Institute of Chemical Technology Prague, Faculty of Food and Biochemical Technology, Department of Food Chemistry and Nutrition, Technická 5, 16628, Prague 6, Czech Republic.
Rapid Commun Mass Spectrom. 2013 Feb 15;27(3):467-75. doi: 10.1002/rcm.6466.
Direct analysis in real time (DART) is a novel ionization technique that has been demonstrated in numerous applications as a useful tool for fast and convenient mass spectrometry (MS)-based analysis of complex samples. In this study, the feasibility of DART ionization coupled to a high-resolution mass spectrometer utilizing an orbitrap mass analyzer (orbitrap MS) for high-throughput analysis of antiparasitic veterinary drugs was explored.
To obtain the best DART-orbitrap MS performance, stepwise optimization of instrumental parameter settings, such as ionization gas temperature and mass resolving power, was performed. The optimized method was applied to feed and bovine milk samples previously extracted following a QuEChERS-like strategy.
Most antiparasitic drugs could be analyzed following the described method. Positive DART ionization provided the protonated molecules M+H; in negative DART ion mode, deprotonated molecules M-H were observed. As an exception, polyether ionophores could be observed as the sodiated adducts M+Na. Samples of milk and feed were extracted using a modified QuEChERS method for the determination of benzimidazoles and coccidiostats respectively and quantification was carried out by matrix-matched calibration curves.
The combination of an analysis time of less than 1 min per sample and the possibility to acquire accurate masses under high mass resolving power (HR) makes the DART-HRMS technique an effective tool for rapid qualitative screening of antiparasitic veterinary drugs. Additionally, the results obtained in this study demonstrated the feasibility of this approach to quantify target analytes at levels down to 1 µg kg(-1) for benzimidazolic compounds in milk and 0.25 mg kg(-1) for coccidiostats in chicken feed.
实时直接分析 (DART) 是一种新颖的离子化技术，已在众多应用中得到证实，是一种用于快速便捷地分析复杂样品的基于质谱 (MS) 的有用工具。在这项研究中，探索了 DART 离子化与利用轨道阱质量分析仪 (轨道阱 MS) 的高分辨率质谱仪相结合，用于高通量分析抗寄生虫兽用药物的可行性。
为了获得最佳的 DART-轨道阱 MS 性能，对仪器参数设置（例如离子化气体温度和质量分辨率）进行了逐步优化。将优化后的方法应用于先前采用 QuEChERS 类似策略提取的饲料和牛奶样品中。
大多数抗寄生虫药物都可以通过描述的方法进行分析。正 DART 离子化提供质子化分子 M+H；在负 DART 离子模式下，观察到去质子化分子 M-H。作为例外，聚醚离子载体可以观察到作为加钠离子的加合物 M+Na。牛奶和饲料样品分别使用改良的 QuEChERS 方法提取，用于测定苯并咪唑类和球虫抑制剂，并通过基质匹配校准曲线进行定量。
分析时间不到 1 分钟/样品，并且在高质量分辨率 (HR) 下能够获得准确质量的可能性，使得 DART-HRMS 技术成为快速定性筛选抗寄生虫兽用药物的有效工具。此外，本研究的结果表明，该方法能够定量分析牛奶中苯并咪唑类化合物的目标分析物达到 1μg/kg(-1) 的水平，鸡饲料中球虫抑制剂达到 0.25mg/kg(-1) 的水平。
