高效液相色谱-串联质谱法测定奶豆腐中6种喹诺酮类药物残留研究  

The determination of six quinolone drug residues in milk tofu by high-performance liquid chromatography-tandem mass spectrometry

作　　者：王雪奇 张学富 杨晓磊 宋丽华[4] 杨宇昊 李向阳[1] WANG Xueqi;ZHANG Xuefu;YANG Xiaolei;SONG Lihua;YANG Yuhao;LI Xiangyang(College of Animal Science and Technology,Inner Mongolia Universityfor Nationalities,Inner Mongolia Tongliao 028000,China;Analysis and Testing Center,Inner Mongolia University for Nationalities,Inner Mongolia Tongliao 028000,China;Food Room of Tongliao Food and Drug Inspection Institute,Inner Mongolia Tongliao 028000,China;Affiliated Hospital of Inner Mongolia University for Nationalities,Inner Mongolia Tongliao 028000,China)

机构地区：[1]内蒙古民族大学动物科技学院,内蒙古通辽028000 [2]内蒙古民族大学分析测试中心,内蒙古通辽028000 [3]通辽食品药品检验所食品室,内蒙古通辽028000 [4]内蒙古民族大学附属医院,内蒙古通辽028000

出　　处：《中国食品卫生杂志》2023年第3期339-345,共7页Chinese Journal of Food Hygiene

基　　金：内蒙古自治区科技创新引导项目(KJCX2001)。

摘　　要：目的建立动物源性食品奶豆腐中6种喹诺酮类药物残留的高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。方法奶豆腐样品经0.1 mmol/L EDTA-Mcllvaine缓冲液处理并加入亚铁氰化氢、乙酸锌各0.1 mL提取,HLB Pro固相萃取柱净化,经Shim-pack FC-ODS(150 mm×20 mm,3μm)分离,用10 mmol/L乙酸铵(含0.1%甲酸)-甲醇乙腈(40:60,V/V)进行梯度洗脱,在全扫描(full MS)模式检测。结果6种喹诺酮类药物在10~100 ng/mL的浓度范围内线性良好,相关系数(R^(2))均大于0.995;检出限(LOD)为0.5~1.5μg/kg,定量限为(LOQ)2~4μg/kg,加标回收率为82.3%~101.6%,相对标准差低于10%。结论该方法灵敏度高、快速、准确,适用于奶豆腐中6种喹诺酮类药物的快速筛查和定量定性分析。Objective To establish a high-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the detection of 6 quinolones residues in milk tofu.Methods The milk tofu sample was extracted with 0.1 mmol/L EDTA-Mcllvaine buffer with 0.1 mL each of ferrocyanide and zinc acetate,purified by HLB Pro solid phase extraction column,and separated by Shim-pack FC-ODS(150 mm×20 mm,3μm),gradient eluted by 10 mmol/L ammonium acetate(containing 0.1%formic acid)-methanol acetonitrile(40:60,V/V),and detected in full scan(full MS)mode.Results The results showed that the 6 quinolones had good linearity in the concentration range of 10-100 ng/mL,the correlation coefficient(R^(2))was all above 0.995,the limit of detection(LOD)was 0.5-1.5μg/kg,the limit of quantification(LOQ)was 2-4μg/kg,the recovery rate of spiked sample was 82.3%-101.6%,and the relative standard deviation was less than 10%.Conclusion This method is highly sensitive,rapid and accurate,and suitable for rapid screening,quantitative and qualitative analysis of 6 quinolones in milk tofu.

关 键 词：UPLC-MS/MS 喹诺酮 奶豆腐 药物残留 

分 类 号：R155[医药卫生—营养与食品卫生学]