,用 PFP 柱实现了 8 种碳青霉烯类抗生素的良好分离。方法验证结果表明,线性范围为 1-100 μg/L 至 10-1,000 μg/L,相关系数均大于 0.995,加标样品的回收率为 79.3%-104%,相对标准偏差小于 15%。该方法成功应用于监测实际牛奶中碳青霉烯类抗生素的残留情况,在 79 份采集的牛奶中检测到 8 种碳青霉烯类抗生素,浓度范围为 15 μg/L∼3,325 μg/L。