基于两性离子共价有机框架材料固相萃取快速检测保健食品/中成药中喹诺酮类抗生素

Rapid determination of quinolone antibiotics in health foods and Chinese patent medicine based on zwitterionic covalent organic framework solid-phase extraction

中文关键词:  共价有机框架  固相萃取  高效液相色谱法  喹诺酮类抗生素  中成药  保健食品

英文关键词:covalent organic frameworks  solid phase extraction  high performance liquid chromatography  quinolone antibiotics  Chinese patent medicine  health foods

中文摘要:

      目的 建立基于两性离子共价有机框架材料(Tp-MTABs)的固相萃取(solid phase extraction, SPE)-高效液相色谱法(high performance liquid chromatography, HPLC)快速测定中成药/保健食品中喹诺酮类抗生素的方法。方法 通过扫描电子显微镜、Ｘ射线衍射仪和红外光谱仪对Tp-MTABs的微观形貌、晶体结构和化学结构进行表征。对影响固相萃取效率的吸附剂用量、吸附时间、洗脱剂种类、洗脱剂体积和洗脱时间等关键因素进行优化。结果 在最优条件下, 8种喹诺酮类抗生素的方法线性范围为2.0~100.0 μg/L, 线性相关系数(r2)均大于等于0.9985, 检出限(limits of detection, LODs)为0.33~0.80 μg/kg。3个加标水平下的回收率为94.8%~104.5%, 相对标准偏差(relative standard deviations, RSDs)为1.1%~2.8%。结论 本方法选择性好、灵敏度高, 适用于清热解毒抗炎类保健食品/中成药中喹诺酮类抗生素的快速检测。

英文摘要:

      Objective To establish a method for the rapid determination of quinolone antibiotics in Chinese patent medicine and health foods by solid-phase extraction (SPE) and high performance liquid chromatography (HPLC) based on zwitterionic covalent organic framework (Tp-MTABs). Methods The microscopic morphology, crystal structure and chemical structure of Tp-MTABs were detailed characterized by scanning electron microscope, X-ray diffractometer and Fourier-transform infrared spectrometer. The key factors affecting the efficiency of solid-phase extraction were fully optimized, including adsorbent dosage, adsorption time, eluent type, eluent volume, and elution time. Results Under the optimal conditions, the linear ranges for the detection of 8 kinds of quinolone antibiotics were 2.0?100.0 μg/L, and the linear correlation coefficients (r2) were all greater than or equal to 0.9985 with the limits of detection (LODs) among 0.33?0.80 μg/kg. The spiked recoveries obtained at the 3 spiked levels were 94.8%?104.5%, and the relative standard deviations (RSDs) were 1.1%?2.8%. Conclusion This established method possesses excellent selectivity and high sensitivity, which is suitable for the rapid detection of quinolone antibiotics in health foods and Chinese patent medicine with heat-clearing, detoxifying and anti-inflammatory effects.