摘要
采用改良的QuEChERS法进行前处理,建立了超高效液相色谱-串联质谱同时测定禽蛋(鸡蛋、鹅蛋、鸭蛋)中9类31种产蛋期禁用兽药(大环内酯类、解热镇痛类、磺胺类、抗菌增效类、抗球虫类、抗线虫类、喹诺酮类、四环素类、酰胺醇类)的检测方法,并对样品前处理和色谱条件进行了优化。称取2.00 g样品,先加入2 mL 0.1 mol/L乙二胺四乙酸二钠溶液,涡旋1 min,将样品充分分散,再用8 mL 3%乙酸乙腈提取,氯化钠(2 g)盐析,离心后,上清液采用十八烷基硅烷键合硅胶(C_(18), 100 mg)、N-丙基乙二胺(PSA, 50 mg)和氨基(NH_2, 50 mg)吸附剂联合净化,待测分析物经Waters CORTECS UPLC C_(18)色谱柱(150 mm×2.1 mm, 1.8μm)分离,分别在正、负离子模式下采集,空白基质匹配标准曲线外标法定量。结果表明,31种产蛋期禁用兽药在相应浓度范围内具有良好的线性关系,相关系数>0.99,检出限为0.3~3.0μg/kg,定量限为1.0~10.0μg/kg。在定量限、最大残留限量、2倍最大残留限量3个添加水平下,3种禽蛋基质中31种产蛋期禁用兽药的平均加标回收率为61.2%~105.7%,相对标准偏差为1.8%~17.6%(n=6)。利用所建立的方法对30份禽蛋样品(20份鸡蛋、5份鹅蛋和5份鸭蛋)进行检测,共有1份样品检出恩诺沙星。本方法简单、经济、实用,适用于禽蛋中多类产蛋期禁用兽药的同时测定。
The consumption of poultry eggs has increased in recent years owing to the abundance of production and improvements in living standards.Thus,the safety requirements of poultry eggs have gradually increased.At present,few reports on analytical methods to determine banned veterinary drugs during egg-laying period in poultry eggs have been published.Therefore,establishing high-throughput and efficient screening methods to monitor banned veterinary drugs during egg-laying period is imperative.In this study,an analytical method based on ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)combined with QuEChERS-based techniques was developed for the simultaneous determination of 31 banned veterinary drugs encompassing nine drug classes(macrolides,antipyretic and analgesic drugs,sulfonamides,antibacterial synergists,anticoccidials,antinematodes,quinolones,tetracyclines,amphenicols)in different types of poultry eggs.The main factors affecting the response,recovery,and sensitivity of the method,such as the extraction solvent,purification adsorbent,LC separation conditions,and MS/MS parameters,were optimized during sample pretreatment and instrumental analysis.The 31 veterinary drug residues in 2.00 g eggs were extracted with 2 mL of 0.1 mol/L ethylene diamine tetraacetic acid disodium solution and 8 mL 3%acetic acid acetonitrile solution,and salted out with 2 g of sodium chloride.After centrifugation,5 mL of the supernatant was cleaned-up using the QuEChERS method with 100 mg of octadecylsilane-bonded silica gel(C 18),50 mg of N-propylethylenediamine(PSA),and 50 mg of NH 2-based sorbents.After nitrogen blowing and redissolution,the 31 target analytes were separated on a Waters CORTECS UPLC C 18 analytical chromatographic column(150 mm×2.1 mm,1.8μm)at a flow rate,column temperature,and injection volume of 0.4 mL/min,30℃,and 5μL,respectively.Among these analytes,26 analytes were acquired in dynamic multiple reaction monitoring(MRM)mode under positive electrospray ionization(ESI+)conditions using(A)5 mmol/L ammonium acetate(pH 4.5)and(B)acetonitrile as mobile phases.The gradient elution program was as follows:0-2.0 min,12%B-30%B;2.0-7.5 min,30%B-50%B;7.5-10.0 min,50%B;10.0-10.1 min,50%B-100%B;10.1-12.0 min,100%B;12.0-12.1 min,100%B-12%B;The five other target analytes were acquired in MRM mode under negative electrospray ionization(ESI-)conditions using(A)H 2O and(B)acetonitrile as mobile phases.The gradient elution program was as follows:0-2.0 min,12%B-40%B;2.0-6.0 min,40%B-80%B;6.0-6.1 min,80%B-100%B;6.1-8.0 min,100%B;8.0-8.1 min,100%B-12%B.Matrix-matched external standard calibration was used for quantification.The results showed that all the compounds had good linear relationships within their respective ranges,with correlation coefficients of>0.99.The limits of detection(LODs)and quantitation(LOQs)were 0.3-3.0μg/kg and 1.0-10.0μg/kg,respectively.The average recoveries of the 31 banned veterinary drugs spiked at three levels(LOQ,maximum residue limit(MRL),and 2MRL)in poultry eggs ranged from 61.2%to 105.7%,and the relative standard deviations(RSDs)ranged from 1.8%to 17.6%.The developed method was used to detect and analyze banned veterinary drugs in 30 commercial poultry egg samples,including 20 eggs,5 duck eggs,and 5 goose eggs.Enrofloxacin was detected in one egg with a content of 12.3μg/kg.The proposed method is simple,economical,practical,and capable of the simultaneous determination of multiple classes of banned veterinary drugs in poultry eggs.
作者
朱万燕
张鸿伟
车立志
徐文远
伦才智
徐久飞
徐豪
陈伟
ZHU Wanyan;ZHANG Hongwei;CHE Lizhi;XU Wenyuan;LUN Caizhi;XU Jiufei;XU Hao;CHEN Wei(Comprehensive Technology Center of Linyi Customs,Linyi 276034,China;Technology Center of Qingdao Customs,Qingdao 266109,China)
出处
《色谱》
CAS
CSCD
北大核心
2024年第5期420-431,共12页
Chinese Journal of Chromatography
基金
青岛市民生科技计划项目(18-6-1-107-nsh)
青岛海关科研项目(QK202017)。
关键词
超高效液相色谱-串联质谱
QUECHERS
兽药
禽蛋
ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
QuEChERS
veterinary drugs
poultry egg
