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基于最佳粒径胶体金的 SERS 法测定猪肉中克伦特罗残留量

A determination method for clenbuterol residue in pork based on optimal particle size gold colloid using SERS.

机构信息

College of Engineering, National R&D Center for Agro-processing Equipment, China Agricultural University, Beijing 100083, China.

College of Engineering, National R&D Center for Agro-processing Equipment, China Agricultural University, Beijing 100083, China.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2023 Dec 5;302:123097. doi: 10.1016/j.saa.2023.123097. Epub 2023 Jul 1.

DOI:10.1016/j.saa.2023.123097
PMID:37418907
Abstract

Clenbuterol is often used as a feed additive to increase the percentage of lean meat in livestock. Meat containing clenbuterol can cause many illnesses and even death for people. In this paper, the particle growth method was used to prepare gold colloids of different sizes, and the enhanced effectiveness of gold colloids of different sizes on clenbuterol in pork was investigated. The results showed that the gold colloid with the best enhanced effectiveness for clenbuterol had a particle size of approximately 90 nm. Second, a sample collection component was designed to detect clenbuterol from bottom to top, solving the problem of poor reproducibility of Surface-enhanced Raman scattering (SERS) detection caused by different droplet sizes and shapes. Then, the influence of different volumes of samples and concentrations of aggregating compounds on the enhanced effectiveness was optimized. The results showed that, based on the sample collection components designed in this article, 5 µL of enhanced substrate, 7.5 µL of clenbuterol and 3 µL of 1 mol/L mixed detection of NaCl solution had the best enhanced performance. Finally, 88 pork samples (0.5, 1, 1.5,…, 10, 12, 14 µg/g) with different concentrations were divided into correction sets and prediction sets in a ratio of 3:1. Unary linear regression models were established between the concentration of clenbuterol residue in the pork and the intensity of the bands at 390, 648, 1259, 1472, and 1601 cm. The results showed that the unary linear regression models at 390, 648, and 1259 cm had lower root mean square errors than those at 1472 and 1601 cm. The intensity of the three bands and the concentration of clenbuterol residue in the pork were selected to establish a multiple linear regression model, and the concentration of clenbuterol residue in the pork was predicted. The results showed that the determination coefficients (R) of the correction set and the prediction set were 0.99 and 0.99, respectively. The root mean square errors (RMSE) of the correction set and the prediction set were 0.169 and 0.184, respectively. The detection limit of clenbuterol in pork by this method is 42 ng/g, which can realize the crude screening of pork containing clenbuterol in the market.

摘要

克伦特罗常被用作饲料添加剂,以增加牲畜的瘦肉百分比。含有克伦特罗的肉类会导致许多人生病,甚至死亡。本文采用粒子生长法制备了不同粒径的金胶体,并研究了不同粒径的金胶体对猪肉中克伦特罗的增强效果。结果表明,增强效果最好的金胶体粒径约为 90nm。其次,设计了一种从底部到顶部采集样品的组件,解决了由于液滴大小和形状不同而导致表面增强拉曼散射(SERS)检测重现性差的问题。然后,优化了不同样品体积和聚集化合物浓度对增强效果的影响。结果表明,基于本文设计的样品采集组件,使用 5µL 的增强基底、7.5µL 的克伦特罗和 3µL 的 1mol/L 混合检测 NaCl 溶液,具有最佳的增强性能。最后,将 88 个不同浓度的猪肉样品(0.5、1、1.5、…、10、12、14µg/g)分为校正集和预测集,比例为 3:1。建立了猪肉中克伦特罗残留浓度与 390、648、1259、1472 和 1601cm 处峰强度之间的一元线性回归模型。结果表明,在 390、648 和 1259cm 处的一元线性回归模型的均方根误差低于在 1472 和 1601cm 处的模型。选择三条谱带的强度和猪肉中克伦特罗残留浓度建立多元线性回归模型,对猪肉中克伦特罗残留浓度进行预测。结果表明,校正集和预测集的决定系数(R)分别为 0.99 和 0.99,校正集和预测集的均方根误差(RMSE)分别为 0.169 和 0.184。该方法检测猪肉中克伦特罗的检测限为 42ng/g,可以实现对市场上含有克伦特罗的猪肉的粗筛。

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