MOE Key Laboratory of Bioinorganic and Synthetic Chemistry/KLGHEI of Environment and Energy Chemistry, School of Chemistry, Sun Yat-sen University, Guangzhou 510275, China.
Molecules. 2019 Apr 28;24(9):1670. doi: 10.3390/molecules24091670.
In this study, the detection and quantification of multiple classes of antibiotics in water matrices are proposed using a lab-made solid phase microextraction (SPME) fiber coupled with high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). The lab-made fiber was prepared using a graphene oxide (G), carbon nanotubes (C), and titanium dioxide (T) composite, namely GCT, with polyacrylonitrile (PAN) as supporting material. The detected antibiotics were enrofloxacin, sulfathiazole, erythromycin, and trimethoprim. The custom-made fiber was found to be superior compared with a commercial C18 fiber. The excellent reproducibility and lower intra-fiber relative standard deviations (RSDs 1.8% to 6.8%) and inter-fiber RSDs (4.5% to 8.8%) made it an ideal candidate for the detection of traces of antibiotics in real environmental samples. The proposed validated method provides a satisfactory limit of detection and good linear ranges with higher (>0.99) coefficient of determination in the aqueous system. Application of the method was made in different real water systems such as river, pond and tap water using the standard spiking method. Excellent sensitivity, reproducibility, lower amount of sample detection and higher recovery was found in a real water sample. Therefore, the extraction method was successfully applied to the detection and quantification of multiple classes of antibiotics in different aqueous systems with satisfactory results.
本研究提出了一种使用实验室自制固相微萃取（SPME）纤维与高效液相色谱-串联质谱（LC-MS/MS）相结合的方法，用于检测和定量水基质中的多种抗生素。实验室自制纤维采用氧化石墨烯（GO）、碳纳米管（CNT）和二氧化钛（TiO2）复合材料 GCT 与聚丙烯腈（PAN）作为支撑材料制备。检测的抗生素有恩诺沙星、磺胺噻唑、红霉素和甲氧苄啶。与商用 C18 纤维相比，这种定制纤维具有优越性。良好的重现性和较低的纤维内相对标准偏差（RSD 为 1.8%至 6.8%）和纤维间 RSD（4.5%至 8.8%）使它成为检测真实环境样品中痕量抗生素的理想候选物。所提出的验证方法在水溶液中提供了令人满意的检测限和良好的线性范围，相关系数大于 0.99。该方法采用标准加标法应用于不同的实际水系，如河流、池塘和自来水。在实际水样中发现了良好的灵敏度、重现性、较低的检测样品量和较高的回收率。因此，该萃取方法成功地应用于不同水系中多种抗生素的检测和定量，结果令人满意。
