固相萃取-超高效液相色谱-串联质谱法测定水中氯霉素、氟甲砜霉素和4种四环素类抗生素

Determination of chloroamphenicol,florfenicol and 4 tetracyclineantibiotics in water by SPE- UPLC- MS /MS

目的建立固相萃取-超高效液相色谱-串联质谱法同时测定水中氯霉素、氟甲砜霉素和4种四环素类抗生素的检测方法。方法样品经HLB固相萃取柱富集、净化后用甲醇洗脱,以超高效液相色谱-串联质谱(UPLC-MS/MS)多反应监测(MRM)正负离子切换模式检测测定水中抗生素残留,外标法定量。结果方法的线性范围为2μg/L^200μg/L,线性相关系数0.9988~0.9995,检出限0.08 ng/L^5.21 ng/L;出厂水和水源水的平均加标回收率分别为82.3%~96.1%和80.4%~92.4%;相对标准偏差(RSD)2.6%~6.8%。结论该方法具有操作简单、干扰少、快速、准确可靠的特点,适用于水样品中抗生素残留的定量及确证检测。

Objective An ultra high performance liquid chromatography - tandem mass spectrometric （ UPLC - MS/MS） meth- od with solid phase extraction was established for determination of chloroamphenicol, florfenicol and 4 tetracycline antibiotics in drinking water and source water. Methods The water samples were enriched and cleaned up by HLB solid phase extraction （SPE） column. The target analytes were elnted by methanol from SPE column and detected by UPLC -MS/MS. Determination was achieved by electrospray ionization（ESI） in positive mode and negative mode using multiple reaction monitoring and quanti- fied with the external method. Results The calibration curves of six antibiotics showed good ]inearity in the range of 2 Ixg/L 200 pLg/L with correlation coefficient in the range of 0. 9988 - 0. 9995. The detection limit of the method was from 0.08 ng/L to 5.21 ng/L, the recoveries of the drinking water and source water ranged from 82.3 % to 96.1% and 80.4% to 92.4% respec- tively, and RSDs was from 2. 6% to 6.8%. Conclusion The method is proved to be suitable for quantitative analysis and confirmation of antibiotic residues in water due to easy to operate, less interference, rapidity and accuracy.