液相色谱质谱法检测土壤中7种典型抗生素残留  

Determination of seven typical antibiotic residues in soil by liquid chromatography-mass spectrometry

作　　者：杨萌 YANG Meng(He’nan Nanyang Ecological Environment Monitoring Center,Nanyang 473000,China)

机构地区：[1]河南省南阳生态环境监测中心,河南南阳473000

出　　处：《中国测试》2023年第7期76-81,共6页China Measurement & Test

摘　　要：该文研究建立加速溶剂提取法提取土壤中的青霉素、阿米卡星、万古霉素、头孢拉定、磺胺嘧啶、氟苯尼考、阿莫西林,凝胶净化色谱法富集、净化待测物,超高压液相色谱-三重四级杆串联质谱定性、定量检测的分析方法。检测过程为随机取有代表性土壤样品,自然风干,粉碎,过筛网。准确称取15.0 g,置萃取池中,加硅藻土20.0 g,混均,甲醇-丙酮=1∶2(V∶V)作为提取溶剂进行提取,提取液冷冻离心,上清液转移至GPC净化瓶中,上GPC仪进行富集、净化;净化液氮吹至近干,加1 mL甲醇溶解,过滤,上UPLC-MS/MS仪定性、定量检测。青霉素、阿米卡星、万古霉素、头孢拉定、磺胺嘧啶、氟苯尼考、阿莫西林7种待测物在0.01~5.0μg/mL范围内线性良好,检出限在0.007~0.041μg/kg之间,三水平加样回收率范围在85.4%~105.2%之间。实验结果证明,该方法具有自动化程度高、检测准确度高和重复性好等特点,可以用于被抗生素污染的土壤中极微量抗生素残留的监测和风险评估。An ASE extraction method was developed for the determination of 7 antibiotics(penicillin,amikacin,vancomycin,cefradine,sulfadiazine,florfenicol,amoxicillin)residues in soil.Gel purification chromatography is used to enrich and purify the matter to be measured,qualitative and quantitative detection were carried out by ultra high pressure liquid chromatography-triple quadrupole tandem mass spectrometry.Representative soil samples were randomly selected,dried naturally,crushed,and screened.15.0 g samples were accurately weighed,and submitted to solvent extraction tank with the addition of 20.0 g diatomite,then the mixture was extracted by methanol-acetone=1:2(V:V)solution.The extracted liquid was frozen and centrifuged,and the supernatant was transferred to GPC purification bottle for enrichment and purification.The purged liquor was blown to nearly dry.The residue was dissolved by 1 mL methanol and filtered.Then samples were qualitatively and quantitatively detected by UPLC-MS/MS.Penicillin,amikacin,vancomycin,cefradine,sulfadiazine,florfenicol and amoxicillin showed good linear relationships in the concentration ranges of 0.01-5.0μg/mL,the detection limits were ranged from 0.007μg/kg to 0.041μg/kg.The average recoveries in 3 concentration levels were 85.4%to 105.2%.The experimental results show that the method has the characteristics of high automation,high detection accuracy and good repeatability,and can be used for monitoring and risk assessment of extremely small amounts of antibiotic residues in soil contaminated by antibiotics.

关 键 词：超高压液相色谱-三重四级杆串联质谱法 土壤 加速溶剂提取 抗生素残留 

分 类 号：O657.63[理学—分析化学] X833[理学—化学]