摘要
为有效监测牛肉、肝和肾中抗菌药物多残留水平,提升风险隐患的排查能力,建立一种快速测定牛肉、肝和肾中9种药物残留的高效液相色谱-串联质谱法(HPLC-MS/MS),药物涉及大环内酯类、磺胺类、喹诺酮类、四环素类、氨基糖苷类共5大类。通过比较提取溶剂、提取次数、称取重量和净化柱选择对9种抗菌药提取效果的影响,考察牛肉组织的基质效应,确定最优的检测条件为:称取2.5 g,采用Mcllvaine-Na 2 EDTA-甲酸-乙腈溶液提取2次,提取液经HLB柱净化,使用C18柱(50 mm×2.1 mm,1.8μL)色谱柱分离,以0.1%甲酸水溶液和甲醇为流动相进行梯度洗脱,采用电喷雾电离(ESI)和多反应监测(MRM)模式检测,基质外标法定量。结果显示,9种抗菌药物在相应线性范围内R^(2)均大于0.99,检出限为0.1~0.5μg/kg,定量限为0.5~2μg/kg;在0.5~200μg/kg添加浓度范围内,平均回收率为71.65%~118.59%,相对标准偏差(RSD)为0.14%~9.57%。建立了牛肉、肝和肾中9种药物残留检测的高效液相色谱串联质谱法,该方法灵敏准确,适用于牛肉、肝和肾3种产品中9种抗菌药物的残留检测。
To effectively monitor the multi residue levels of antimicrobials in beef,liver and kidney,and improve the ability to identify risk hazards,a high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method was established for the rapid determination of 9 drug residues in beef,liver and kidney.involving five major categories of macrolides,sulfonamides,quinolones,tetracyclines and aminoglycosides.The effects of extraction solvent,extraction times,weighing weight and purification column selection on the extraction effect of nine antimicrobial drugs were compared,the matrix effect of beef tissue was investigated,and the optimal experimental conditions were determined as follows:2.5 g was weighed,extracted twice by Mcllvaine-Na 2 EDTA-formic acid-acetonitrile solution,the extract was purified by HLB column,separated by C18 column(50 mm×2.1 mm,1.8μL)chromatographic column,and gradient elution was carried out with 0.1%formic acid aqueous solution and methanol as mobile phase.Electrospray ionization(ESI)and multi-reaction monitoring(MRM)modes were used for detection,and matrix external standard method was used for quantification.The results showed that the R 2 of the nine antimicrobial drugs was greater than 0.99 in the corresponding linear range,the detection limit was 0.1-0.5μg/kg,and the quantitative limit was 0.5-2μg/kg.In the range of 0.5-200μg/kg concentration,the average recovery rate was 71.65%-118.59%,and the relative standard deviation(RSD)was 0.14%-9.57%.A high-performance liquid chromatography tandem mass spectrometry method for the detection of 9 drug residues in beef,liver and kidney was established,which was sensitive and accurate,and was suitable for the detection of 9 antimicrobial residues in 3 products of beef,liver and kidney.
作者
张浩浩
芝吉
赵学慧
何曾文
范子秋
马永辉
马金锐
邓静
张坤中
崇倩
曹青
薛慧文
苟惠天
ZHANG Hao-hao;ZHI Ji;ZHAO Xue-hui;HE Zeng-wen;FAN Zi-qiu;MA Yong-hui;MA Jin-rui;DENG Jing;ZHANG Kun-zhong;CHONG Qian;CAO Qing;XUE Hui-wen;GOU Hui-tian(College of Veterinary Medicine,Gansu Agricultural University,Lanzhou,Gansu,730070,China)
出处
《动物医学进展》
北大核心
2024年第12期44-52,共9页
Progress In Veterinary Medicine
基金
国家重点研发计划项目(2019YFC1605705-2)。
