使用自动化的样品制备结合LC-MS/MS分析蜂蜜中氯霉素
简介
Chloramphenicol (CAP) (Figure 1) is a bacteriostatic antimicrobial previously used in veterinary medicine. CAP has been found to be potentially carcinogenic, which makes it an unacceptable substance for use with any foodproducing animals, including honey bees. The United States, Canada, and the European Union (EU), as well as many other countries, have completely banned the usage of CAP in the production of food. The EU has set a minimum required performance level (MRPL) for CAP in food of animal origin at a level of 0.3 μg/kg1. Currently sample preparation for the detection of CAP in honey by liquid chromatography-mass spectrometry (LC-MS/MS) involves complex offline extraction methods such as solid phase extraction, QuEChERS, or liquid/liquid extraction, all of which require additional sample concentration and reconstitution in an appropriate solvent. These sample preparation methods are timeconsuming, often taking 2 hours or more per sample, and are more vulnerable to variability due to errors in manual preparation. To offer a high sensitivity (low ppbs) CAP detection method and timely, automated analysis of multiple samples, our approach is to use the Thermo Scientific Aria TLX-1 system powered by TurboFlow™ automated sample preparation technology coupled to the detection capabilities of a high-sensitivity Thermo Scientific TSQ Vantage triple stage quadrupole mass spectrometer.
目标
Develop a quick, automated sample preparation, LC-MS/MS method for chloramphenicol (CAP) in honey by negative ion heated electrospray ionization (H-ESI) using a deuterated internal standard (CAP-d5).
实验仪器
结论
A quick, automated online extraction, LC-MS/MS method has been developed here that is sensitive enough to detect 0.023 μg/kg (LOD) and quantify 0.047 μg/kg (LLOQ) of CAP in honey for screening purposes. This is significantly lower than the MRPL of 0.3 μg/kg (ppb) set by the EU. This method eliminates the need for time-consuming sample preparation procedures such as solid phase extraction, QuEChERS, and liquid-liquid extraction. Dilution with water to reduce sample viscosity is the only pretreatment required. The LC-MS/MS method run time is 5 minutes, and the sample throughput can be improved by multiplexing on an Aria TLX-4 system.
