Zhou Weie, Ling Yun, Liu Tong, Zhang Yuan, Li Jianzhi, Li Hongna, Wu Wenjie, Jiang Shoujun, Feng Feng, Yuan Fei, Zhang Feng
Institute of Food Safety, Chinese Academy of Inspection & Quarantine, Beijing, 100176, China; College of Pharmacy, Guangxi University of Chinese Medicine, Nanning, 530299, China.
Institute of Food Safety, Chinese Academy of Inspection & Quarantine, Beijing, 100176, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Sep 1;1061-1062:411-420. doi: 10.1016/j.jchromb.2017.07.046. Epub 2017 Aug 5.
A novel analytical method was developed and validated for simultaneous analysis of 16 macrolide antibiotics and 4 metabolites in milk. A modified quick, easy, cheap, effective, rugged, and safe extraction method (QuEChERS) optimized by response surface methodology (RSM) was used for sample preparation. All the drugs were subsequently separated and detected by high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS), using roxithromycin as internal standards for maximum accuracy and precision. The method was validated following the guidelines specified in Commission Decision 2002/657/EC. The recoveries of all the analytes were in the range of 62.27%-115.28%. Most macrolide antibiotics and metabolites could be detected in the concentration of 1-100ng/mL with good correlation coefficient (r>0.998). The LODs and LOQs of all analytes were in the range of 0.30-0.85μg/kg and 1.1-4.0μg/kg, respectively. The intra-day and inter-day precision were lower than 10% and 15%, respectively. The developed method has been successfully applied to screen these compounds in different milk products.
开发并验证了一种同时分析牛奶中16种大环内酯类抗生素和4种代谢物的新型分析方法。采用响应面法（RSM）优化的改良快速、简便、廉价、高效、耐用且安全的萃取方法（QuEChERS）进行样品制备。随后，使用罗红霉素作为内标，通过高效液相色谱串联质谱法（HPLC-MS/MS）对所有药物进行分离和检测，以实现最高的准确度和精密度。该方法按照委员会第2002/657/EC号决定规定的指南进行验证。所有分析物的回收率在62.27%-115.28%范围内。大多数大环内酯类抗生素和代谢物能够在1-100ng/mL的浓度下被检测到，且具有良好的相关系数（r>0.998）。所有分析物的检测限（LOD）和定量限（LOQ）分别在0.30-0.85μg/kg和1.1-4.0μg/kg范围内。日内和日间精密度分别低于10%和15%。所开发的方法已成功应用于不同奶制品中这些化合物的筛查。
