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高效液相色谱-串联质谱法测定猪毛中莱克多巴胺和沙丁胺醇

Determination of ractopamine and salbutamol in pig hair by liquid chromatography tandem mass spectrometry.

机构信息

Division of Animal Industry, Agricultural Technology Research Institute, Miaoli, Taiwan.

Department of Veterinary Medicine, College of Veterinary Medicine, National Pingtung University of Science and Technology, Pingtung, Taiwan.

出版信息

J Food Drug Anal. 2018 Apr;26(2):725-730. doi: 10.1016/j.jfda.2017.09.005. Epub 2017 Nov 12.

Abstract

A liquid chromatography tandem mass spectrometric method was developed for the determination of two β-agonists (ractopamine and salbutamol) in pig hair samples. An isotope of ractopamine-d5 or salbutamol-d6 as an internal standard was used to carry out quantitative analysis. Concentrated sodium hydroxide was used to pretreat hair samples and then purified by the solid phase extraction (SPE) procedure. The extracted solution was evaporated and reconstituted for injection in the instrument with electrospray ionization (ESI) operating in a positive multiple-reaction-monitoring (MRM) mode. Ractopamine and salbutamol separation were performed on C18 analytical column under gradient condition. The internal standard calibration curve was linear in the range of concentration from 0.5 to 100 ng mL (R > 0.995). Recoveries of this method estimated at three spiked concentrations of 100, 250 and 500 ng mL in pig hair samples, were 79-82% for ractopamine and 77-96% for salbutamol. The corresponding inter-day and intra-day precisions expressed as relative standard deviation (RSD %) were 3.8-6.4% and 3.8-8.6%, respectively. The analytical time for one sample was 8 min. The detection limit of this method was 0.6 and 8.3 ng mL for ractopamine and salbutamol, respectively. This developed method can be applied for monitoring the use of the β-agonists salbutamol and ractopamine in swine feed incurred pig hair.

摘要

建立了一种用于测定猪毛样品中两种β-激动剂(莱克多巴胺和沙丁胺醇)的液相色谱-串联质谱分析方法。采用莱克多巴胺-d5 或沙丁胺醇-d6 作为内标进行定量分析。采用浓氢氧化钠预处理毛发样品,然后通过固相萃取(SPE)程序进行纯化。提取溶液经蒸发后,用电喷雾电离(ESI)在正多重反应监测(MRM)模式下进行仪器进样。莱克多巴胺和沙丁胺醇在 C18 分析柱上在梯度条件下进行分离。内标校准曲线在浓度为 0.5 至 100ngmL-1 范围内呈线性(R>0.995)。在猪毛样品中三个添加浓度(100、250 和 500ngmL-1)下,该方法的回收率估计为莱克多巴胺 79-82%,沙丁胺醇 77-96%。日内和日间精密度分别表示为相对标准偏差(RSD%)为 3.8-6.4%和 3.8-8.6%。每个样品的分析时间为 8 分钟。该方法的检测限为莱克多巴胺和沙丁胺醇分别为 0.6 和 8.3ngmL-1。该方法可用于监测猪饲料中β-激动剂沙丁胺醇和莱克多巴胺在猪毛中的使用情况。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/a69a/9322239/3d0aa65b171b/jfda-26-02-725f1.jpg

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