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酶探针超声和离子色谱-电感耦合等离子体质谱法定量饲料中的硒形态。

Quantitative selenium speciation in feed by enzymatic probe sonication and ion chromatography-inductively coupled plasma mass spectrometry.

机构信息

Institute of Quality Standard and Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences , Beijing, China.

Beijing Institute of Feed Control , Beijing, China.

出版信息

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2021 Feb;38(2):268-279. doi: 10.1080/19440049.2020.1849820. Epub 2021 Jan 6.

Abstract

A rapid, sensitive and species preservative analytical method for the simultaneous determination of six selenium (Se) species has been developed. Enzymatic probe sonication (EPS) was investigated as a novel and alternative technology for the extraction of Se species from feed matrices and the results were compared with the conventional hot water extraction, enzymatic hydrolysis and sequential extraction. The critical parameters of EPS such as enzyme types, extraction time, temperature, ultrasonic power and sample/enzyme ratio were varied with control. The Se species were separated and quantitatively determined by ion chromatography-inductively coupled plasma mass spectrometry (IC-ICP-MS). Under current optimised conditions, six inorganic and organic Se species were completely separated within 15 min in a single chromatographic run. The spectral interferences from the argon plasma Ar, ArCl or HBr were effectively removed by employing the kinetic energy discrimination (KED) mode. Quantitative extraction for total Se (>94.8%) and more than 89.0% for the sum of different Se chemical forms without species transformation were obtained in only 60 s by applying the EPS treatment using aqueous protease XIV. The limits of detection (LODs) and quantification (LOQs) for Se species were in the ranges of 0.21-0.56 µg kg and 0.69-1.87 µg kg, respectively. The proposed method was successfully applied to the speciation of Se in several reference materials and feed samples collected from the markets and local farms.

摘要

建立了一种同时测定六种硒(Se)形态的快速、灵敏、具有物种保留性的分析方法。研究了酶探针超声(EPS)作为一种新颖的替代技术,用于从饲料基质中提取硒形态,结果与常规热水提取、酶水解和顺序提取进行了比较。通过控制,改变了 EPS 的关键参数,如酶的类型、提取时间、温度、超声功率和样品/酶的比例。采用离子色谱-电感耦合等离子体质谱法(IC-ICP-MS)对硒形态进行分离和定量测定。在当前优化的条件下,六种无机和有机硒形态在单个色谱运行中可在 15 分钟内完全分离。通过采用动力学能量甄别(KED)模式,可以有效地消除氩等离子体 Ar、ArCl 或 HBr 的光谱干扰。仅在 60 秒内,通过使用水蛋白酶 XIV 进行 EPS 处理,即可获得总 Se(>94.8%)和不同 Se 化学形态总和(无形态转化)的定量提取,提取率>89.0%。硒形态的检测限(LOD)和定量限(LOQ)分别在 0.21-0.56 μg kg 和 0.69-1.87 μg kg 范围内。该方法成功应用于从市场和当地农场采集的几种参考材料和饲料样品中硒的形态分析。

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