苏云金杆菌制剂中违禁添加高效氯氟氰菊酯的红外光谱快速定量方法研究  

Rapid Quantification of Illegal Addition of Lambda-Cyhalothrin in Bacillus Thuringiensis Preparations by Infrared Spectroscopy

作　　者：陈月飞 夏静静 韦芸 徐惟馨 毛欣然 闵顺耕[1] 熊艳梅[1] CHEN Yue-fei;XIA Jing-jing;WEI Yun;XU Wei-xin;MAO Xin-ran;MIN Shun-geng;XIONG Yan-mei(College of Science,China Agricultural University,Beijing 100193,China)

机构地区：[1]中国农业大学理学院,北京100193

出　　处：《光谱学与光谱分析》2025年第5期1348-1354,共7页Spectroscopy and Spectral Analysis

基　　金：国家自然科学基金项目(31301685)资助。

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)对苏云金杆菌制剂中违禁添加的高效氯氟氰菊酯含量进行了快速定量检测。在3种不同来源的苏云金杆菌制剂中加入不同质量的95%(w/w)高效氯氟氰菊酯原药,配制成浓度为0.00%~5.00%的混合样品153个,乙腈作为萃取剂,选用较少萃取剂用量提高隐性成分在萃取液中浓度以增强红外吸收。选择3种预处理方法:平滑法(smooth)、标准正态变换法(SNV)和多元散射校正法(MSC)以及6种变量选择算法:无信息变量消除法(UVE)、区间偏最小二乘法(iPLS)、移动窗口偏最小二乘法(MWPLS)、竞争性自适应重加权采样(CARS)、自助软收缩法(BOSS)、区间组合优化(ICO),考察了不同预处理方法及变量选择方法对模型结果的影响。其中,MSC预处理结合BOSS算法获得最优的模型效果:交叉验证均方根误差(RMSECV)为1.18×10^(-3),交叉验证集决定系数(R2cv)为9.94×10^(-1),预测均方根误差(RMSEP)为1.01×10^(-3),预测集决定系数(R2pre)为9.93×10^(-1)。对于高效氯氟氰菊酯含量范围在0.10%~5.00%的样品,外部检验样品预测平均相对误差为4.44%,含量范围在2.00%~5.00%的样品,外部检验样品平均相对误差仅2.64%。该方法可应用于苏云金杆菌制剂中违禁添加高效氯氟氰菊酯的快速检测。Rapid quantitative determination of the illegal addition of lambda-cyhalothrin in Bacillus thuringiensis preparations was carried out using attenuated total reflection Fourier transform infrared spectroscopy(ATR-FTIR)coupled with partial least squares(PLS)method.Three different sources of Bacillus thuringiensis preparations with different masses of 95%(w/w)lambda-cyhalothrin prodrug were added to prepare 153 mixed samples,concentrations ranging from 0.00%to 5.00%,acetonitrile was used as the extractant,and less extractant was used to increase the concentration of lambda-cyhalothrin in the extract to enhance the infrared absorption.Three pretreatment methods(smoothing,standard normal variation(SNV)and multiple scattering correction(MSC))and six variable selection algorithms(uninformative variable elimination(UVE),interval partial least squares(iPLS),moving window partial least squares(MWPLS),competitive adaptive reweighted sampling(CARS),the bootstrapping soft shrinkage(BOSS)and interval combination optimization(ICO)),were used to examine the effects of different pretreatment methods and variable selection methods on the model results.Among them,the MSC pretreatment method combined with the BOSS algorithm obtained the optimal model results,with this method,RMSECV=1.18×10^(-3),R2cv=9.94×10^(-1),RMSEP=1.01×10^(-3),and R2pre=9.93×10^(-1).For samples with lambda-cyhalothrin concentrations ranging from 0.10%to 5.00%,the average relative error of external test samples was 4.44%,and for samples with concentrations ranging from 2.00%to 5.00%,the average relative error of external test samples was only 2.64%.This method could be applied to rapidly detect the illegal addition of lambda-cyhalothrin in Bacillus thuringiensis preparations.

关 键 词：红外光谱 偏最小二乘法 变量选择 高效氯氟氰菊酯 苏云金杆菌 

分 类 号：O657.33[理学—分析化学]