哈尔滨蔬菜基地土壤中喹诺酮类抗生素的污染现状
Pollution Status of Quinolones Antibiotics in Soil of Harbin Vegetable Base
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摘要: 建立超高效液相色谱-紫外检测（LC-UV）结合质谱检测（MS）法测定哈尔滨周边蔬菜基地土壤中喹诺酮类抗生素残留，并对其生态风险进行评估。样品经乙腈-磷酸盐缓冲液提取，C18固相萃取小柱富集、净化后用甲醇洗脱液进行洗脱。采用多反应监测负离子模式内标法检测蔬菜基地土壤中喹诺酮类抗生素残留。确定最佳提取条件，包括样品提取时间、温度和提取溶剂量等。4种喹诺酮类抗生素在相关范围内线性关系良好，相关系数为0.9994~0.9997。4种喹诺酮类抗生素的加标样品检测值的相对标准偏差为1.13%~2.15%，加标回收率为68.1%~80.2%。哈尔滨蔬菜基地土壤中检出的喹诺酮类抗生素残留浓度范围为21.73~132.45 μg·kg-1，双城蔬菜基地中仅检测出环丙沙星（CIP），为116.53 μg·kg-1；五常蔬菜基地检测出环丙沙星和诺氟沙星（NOR），其中环丙沙星的检出量最高，为132.45 μg·kg-1；平房蔬菜基地检测出环丙沙星和恩诺沙星（ENR），残留量分别为128.54 μg·kg-1和21.73 μg·kg-1；呼兰蔬菜基地土壤中环丙沙星、恩诺沙星、洛美沙星（LOM）和诺氟沙星均被检出，浓度分别为20.54、120.35、37.41和37.41 μg·kg-1。生态风险评估结果表明，土壤中检测出的抗生素的风险商（RQ）值均≥1，表现出高度风险，对生态系统具有潜在的不利影响。Abstract: An ultra-high performance liquid chromatography-ultraviolet detection (LC-UV) combined with mass spectrometry (MS) method was established to determine quinolone antibiotic residues in the soil of vegetable bases around Harbin, and to evaluated their ecological risks. The samples were extracted with acetonitrile-phosphate buffer, enriched and purified by C18 solid phase extraction cartridge, and eluted with methanol eluent. Multiple reaction monitoring negative ion mode internal standard method was used to detect quinolone antibiotic residues in vegetable base soil. In this experiment, the sample extraction time, temperature and extraction solvent were tested to determine the optimal extraction conditions. The four quinolone antibiotics had a good linear relationship in the relevant range, with correlation coefficients ranging from 0.9994 to 0.9997. The relative standard deviations of the spiked samples of the four quinolone antibiotics were 1.13%~2.15%, and the spiked recoveries were 68.1%~80.2%. The residual concentrations of quinolone antibiotic in the soil of Harbin vegetable base ranged from 21.73 to 132.45 μg·kg-1, and only ciprofloxacin (CIP) was detected in Shuangcheng vegetable base at 116.53 μg·kg-1. Ciprofloxacin and norfloxacin (NOR) were detected in Wuchang vegetable base, with the highest detection amount of ciprofloxacin at 132.45 μg·kg-1. Ciprofloxacin and enrofloxacin (ENR) were detected in Pingfang vegetable base, and the residues were 128.54 μg·kg-1 and 21.73 μg·kg-1, respectively. Ciprofloxacin, enrofloxacin, lomefloxacin (LOM), and norfloxacin were all detected in the soil of Hulan vegetable base, with concentrations of 20.54, 120.35, 37.41 and 37.41 μg·kg-1. The ecological risk assessment results showed that the risk quotient (RQ) values of antibiotics detected in the soil were all greater than 1, showing a high risk and potential adverse effects on ecosystems.
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