脂质去除分散固相萃取-超高效液相色谱-串联质谱法测定动物源性食品中5种α2-受体激动剂

doi:10.19894/j.issn.1000-0518.200295

摘要/Abstract

摘要： 采用增强型脂质去除吸附剂(Enhanced Matrix Removal-lipid,EMR-Lipid)对样品进行净化,结合超高效液相色谱-串联质谱(UPLC-MS/MS)检测,建立快速测定动物源性食品中5种α₂-受体激动剂(安普乐定、溴莫尼定、替扎尼定、可乐定、赛拉嗪)的方法。对样品前处理方式、质谱及色谱条件进行了优化,样品经2.0%氨水溶液充分分散,5种α₂-受体激动剂经乙腈提取,所得提取液经萃取盐包(内含4.0 g无水硫酸镁、1.0 g氯化钠)盐析除水后取乙腈相,采用EMR-Lipid专利脂质去除分散固相萃取净化,净化液再经除脂萃取剂(EMR-Lipid Bond Elut Polish,EMR-Polish)盐析反萃后氮吹浓缩,采用Eclipse Plus C₁₈柱(50 mm×2.1 mm,1.8 μm)进行分离,以体积分数为0.10%甲酸水溶液和甲醇作为流动相进行梯度洗脱。采用电喷雾电离源、正离子模式下以多反应监测(MRM)进行定性和定量分析。结果表明,5种α₂-受体激动剂在0.20~20 μg/L范围内线性关系良好(r²＞0.999),方法检出限为0.20~0.70 μg/kg,方法定量限为0.60~2.0 μg/kg。在2.0、4.0和20 μg/kg共3个添加水平下的加标回收率为76.1%~103%,相对标准偏差(RSD)为1.3%~12%(n=6)。基质效应研究表明,5种α₂-受体激动剂均为弱基质效应。该方法简便高效,且准确性好、灵敏度高,适用于动物源性食品中5种α₂-受体激动剂残留测定。

关键词: 超高效液相色谱-串联质谱, 增强型脂质去除吸附剂, α₂-受体激动剂, 动物源性食品

Abstract: A method is established for the rapid determination of five alpha-agonists (apraclonidine, brimonidine, tizanidine, clonidine and xylazine) in animal derived food by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) after clean-up by the enhanced matrix removal of lipids (EMR-Lipid). After the pretreatment and UPLC-MS/MS conditions are optimized, the samples are dispersed with 2.0% ammonium hydroxide, then the analytes are extracted with acetonitrile and dried with the extraction salt packet which contains 4.0 g of anhydrous magnesium sulfate and 1.0 g of sodium chloride. Afterward, the acetonitrile layer is purified with EMR-Lipid, and salted out with EMR-Lipid Bond Elut Polish (EMR-Polish). After the solvent is evaporated under nitrogen and reconstituted, the separation is performed on an Eclipse Plus C₁₈ (50 mm×2.1 mm, 1.8 μm) column with 0.10% formic acid aqueous solution and methanol as the mobile phase by gradient elution. The electrospray source is in the positive ion mode and monitored in the multiple reactions monitoring mode. The five alpha-agonists show great linear relationships in the range of 0.20～20 μg/L with correlation coefficients (r²) greater than 0.999. The limits of detection (LOD) and limits of quantitation (LOQ) are in the ranges of 0.20～0.70 μg/kg and 0.60～2.0 μg/kg, respectively. The average recoveries of five targets vary from 76.1% to 103%, and the relative standard deviations are between 1.3% and 12% at the spiked levels of 2.0, 4.0 and 20 μg/kg. The results of matrix effect study show that the matrix has weak effects on all of the five alpha-agonists. The experimental results indicate that the proposed method is simple, quick, accurate and sensitive, and is suitable for the determination of five alpha-agonists in animal derived food.

Key words: Ultra-performance liquid chromatography-tandem mass spectrometry, Enhanced matrix removal of lipids, Alpha-agonists, Animal derived food

中图分类号:

O655

朱富强, 丁卫平, 韩岩君, 田洪根. 脂质去除分散固相萃取-超高效液相色谱-串联质谱法测定动物源性食品中5种α₂-受体激动剂[J]. 应用化学, 2021, 38(6): 713-721.

ZHU Fu-Qiang, DING Wei-Ping, HAN Yan-Jun, TIAN Hong-Gen. Determination of Five Alpha-agonists in Animal Derived Food by Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry Using an Enhanced Matrix Removal-lipid Sorbent for Clean-up[J]. Chinese Journal of Applied Chemistry, 2021, 38(6): 713-721.

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脂质去除分散固相萃取-超高效液相色谱-串联质谱法测定动物源性食品中5种α₂-受体激动剂

Determination of Five Alpha-agonists in Animal Derived Food by Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry Using an Enhanced Matrix Removal-lipid Sorbent for Clean-up

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