Ye Diru, Wu Susu, Xu Jianqiao, Jiang Ruifen, Zhu Fang, Ouyang Gangfeng
MOE Key Laboratory of Aquatic Product Safety/KLGHEI of Environment and Energy Chemistry, School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275, China.
MOE Key Laboratory of Aquatic Product Safety/KLGHEI of Environment and Energy Chemistry, School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275, China
J Chromatogr Sci. 2016 Feb;54(2):112-8. doi: 10.1093/chromsci/bmv126. Epub 2015 Aug 25.
Direct immersion solid-phase microextraction (DI-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) was developed for rapid analysis of clenbuterol in pork for the first time. In this work, a low-cost homemade 44 µm polydimethylsiloxane (PDMS) SPME fiber was employed to extract clenbuterol in pork. After extraction, derivatization was performed by suspending the fiber in the headspace of the 2 mL sample vial saturated with a vapor of 100 µL hexamethyldisilazane. Lastly, the fiber was directly introduced to GC-MS for analysis. All parameters that influenced absorption (extraction time), derivatization (derivatization reagent, time and temperature) and desorption (desorption time) were optimized. Under optimized conditions, the method offered a wide linear range (10-1000 ng g(-1)) and a low detection limit (3.6 ng g(-1)). Finally, the method was successfully applied in the analysis of pork from the market, and recoveries of the method for spiked pork were 97.4-105.7%. Compared with the traditional solvent extraction method, the proposed method was much cheaper and fast.
首次开发了直接浸入式固相微萃取(DI-SPME)与气相色谱-质谱联用(GC-MS)技术用于快速分析猪肉中的克伦特罗。在这项工作中,采用了低成本自制的44μm聚二甲基硅氧烷(PDMS)固相微萃取纤维来萃取猪肉中的克伦特罗。萃取后,通过将纤维悬浮在充满100μL六甲基二硅氮烷蒸汽的2mL样品瓶顶空中进行衍生化。最后,将纤维直接引入GC-MS进行分析。对影响吸附(萃取时间)、衍生化(衍生化试剂、时间和温度)和解吸(解吸时间)的所有参数进行了优化。在优化条件下,该方法具有宽线性范围(10-1000 ng g(-1))和低检测限(3.6 ng g(-1))。最后,该方法成功应用于市售猪肉的分析,加标猪肉的回收率为97.4-105.7%。与传统溶剂萃取方法相比,该方法成本更低且速度更快。