动物营养学报 >

2018 , Vol. 30 >Issue 6: 2394 - 2401

DOI: https://doi.org/10.3969/j.issn.1006-267x.2018.06.045

饲料检测 Feed Detection

固相萃取-超高效液相色谱-串联质谱法测定饲料中沃尼妙林和泰妙菌素

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  • 浙江大学饲料科学研究所, 浙江省饲料与动物营养重点实验室, 杭州 310058
王凤芹(1976-),女,湖北黄梅人,博士,从事动物营养与饲料分析方法建立研究。E-mail:wangfq@zju.edu.cn

收稿日期: 2018-01-26

  网络出版日期: 2018-06-20

基金资助

现代农业生猪产业体系（CARS-36）

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Determination of Valnemulin and Tiamulin in Feed by Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

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  • Key Laboratory of Animal Feed and Nutrition of Zhejiang Province, Feed Science Institute of Zhejiang University, Hangzhou 310058, China

Received date: 2018-01-26

  Online published: 2018-06-20

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摘要

本试验旨在建立一种高效快速测定饲料中沃尼妙林和泰妙菌素的固相萃取-超高效液相色谱-串联质谱方法。用甲醇提取饲料中的沃尼妙林和泰妙菌素，经过Oasis MCX固相萃取柱净化后，由C18色谱柱分离，流动相为水（含0.1%甲酸）-乙腈（含0.1%甲酸），梯度洗脱，以电喷雾离子源（ESI）正离子扫描方式，在多反应监测（MRM）模式下进行测定，外标法定量。结果表明：本试验建立的固相萃取-超高效液相色谱-串联质谱法对饲料中沃尼妙林和泰妙菌素的检测限分别为25.0和5.0 ng/g。沃尼妙林和泰妙菌素浓度在0.01~5.00 μg/mL范围内线性关系良好，相关系数（R2）均大于0.99。在3个添加水平（2.5、25.0、125.0 mg/kg）下，沃尼妙林的回收率为85.17%~94.55%，相对标准偏差（RSD）为2.56%~7.65%，泰妙菌素的回收率为84.69%~99.36%，RSD为1.57%~4.95%。结果表明，本试验建立的固相萃取-超高效液相色谱-串联质谱法操作简单、准确度高，可应用于饲料中沃尼妙林和泰妙菌素的快速定量测定。

关键词： 固相萃取; 超高效液相色谱-串联质谱; 饲料; 沃尼妙林; 泰妙菌素

本文引用格式

王凤芹, 杨媛媛, 陈楚昊, 胡喻涵, 路则庆, 汪以真 . 固相萃取-超高效液相色谱-串联质谱法测定饲料中沃尼妙林和泰妙菌素[J]. 动物营养学报, 2018 , 30(6) : 2394 -2401 . DOI: 10.3969/j.issn.1006-267x.2018.06.045

Abstract

This experiment was conducted to develop a fast and effective method for the determination of valnemulin and tiamulin in feed by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS). After the feed sample was extracted by methanol and cleaned-up on an Oasis MCX solid phase extraction (SPE) column, the valnemulin and tiamulin were separated by a C18 chromatographic column with gradient elution using 0.1% formic acid in water and 0.1% formic acid in acetonitrile as mobile phase, and finally quantified for the external standard method under the multiple reaction monitoring (MRM) mode in the positive ionization scanning mode using electrospray ionization (ESI). The results showed that the limit of detection (LOD) of the SPE-UPLC-MS/MS method developed in this experiment was 25.0 ng/g for valnemulin and 5.0 ng/g for tiamulin. The correlation coefficient of linear calibration curve for valnemulin and tiamulin was over 0.99 within the concentration range 0.01 to 5.00 μg/mL. At the three supplemental levels (2.5, 25.0 and 125.0 mg/kg), the recovery for the valnemulin was between 85.17% and 94.55% and the relative standard deviation (RSD) was from 2.56% to 7.65%; the recovery for the tiamulin was between 84.69% and 99.36% and the RSD was from 1.57% to 4.95%. The results showed that the SPE-UPLC-MS/MS method developed in this experiment is simple and sensitive, and it is fit for the rapid and quantitative determination of valnemulin and tiamulin in feed.

Key words： solid phase extraction; ultra performance liquid chromatography-tandem mass spectrometry; feed; valnemulin; tiamulin

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