College of Animal Science and Technology, Jiangxi Agricultural University, Nanchang, 330045, China.
College of Animal Science and Technology, Jiangxi Agricultural University, Nanchang, 330045, China.
Chemosphere. 2019 Sep;230:337-346. doi: 10.1016/j.chemosphere.2019.05.047. Epub 2019 May 9.
We developed a QuEChERS (quick, easy, cheap, effective, rugged and safe) method for the high through-put determination of 28 common veterinary antibiotics in swine wastewater using one-step dispersive solid-phase extraction (d-SPE) for sample cleanup and ultra-performance liquid chromatography-tandem mass spectrometry for detection. The orthogonal test method was used to systematically investigate the parameters that might influence d-SPE efficiency. The optimal d-SPE procedure utilized 40 mg primary secondary amine sorbent and 3 g L NaEDTA. The recoveries ranged from 50 to 100% with relative standard deviations <20% for all target analytes except for enrofloxacin and chlortetracycline. The limits of detection and limits of quantification for all the analytes ranged from 0.002 to 0.200 ng mL and 0.005-0.500 ng mL, respectively. The developed method was successfully applied to the analysis of 28 antibiotic residues in swine wastewater from 10 pig farms located in central China. Fourteen antibiotics including 4 sulfonamides (sulfadiazine, sulfamerazine, sulfamonomethoxine and trimethoprim), 5 fluoroquinolones (norfloxacin, ciprofloxacin, pefloxacin, enrofloxacin, and ofloxacin), 1 lincosamide (lincomycin) and 4 tetracyclines (doxycycline, tetracycline, oxytetracycline, and chlortetracycline) were detected at levels ranging from 0.0560 to 1793 ng mL. Our results demonstrated that the optimized method is a simple but reliable analytical technique for the routine monitoring of veterinary antibiotics in swine wastewater. Swine wastewater samples that we analyzed from 10 pig farms in Jiangxi Province, China were highly contaminated and pose a serious threat to ecosystems and to public health.
我们开发了一种 QuEChERS（快速、简单、廉价、有效、耐用和安全）方法，用于通过一步分散固相萃取（d-SPE）进行样品净化和超高效液相色谱-串联质谱法进行检测，高通量测定猪废水中的 28 种常见兽医抗生素。正交试验法用于系统研究可能影响 d-SPE 效率的参数。最佳 d-SPE 程序使用 40mg 一级二级胺吸附剂和 3g/L NaEDTA。除恩诺沙星和金霉素外，所有目标分析物的回收率均在 50%至 100%之间，相对标准偏差<20%。所有分析物的检测限和定量限范围为 0.002-0.200ng/mL 和 0.005-0.500ng/mL。该方法成功应用于中国中部 10 个养猪场猪废水中 28 种抗生素残留的分析。检测到包括 4 种磺胺类药物（磺胺嘧啶、磺胺甲恶唑、磺胺二甲氧嘧啶和甲氧苄啶）、5 种氟喹诺酮类药物（诺氟沙星、环丙沙星、培氟沙星、恩诺沙星和氧氟沙星）、1 种林可酰胺类药物（林可霉素）和 4 种四环素类药物（强力霉素、四环素、土霉素和金霉素）在内的 14 种抗生素，浓度范围为 0.0560-1793ng/mL。我们的结果表明，优化后的方法是一种简单但可靠的分析技术，可用于常规监测猪废水中的兽医抗生素。我们分析的来自中国江西省 10 个养猪场的猪废水样本受到高度污染，对生态系统和公众健康构成严重威胁。
