论文
红外光谱对牛预混料中违禁添加盐酸土霉素的快速定量
徐惟馨，夏静静，韦 芸，陈玥瑶，毛欣然，闵顺耕* ，熊艳梅*
中国农业大学理学院，北京 100193
Rapid Determination of Oxytetracycline Hydrochloride Illegally Added in Cattle Premix by ATR-FTIR
XU Wei-xin, XIA Jing-jing, WEI Yun, CHEN Yue-yao, MAO Xin-ran, MIN Shun-geng* , XIONG Yan-mei*
College of Science，China Agricultural University，Beijing 100193，China
摘要 ： 利用衰减全反射傅里叶变换红外光谱（ATR-FTIR）结合偏最小二乘法（PLS）对牛预混料中违禁添加的盐酸土霉素含量进行了快速定量检测。在空白牛预混料中中添加不同质量的98.00% (W /W )盐酸土霉素原药，配制成盐酸土霉素浓度为0.00%～5.00%的113个混合样品，纯水作为萃取剂，萃取液经红外灯烤干后用于红外光谱测定。为考察不同光谱预处理方法及变量选择方法对模型结果的影响，选用了3种预处理方法：Savitzky-Golay卷积平滑法(S-G)、标准正态变换法(SNV) 和多元散射校正法(MSC)和3种变量选择算法：区间偏最小二乘法(iPLS)、移动窗口偏最小二乘法(MWPLS)、自主软收缩法(BOSS)。其中，SNV预处理结合BOSS算法获得了最佳模型效果：RMSECV=0.337，R 2 CV =0.947，RMSEP=0.317 7，R 2 pre =0.935。所得模型对含量在0.53%~4.67%的29个样品进行外部验证，预测结果的平均相对误差为0.127，预测效果较好。同时，BOSS算法选取的变量主要集中在盐酸土霉素特征峰的吸收区域（1 674~1 593和1 175～1 017 cm-1 ），可以为ATR-FTIR技术对饲料中土霉素盐酸盐的快速检测提供有价值的参考。
关键词 ：衰减全反射；偏最小二乘法；定量分析；变量选择；盐酸土霉素
Abstract ：A rapid quantification of oxytetracycline hydrochloride in cattle premix using Attenuated total reflection-Fourier-transform infrared spectroscopy (ATR-FTIR) combined with partial least squares (PLS) was performed. Rapid quantification of the prohibited component of oxytetracycline hydrochloride in cattle premix was carried out. 98.00% (W /W ) oxytetracycline hydrochloride was added to the blank cattle premix, and 113 mixed samples were prepared with oxytetracycline hydrochloride concentrations ranging from 0.00% to 5.00%. Pure water was used as the extractant, and the extract was dried by an infrared lamp and used for IR spectroscopy. Three pretreatment methods were employed: Savitzky-Golay convolution smoothing (S-G), standard normal variation (SNV), multivariate scattering correction (MSC), and three variable selection algorithms: Interval partial least-squares (iPLS), Moving partial window least-squares (MWPLS), the bootstrapping soft shrinkage (BOSS). Among them, SNV combined with the BOSS algorithm obtained the best model results: RMSECV=0.337 0, R 2 CV =0.946 9, RMSEP=0.317 3, R 2 pre =0.934 6. The model predicted 29 samples with contents ranging from 0.53% to 4.67%, and the average relative error of prediction was 0.126 7. Meanwhile, the variables selected by the BOSS algorithm were mainly concentrated in the absorption regions of the characteristic peaks of oxytetracycline hydrochloride (1 674~1 593 and 1 175~1 017 cm-1 ), which can provide a valuable reference for the ATR-FTIR technique in the rapid detection of oxytetracycline hydrochloride in feed.
Key words ：Infrared spectrum; Quantitative analysis; Partial least squares; Variable selection; Oxytetracycline Hydrochloride
收稿日期: 2022-01-07
修订日期: 2022-04-14
基金资助: 国家自然科学基金项目（21023048）资助
通讯作者:
闵顺耕，熊艳梅
E-mail: minsg@cau.edu.cn；xiongym@cau.edu.cn
作者简介: 徐惟馨，女，1998年生，中国农业大学理学院硕士研究生 e-mail: xuweixin1998@cau.edu.cn
引用本文:
徐惟馨，夏静静，韦 芸，陈玥瑶，毛欣然，闵顺耕，熊艳梅. 红外光谱对牛预混料中违禁添加盐酸土霉素的快速定量[J]. 光谱学与光谱分析, 2023, 43(03): 842-847.
链接本文:
https://www.gpxygpfx.com/CN/10.3964/j.issn.1000-0593(2023)03-0842-06
或
https://www.gpxygpfx.com/CN/Y2023/V43/I03/842
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