超高效液相色谱-串联质谱法测定血豆腐中93种兽药残留  

Determination of 93 Veterinary Drug Residues in Blood Tofu by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：杜业刚[1] 张凯旋 李海玲 刘奕雄[1] 陶怡 朱雨田[1] DU Yegang;ZHANG Kaixuan;LI Hailing;LIU Yixiong;TAO Yi;ZHU Yutian(Shenzhen Academy of Metrology&Quality Inspection,National Nutrition Food Testing Center(Guangdong),Shenzhen 518100,China)

机构地区：[1]深圳市计量质量检测研究院,国家营养食品质量检验检测中心(广东),广东深圳518100

出　　处：《食品科技》2025年第1期308-316,共9页Food Science and Technology

基　　金：国家重点研发计划项目(2022YFF0607900);国家市场监管总局科技计划项目(2023MK143)。

摘　　要：目的:建立超高效液相色谱-串联质谱法测定血豆腐中93种兽药残留的分析方法。方法:血豆腐样品采用乙腈提取,PRiME HLB固相萃取柱净化,氮吹复溶后,采用ACQUITY UPLC BEH C_(18)色谱柱(50 mm×2.1 mm,1.7μm)进行分离,以甲醇和0.01%甲酸水溶液为流动相进行梯度洗脱,利用电喷雾离子源和多反应监测模式进行检测,基质匹配标准曲线外标法定量。结果:93种兽药在相应的浓度范围内线性关系良好,相关系数均大于0.990,定量限为0.1~10μg/kg。鸭血豆腐和猪血豆腐在低、中、高3个加标水平下的平均回收率为61.4%~118%,相对标准偏差(n=6)为1.27%~19.2%。结论:该方法简便、灵敏度高、准确度高,可用于血豆腐中93种兽药残留的测定。Objective:To establish a method for determination of 93 veterinary drug residues in blood tofu by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods:The blood tofu samples were extracted by acetonitrile,purified by PRiME HLB solid-phase extraction column,and dissolved again after nitrogen blowing.The separation was achieved using an ACQUITY UPLC BEH C_(18)column(50 mm×2.1 mm,1.7μm)with methanol and 0.01%formic acid solution as mobile phase for gradient elution.Detection was performed by use of electrospray ionization(ESI)and multiple reaction monitoring(MRM)mode,and the matrix matched calibration curve method was used for quantification.Results:The calibration curves for the 93 veterinary drugs showed good linearity within their corresponded concentration ranges,with correlation coefficients greater than 0.990.The limits of quantification ranged from 0.1μg/kg to 10μg/kg.The average recoveries of duck blood tofu and pig blood tofu at low,medium and high levels were 61.4%–118%,and the relative standard deviations were 1.27%–19.2%(n=6).Conclusion:This method has the advantages of simple,high sensitivity and high accuracy,and can be applied to the determination of 93 veterinary drug residues in blood tofu.

关 键 词：超高效液相色谱-串联质谱法 血豆腐 兽药残留 

分 类 号：TS207.53[轻工技术与工程—食品科学]