Wang Jian
Canadian Food Inspection Agency, Calgary Laboratory, 3650-36th Street N.W., Calgary, Alberta, Canada T2L 2L1.
Mass Spectrom Rev. 2009 Jan-Feb;28(1):50-92. doi: 10.1002/mas.20189.
Macrolides are a group of antibiotics that have been widely used in human medical and veterinary practices. Analysis of macrolides and related compounds in food, biological, and environmental matrices continue to be the focus of scientists for the reasons of food safety, pharmacokinetic studies, and environmental concerns. This article presents an overview on the primary biological properties of macrolides and their associated analytical issues, including extraction, liquid chromatography-mass spectrometry (LC-MS), method validation, and measurement uncertainty. The main techniques that have been used to extract macrolides from various matrices are solid-phase extraction and liquid-liquid extraction. Conventional liquid chromatography (LC) with C18 columns plays a dominant role for the determination of macrolides, whereas ultra-performance liquid chromatography (UPLC) along with sub-2 microm particle C18 columns reduces run time and improves sensitivity. Mass spectrometry (MS), serving as a universal detection technique, has replaced ultraviolet (UV), fluorometric, and electrochemical detection for multi-macrolide analysis. The triple-quadrupole (QqQ), quadrupole ion trap (QIT), triple-quadrupole linear ion trap, time-of-flight (TOF), and quadrupole time-of-flight (QqTOF) mass spectrometers are current choices for the determination of macrolides, including quantification, confirmation, identification of their degradation products or metabolites, and structural elucidation. LC or UPLC coupled to a triple-quadrupole mass spectrometer operated in the multiple-reaction monitoring (MRM) mode (LC/MS/MS) is the first choice for quantification. UPLC-TOF or UPLC-QqTOF has been recognized as an emerging technique for accurate mass measurement and unequivocal identification of macrolides and their related compounds.
大环内酯类是一类抗生素,已广泛应用于人类医学和兽医实践中。由于食品安全、药代动力学研究以及环境问题等原因,对食品、生物和环境基质中的大环内酯类及其相关化合物进行分析一直是科学家们关注的焦点。本文概述了大环内酯类的主要生物学特性及其相关分析问题,包括提取、液相色谱 - 质谱联用(LC - MS)、方法验证和测量不确定度。用于从各种基质中提取大环内酯类的主要技术是固相萃取和液液萃取。使用C18柱的传统液相色谱(LC)在大环内酯类的测定中起主导作用,而超高效液相色谱(UPLC)与粒径小于2微米的C18柱一起使用可减少运行时间并提高灵敏度。质谱(MS)作为一种通用检测技术,已取代紫外(UV)、荧光和电化学检测用于多大环内酯类分析。三重四极杆(QqQ)、四极杆离子阱(QIT)、三重四极杆线性离子阱、飞行时间(TOF)和四极杆飞行时间(QqTOF)质谱仪是目前测定大环内酯类的选择,包括定量、确认、鉴定其降解产物或代谢物以及结构解析。液相色谱或超高效液相色谱与在多反应监测(MRM)模式下运行的三重四极杆质谱仪联用(LC/MS/MS)是定量的首选方法。超高效液相色谱 - 飞行时间质谱(UPLC - TOF)或超高效液相色谱 - 四极杆飞行时间质谱(UPLC - QqTOF)已被认为是一种新兴技术,用于准确质量测量和明确鉴定大环内酯类及其相关化合物。