采用微波辅助中空纤维液相微萃取的样品前处理方法,在一段中空纤维管内注入正辛醇-甲苯(1:1,v/v)作为接受相,两端封口后浸入供相溶液进行萃取。在700r/min连续磁力搅拌和间歇微波辐照下,12.67rain即可完成27种目标化合物同时萃取。建立了微波辅助中空纤维液相微萃取联用液相色谱一串联质谱同时测定牛奶中27种抗生素(9种喹诺酮、15种磺胺、3种大环内酯)痕量残留的方法。以基质标准曲线外标法定量,线性范围为0.2-5.0μg/kg,相关系数均大于0.99(n=3),定量限(LOQ,S/N=10)在0.036-0.568μg/kg范围内。以0.5、1.0和2.0μg/kg添加浓度水平进行方法验证,回收率为49.0%~115.0%,相对标准偏差为0.89%~21.1%。
A novel sample preparation technique based on microwave assisted extraction coupled with hollow fiber liquid phase microextraction (HF-LPME) was studied. Octanol/toluene (1:1, V/V) was poured into a hollow fiber as accepted phase, and both ends were sealed. The fiber was immerged into donated phase for extraction. Twenty-seven target compounds were simultaneously extracted during 12. 67 min under the conditions of continuous 700 r/min stirring and intermittent microwave (MW) irradiation. The method based on MW assisted HF-LPME coupled with LC-MS/MS detection was developed. It was successfully applied to simultaneous analysis of 27 antibiotics (9 quinolones, 15 sulfanilamides and 3 macrolides) residues in milk. The matrix-matched calibrations were respectively used to quantify these compounds, and the linear range was 0.2-5.0 μg/kgwith the correlation coefficients above 0.99 (r≥0.99, n=3). The quantitative limit (LOQ, S/N= 10) was 0.036-0. 568 μg/kg. Method validation was carried out at three standard addition levels of 0.5, 1.0, 0. 9% -21 2.0 μg/kgand the recovery was 49.0%-115.0% with relative standard deviations (RSDs) of