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
作者:
作者单位:

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

作者简介:

王雪奇 男 硕士研究生 研究方向为食品药物残留 E-mail:xueqi1994wang@163.com

通讯作者:

李向阳 男 教授 研究方向为食品药物残留检测技术及标准研究 E-mail:13904752248@139.com

中图分类号:

R155

基金项目:

内蒙古自治区科技创新引导项目(KJCX2001)


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

1.College of Animal Science and Technology, Inner Mongolia Universityfor Nationalities, Inner Mongolia Tongliao 028000, China;2.Analysis and Testing Center, Inner Mongolia University for Nationalities, Inner Mongolia Tongliao 028000, China;3.Food Room of Tongliao Food and Drug Inspection Institute, Inner Mongolia Tongliao 028000, China;4.Affiliated Hospital of Inner Mongolia University for Nationalities, Inner Mongolia Tongliao 028000, China

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    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,3 μm)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(R2)均大于0.995;检出限(LOD)为0.5~1.5 μg/kg,定量限为(LOQ)2~4 μg/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。

    Abstract:

    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, 3 μm), 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 (R2) was all above 0.995, the limit of detection (LOD) was 0.5-1.5 μg/kg, the limit of quantification (LOQ) was 2-4 μg/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.

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王雪奇,张学富,杨晓磊,宋丽华,杨宇昊,李向阳.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[J].中国食品卫生杂志,2023,35(3):339-345.

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  • 收稿日期:2021-09-28
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  • 在线发布日期: 2023-05-24
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