中国渔业质量与标准2025，Vol.15Issue(1)：26-36,11.DOI:10.3969/j.issn.2095-1833.2025.01.004
QuEChERS结合UHPLC-MS/MS法同时测定水产品地西泮、孔雀石绿、喹诺酮类、磺胺类药物残留
Determination of diazepam,malachite green,quinolones,and sulfonamides in aquatic products by UHPLC-MS/MS Combined with QuEChERS
摘要
Abstract
An analytical method for the simultaneous determination of residues of diazepam,malachite green,quinolo-nes,and sulfonamides in aquatic products based on QuEChERS pretreatment combined with ultra-high performance liquid chromatography-mass spectrometry(UHPLC-MS/MS)was established.The results showed that 10 mL of hydrochloric acid acidified acetonitrile,3 g of MgSO4,2 g of NaCl and 150 mg of PSA were added.After Vortex ex-traction for 1 minute,ultrasonic oscillation for 10 minutes,centrifugation at 8000 r/min for 3 minutes,the superna-tant was transfered to a 15 mL glass centrifuge tube.using nitrogen blew to near dryness at 40℃which was diluted with 1.0 mL acetonitrile water(1∶9,V/V),and passed through a 0.22 μm microfiltration membrane waiting for UH-PLC-MS/MS determination.The results showed that the linear range of diazepam and malachite green was0.5-20 ng/mL;The linear range for sulfonamides and quinolones was 5-200 ng/mL.The detection limit for diazepam and malachite green in aquatic products is 0.2 μg/kg,and the quantification limit was 0.5 μg/kg;The detection limit of sulfonamides and quinolones was 0.5 μg/kg,the quantification limit is 1.0 μg/kg,the average recovery was 71.3%-96.4%,and the relative standard deviation of the measured values(n=6)was 1.2%-8.2%.The method was used to analyze actual samples,and the results showed that this method was used to detect 200 samples under supervi-sion.Among them,enrofloxacin was detected at 50.5 μg/kg and 48.6 μg/kg in 2 samples,respectively,and no oth-er compounds were detected.This method was fast,sensitive,and accurate,and is suitable for the determination of residues of diazepam,malachite green,quinolones,and sulfonamides in aquatic products.[Chinese Fishery Quality and Standards,2025,15(1):26-36].关键词
QuEChERS/UHPLC-MS/MS/水产品/地西泮/孔雀石绿/喹诺酮类/磺胺类Key words
QuEChERS/UHPLC-MS/MS/aquatic product/diazepam/malachite green/quinolones/sulfonamides分类
轻工业引用本文复制引用
陈永平,成振华,李楠,韩现芹,时文博,王愿宁,苏梦寒..QuEChERS结合UHPLC-MS/MS法同时测定水产品地西泮、孔雀石绿、喹诺酮类、磺胺类药物残留[J].中国渔业质量与标准,2025,15(1):26-36,11.基金项目
天津市科技计划项目(24ZYCGSN01420) （24ZYCGSN01420）
