高邮养殖区罗氏沼虾中多种抗生素的残留与膳食暴露评估

Residues and dietary exposure assessment of antibiotics in Macrobrachium rosenbergii in Gaoyou aquaculture area

对高邮市9个养殖区的45个罗氏沼虾(Macrobrachium rosenbergii)样品中的4类(磺胺类、喹诺酮类、四环素类及大环内脂类)39种抗生素残留进行快速筛查验证,分析残留现状与健康风险.样品罗氏沼虾经酸化乙腈和乙二胺四乙酸二钠提取浓缩后,再经正己烷去脂,应用液相色谱-三重四级杆复合线性离子阱质谱(LC-Q-TRAP/MS)技术,采用内标法定量和分段时间多反应监测-信息关联采集-增强离子扫描的方式(sMRM-IDA-EPI),进行定性和定量分析.结果表明,9个养殖区抗生素残留中磺胺类、四环素类和大环内酯类均未检出,喹诺酮类抗生素洛美沙星、培氟沙星、氧氟沙星和诺氟沙星4种禁用兽药均未检出,仅有环丙沙星、恩诺沙星及达氟沙星被检出,检出率分别为44.4%、82.2%和51.1%,总体合格率为93.3%.达氟沙星含量较小,平均含量范围在ND(未检出)~9.00μg/kg.恩诺沙星和环丙沙星总量范围在N.D.~157.00μg/kg,个别养殖区组(SQZ组和SDZ组)内检出率100%,其中3个样品超过限量值100μg/kg.使用每日允许摄入量(acceptable daily intake,ADI)和估计日摄入量(estimated daily intake,EDI)评价膳食安全,喹诺酮类(恩诺沙星和环丙沙星)、达氟沙星暴露风险(EDI/ADI)值在1.66×10^-5~8.06×10^-3范围内,表明9个养殖区罗氏沼虾虾体膳食暴露评估风险水平在可接受范围内,对人体造成健康风险的可能性较小.研究认为,高邮养殖区罗氏沼虾中抗生素污染程度较轻,罗氏沼虾中喹诺酮类药物残留量较高,经膳食暴露评估尚在安全范围内,建议进一步加强高邮地区罗氏沼虾等养殖水产品中喹诺酮类等抗生素的监控管理.

39 antibiotics residues of 4 kinds, i.e. sulfonamides, quinolones, tetracyclines and macrolides, in 45 samples of Macrobrachium rosenbergii from 9 aquaculture areas in Gaoyou city were screened and validated in this study. The status of residues and health risks were analyzed and evaluated. Firstly, the samples of Macrobrachium rosenbergii was extracted and concentrated by acidified acetonitrile and disodium ethylene diamine tetraacetate, and then degreased with n-hexane. The qualitative and quantitative analysis was performed using high performance liquid chromatography-triple quadrupole-linear ion trap mass spectrometry(LC-Q-TRAP/MS) based on scheduled-multiple reaction monitoring with information correlation information-dependent acquisition of enhanced product ion(SMRM-IDA-EPI). The internal standard method was adopted to achieve quantitative analysis. Sulfonamides, tetracyclines and macrolides were not detected in antibiotic residues in 9 aquaculture areas. The four prohibited veterinary drugs, i.e. lomefloxacin, pefloxacin, ofloxacin and norfloxacin, were not detected. And only ciprofloxacin, enrofloxacin and dafloxacin were detected in quinolone antibiotics, whose detection frequencies were 44.4 %, 82.2 % and 51.1%, respectively, and the overall eligibility rate was 93.3%. The content of dafloxacin was relatively low, with an average N.D.(not detected) ~9.00 μg/kg. The total amount of enrofloxacin and ciprofloxacin ranged from N.D. to 157.00 μg/kg, whose detection frequency was 100% in a few aquaculture areas(SQZ and SDZ groups), and three samples exceeded the limit value of 100 μg/kg. Considering that the related drugs were added artificially, and the qualified rate was still high, ADI(acceptable daily intake) and EDI(estimated daily intake) values were used to evaluate dietary safety. The exposure risks(EDI/ADI) of quinolones(enrofloxacin and ciprofloxacin) and ofloxacin were in the range of 1.66×10^-5~8.06×10^-3. It showed that the risk level of dietary exposure assessment of Macrobrachium rosenbergii from 9 farming areas was acceptable and there was not health risk. In conclusion, the antibiotic pollution in Macrobrachium rosenbergii in Gaoyou aquaculture area is relatively light. And only quinolones residues are relatively high, which is still within the safe range after dietary exposure assessment. It is suggested to further strengthen the monitoring and management of quinolones in aquatic products such as Macrobrachium rosenbergii in Gaoyou area.