首页|期刊导航|中国渔业质量与标准|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

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OA

Determination of diazepam,malachite green,quinolones,and sulfonamides in aquatic products by UHPLC-MS/MS Combined with QuEChERS

中文摘要英文摘要

本研究基于QuEChERS前处理法结合超高效液相色谱质谱联用仪(UHPLC-MS/MS)建立了同时测定水产品中地西泮、孔雀石绿、喹诺酮类、磺胺类残留的分析方法.在样品中加入10 mL盐酸酸化乙腈、3g无水硫酸镁和2g氯化钠,同时加入150 mg PSA.涡旋提取1 min,超声波振荡10 min,8 000 r/min离心3 min,移取上清液至15 mL玻璃离心管中,40℃下氮吹至近干,1 mL乙腈水(1∶9,V/V)定容,过0.22 μm滤膜,待UHPLC-MS/MS 测定.结果显示地西泮、孔雀石绿的线性范围为0.5~20.0 ng/mL;磺胺类与喹诺酮类线性范围为5~200 ng/mL,水产品中地西泮、孔雀石绿检出限为0.2 μg/kg,定量限为0.5 μg/kg;磺胺类、喹诺酮检出限为0.5 μg/kg,定量限为1.0 μg/kg,平均回收率为71.3%~96.4%,测定值的相对标准偏差(n=6)为1.2%~8.2%.该方法在分析实际样品中显示,采用该方法对监督抽检200 批次水产品进行检测,其中2批次检测出恩诺沙星分别为50.5 μg/kg、48.6 μg/kg,其他化合物均未检出.该方法快速、灵敏、准确,适用于水产品中地西泮、孔雀石绿、喹诺酮类、磺胺类残留的测定.[中国渔业质量与标准,2025,15(1):26-36]。

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].

陈永平;成振华;李楠;韩现芹;时文博;王愿宁;苏梦寒

天津市农业生态环境监测与农产品质量检测中心,天津 300193天津市农业生态环境监测与农产品质量检测中心,天津 300193天津市水产研究所,天津 300221天津市农业生态环境监测与农产品质量检测中心,天津 300193天津市农业生态环境监测与农产品质量检测中心,天津 300193天津市农业生态环境监测与农产品质量检测中心,天津 300193天津市农业生态环境监测与农产品质量检测中心,天津 300193

轻工纺织

QuEChERSUHPLC-MS/MS水产品地西泮孔雀石绿喹诺酮类磺胺类

QuEChERSUHPLC-MS/MSaquatic productdiazepammalachite greenquinolonessulfonamides

《中国渔业质量与标准》 2025 (1)

26-36,11

天津市科技计划项目(24ZYCGSN01420)

10.3969/j.issn.2095-1833.2025.01.004

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