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基于石墨化羧基多壁碳纳米管的QuEChERS萃取法测定家畜尿液中47种违禁药物及相关化学残留的液相色谱-串联质谱法的优化、验证及应用

Optimization, validation, and application of a liquid chromatography-tandem mass spectrometry method for the determination of 47 banned drug and related chemical residues in livestock urine using graphitized carboxyl multi-walled carbon nanotubes-based QuEChERS extraction.

作者信息

Su Youzhi, Lu Jianjiang, Liu Jun, Wang Ning, Li Fang, Lei Hongqin

机构信息

School of Chemistry and Chemical Engineering/Key Laboratory of Environmental Monitoring and Pollutant Control, Shihezi University, North 4th road NO.221, Shihezi 832003, China; Yining Customs Technology Center, Yining 83500, China.

School of Chemistry and Chemical Engineering/Key Laboratory of Environmental Monitoring and Pollutant Control, Shihezi University, North 4th road NO.221, Shihezi 832003, China.

出版信息

J Chromatogr A. 2024 Apr 26;1721:464858. doi: 10.1016/j.chroma.2024.464858. Epub 2024 Mar 30.

DOI:10.1016/j.chroma.2024.464858
PMID:38564928
Abstract

The establishment of an efficient method for the analysis of drug residues in animal urine facilitates the real-time monitoring of drugs used in the production of animal-derived food. A modified QuEChERS extraction-liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was established for the determination of 47 banned drug and related chemical residues in livestock urine. The sample was extracted with acetonitrile by converting the acid-base environment. The sample cleanup effects of seven solid phase extraction cartridges and two EMR-Lipid products were compared, and three materials, including graphitized carboxyl multi-walled carbon nanotubes (MWCNTs), PSA, and C, were selected as QuEChERS adsorbents from 24 materials. All analytes showed good linearity, with correlation coefficients (R) greater than 0.9936. Low limits of quantification could be obtained, ranging from 0.2 to 5.5 ng/mL. The average recoveries at low, medium, and high spiked levels were in the range of 70.8-114.9 %, with intra-day precision ranging from 2.4 % to 11.2 % and inter-day precision ranging from 4.5 % to 16.1 %. Swine urine and bovine urine samples collected from different farms were effectively analyzed using the developed method, and metronidazole was detected in three swine urine samples.

摘要

建立一种高效的动物尿液中药物残留分析方法,有助于对动物源性食品生产中使用的药物进行实时监测。建立了一种改进的QuEChERS萃取-液相色谱-串联质谱(LC-MS/MS)法,用于测定家畜尿液中47种违禁药物及相关化学残留。通过改变酸碱环境,用乙腈对样品进行萃取。比较了7种固相萃取柱和2种EMR-Lipid产品的样品净化效果,并从24种材料中选择了石墨化羧基多壁碳纳米管(MWCNT)、PSA和C三种材料作为QuEChERS吸附剂。所有分析物均表现出良好的线性,相关系数(R)大于0.9936。可获得较低的定量限,范围为0.2至5.5 ng/mL。低、中、高加标水平下的平均回收率在70.8-114.9%范围内,日内精密度在2.4%至11.2%之间,日间精密度在4.5%至16.1%之间。使用所建立的方法对从不同养殖场采集的猪尿和牛尿样品进行了有效分析,在三个猪尿样品中检测到了甲硝唑。

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引用本文的文献

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