快速滤过型净化结合超高效液相色谱—串联质谱法同时测定水产品中10种药物残留量OA
Simultaneous Determination of 10 Drug Residues in Aquatic Products Using Multi-plug Filtration Cleanup Coupled with Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry
建立了快速滤过型净化(m-PFC)技术结合超高效液相色谱—串联质谱法(UPLC-MS/MS)同时测定水产品中喹诺酮类、氯霉素及地西泮等10种药物残留的分析方法.样品经0.2 mol·L-1乙酸铵浸润后,采用1％甲酸—乙腈提取并高速冷冻离心,上清液经m-PFC柱净化后进行UPLC-MS/MS分析.质谱采用电喷雾正负离子模式及多反应监测模式采集数据,基质匹配标准曲线定量.结果表明,10种药物在0.5～50 μg·L-1范围内线性关系良好(r＞0.999),定量限为1 μg·kg-1,检出限为0.2～0.4 μg·kg-1.在1～100μg·kg-1添加水平下,平均回收率为76.2％～108.4％,相对标准偏差为2.6％～6.8％.此方法操作简便、灵敏度高且准确度好,适用于大批量水产品10种药物的快速定量检测.
An analytical method based on multi-plug filtration cleanup(m-PFC)coupled with ultra-high performance liquid chromatography-tandem mass spectrometry was developed for the simultaneous de-termination of 10 drug residues,including quinolones,chloramphenicol and diazepam,in aquatic prod-ucts.Samples were extracted with 1％formic acid in acetonitrile after pretreatment with ammonium acetate solution,followed by high-speed freezing centrifugation and m-PFC purification.Detection was performed using electrospray ionization in positive and negative modes with multiple reaction monito-ring,and quantification was based on matrix-matched calibration.The method showed good linearity(r＞0.999)in the range of 0.5～50 μg·L-1,with a limit of quantification of 1 μg·kg-1and detection limits of 0.2～0.4 μg·kg-1.At three spiked levels(1,10,and 100 μg·kg-1),the average recoveries ranged from 76.2％to 108.4％,with relative standard deviations of 2.6％～6.8％.The proposed methodis simple,sensitive,accurate and suitable for high-throughput rapid detection of multi-drug residues in aquatic products.
杜鑫;易珊珊;陈伟成;覃明丽
南充农产品质量监测检验中心,四川南充 637000南充农产品质量监测检验中心,四川南充 637000南充农产品质量监测检验中心,四川南充 637000南充农产品质量监测检验中心,四川南充 637000
化学化工
快速滤过型净化喹诺酮类地西泮氯霉素水产品
Multi-plug filtration cleanup(m-PFC)QuinolonesDiazepamChloramphenicolAquatic products
《云南师范大学学报（自然科学版）》 2026 (3)
33-40,8
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