Abstract：
A quick, easy, cheap, effective, rugged, and safe method was developed for the multi-residue analysis of pesticides and antibiotics in aquaculture sediment using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The developed method is based on ultrasonic extraction with acetonitrile and phosphate buffer, salting with sodium chloride, and cleaning with dispersive solid-phase extraction adsorbent using primary secondary amine, C18, and graphitized carbon black, followed by HPLC-MS/MS detection. We optimized different extraction methods and the ratio of the cleanup adsorbents to achieve good recoveries at three spiking levels that ranged from 60.4% to 114% with a relative standard deviation below 15% (n = 6). For all analytes, except for flufenoxuron, the limits of quantification were between 1 and 5 µg/kg (dry weight). The validated method was successfully applied to real samples collected from 20 aquacultural ponds, confirming the feasibility of the proposed method. The concentrations of the target analytes in the sediments (dry weight) were in the ranges of 2.2-35.0 µg/kg for sulfonamides, 0-409.1 µg/kg for quinolones, 0-6.56 µg/kg for macrolides, and 0-4.9 µg/kg for pesticides. Moreover, the co-occurrence of pesticides and antibiotics may potentially pose a high risk to sediment-dwelling organisms in nine out of the 20 investigated locations.
摘要：
很快，easy,便宜,有效,崎岖,建立了高效液相色谱-串联质谱(HPLC-MS/MS)分析水产养殖底泥中农药和抗生素多残留的安全方法。所开发的方法基于乙腈和磷酸盐缓冲液的超声提取，用氯化钠盐渍，并使用伯仲胺进行分散固相萃取吸附剂清洗，C18和石墨化炭黑，随后进行HPLC-MS/MS检测。我们优化了不同的提取方法和清洁吸附剂的比例，以在三个加标水平下实现良好的回收率，该水平范围为60.4％至114％，相对标准偏差低于15％（n=6）。对于所有分析物，除了氟非诺酮,定量限在1至5µg/kg（干重）之间。经过验证的方法已成功应用于20个水产养殖池塘的实际样品中，证实了所提出方法的可行性。对于磺胺类药物，沉积物中目标分析物的浓度（干重）在2.2-35.0µg/kg的范围内，喹诺酮类药物为0-409.1微克/千克，0-6.56µg/kg大环内酯类，和0-4.9µg/kg的农药。此外，在被调查的20个地点中，有9个地点的杀虫剂和抗生素的同时出现可能对沉积居住的生物构成高风险。
