目的:建立快速检测粉末状抗生素药品的方法。方法:将自制表面解吸常压化学电离(SDAPCI)源耦合到线性离子阱质谱仪中,在无需样品预处理的前提下,以潮湿窄气作为试剂,通过电晕放电产生大量试剂离子(即活性质子),对市售粉末状阿莫西林、诺氟沙星、罗红霉素及头孢拉定等常见抗生素药物的活性成分直接进行串联质谱检测。结果:方法具有较高的灵敏度,对诺氟沙星等抗生素的检测限为8×10^-13g·cm^-1,能够直接用于诺氟沙星药品光解产物的检测与鉴定。结论:单个样品的分析时间不到1min,可广泛用于粉末状药品活性成分与痕量杂质的快速检测。
Objective:To establish a novel method for the rapid determination of powdered antibiotics. Methods:A novel method using a homemade surface desorption atmospheric pressure chemical ionization (SDAPCI) source coupled to a linear ion trap mass spectrometer was developed for direct detection of various active constituents such as amoxicillin, norfloxacin, roxithomycin in powdered pharmaceutical preparations. In the SDAPCI source, corona discharged was employed to generate the primary reagent ions, using ambient moisture in the air, for chemical ionization of analytes in ambient conditions. Photolysis products of norfloxacin were rapidly detected and identified using tandem mass spectrometry. Results :The detection limit was 8 ×10^-13g·cm^-2 for tested antibiotics. A single sample analysis was completed in less than l min. Conclusion:The data showed that multiple stage SDAPCI mass spectrometry is a useful tool for fast detection of active ingredients and trace impurities in powdered medicines.