基于MEMS微镜技术的近红外光谱检测奶粉中的三聚氰胺
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摘要
为实现奶粉中三聚氰胺的无损定量快速检测,搭建了一款便携式光学仪器。采用基于MEMS微镜的微型光学平台及手持式探头、光纤及样品池等搭建的傅里叶变换近红外光谱仪,在1 000～2 500 nm波长范围内采集样品光谱,结合光谱预处理、特征波段筛选及主成分数选取来优化光谱信息,依照偏最小二乘法结合交叉验证建立定量模型。在1 400～1 600 nm和1 900～2 400 nm波段内,二阶导数+Savitzky-Golay九点平滑的预处理方法下,当主成分数为5时,交叉验证相关系数为0.965 2,交叉验证均方差为8.22,外部验证结果预测偏差均小于5%,模型预测性能良好。基于MEMS微镜的便携式近红外光谱仪能实现奶粉掺假三聚氰胺定量检测。
In order to identify and quantitatively detect the melamine in milk powder, build a portable optical instrument. A spectral platform of Fourier transform near-infrared spectroscopy based on MEMS micro-mirror, handheld probe, optical fiber and sample cell was constructed to a Fourier transform near infrared spectrometer. The near infrared diffuse reflectance spectra of mixed samples using milk powder and melamine with different proportions are collected from 1 000 to 2 500 nm. The reliability of the established PLS model was verified by cross-validation and external test. In 1 400-1 600 nm and 1 900-2 400 nm band, using the second derivative+Savitzky-Golay 9 spots smoothing pretreatment method and the main component of 5, the calibrate correlation coefficient of the quantitative analysis model was 0.965 2, and the root mean square error of calibration was 8.22. The predicted deviation of external validation results was under 5%. The results showed that the portable near infrared spectroscopy based on MEMS micro-mirror could be used for rapid and quantitative identification of adulterated milk powder.
In order to identify and quantitatively detect the melamine in milk powder, build a portable optical instrument. A spectral platform of Fourier transform near-infrared spectroscopy based on MEMS micro-mirror, handheld probe, optical fiber and sample cell was constructed to a Fourier transform near infrared spectrometer. The near infrared diffuse reflectance spectra of mixed samples using milk powder and melamine with different proportions are collected from 1 000 to 2 500 nm. The reliability of the established PLS model was verified by cross-validation and external test. In 1 400-1 600 nm and 1 900-2 400 nm band, using the second derivative+Savitzky-Golay 9 spots smoothing pretreatment method and the main component of 5, the calibrate correlation coefficient of the quantitative analysis model was 0.965 2, and the root mean square error of calibration was 8.22. The predicted deviation of external validation results was under 5%. The results showed that the portable near infrared spectroscopy based on MEMS micro-mirror could be used for rapid and quantitative identification of adulterated milk powder.
引文
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[15]曹春廷,孙建霞,白卫滨,等.蛋白粉和奶粉的鉴伪技术研究进展[J].食品工业科技,2013,34(23):368-372.
[16]杜晨朝,吴志生,赵娜,等.基于两类误差检测理论金银花提取过程的MEMS-NIR在线分析建模方法研究[J].中国中药杂志,2016,41(19):3563-3568.
[2]于景华.我国奶粉的质量安全问题与控制现状[J].食品科学技术学报,2015,33(6):7-10.
[3]GARCIAA J,SANVIDOB G,SARAIVAB S,et al.Bovine milk powder adulteration with vegetable oils or fats revealed by MALDI-QTOF MS[J].Food Chem,2012,131(2):722-726.
[4]邓立友,邓浩昌.从乳品分类看我国乳制品发展方向[J].中国供销商情(乳业导刊),2006(4):37-38.
[5]杨杰,高洁,苗虹.论食品欺诈和食品掺假[J].食品与发酵工业,2015,12:235-240.
[6]钟质.乳粉的质量鉴别[J].广西质量监督导报,2005(4):36.
[7]尚攀峰,岳中瑾,常宏,等.食用含三聚氰胺奶粉婴幼儿泌尿系统结石的危险因素分析[J].中国循证医学杂志,2013,13(1):13-17.
[8]郭铁筝,潘国卿,赵治国,等.牛奶和奶粉中三聚氰胺的快速测定方法[J].内蒙古师范大学学报(自然科学汉文版),2012,41(4):406-409.
[9]王余波,李延昭,郝卫强,等.应用HILIC技术检测乳制品中的尿素[J].中国乳品工业,2011,39(7):50-52.
[10]陈钰,王捷,刘仲明,等.喷射式电化学发光流动检测技术快速测定奶粉及液态奶中三聚氰胺[J].分析测试学报,2014,32(7):890-893.
[11]ROMAN M,BALABIN B,SERGEY V SMIRNOV.Melamine detection by mid-and near-infrared(MIR/NIR)spectroscopy:A quick and sensitive method for dairy products analysis including liquid milk,infant formula,and milk powder[J].TALANTA,2011,85(1):562-568.
[12]翁诗浦.傅立叶变换红外分析[M].2版.北京:化学工业出版社,2010.
[13]陆婉珍.现代近红外光谱分析技术[M].北京:中国石化出版社,2007.
[14]后其军,鞠兴荣,何荣.近红外光谱分析技术在粮油品质评价中的研究应用进展[J].中国粮油学报,2015,30(7):135-140.
[15]曹春廷,孙建霞,白卫滨,等.蛋白粉和奶粉的鉴伪技术研究进展[J].食品工业科技,2013,34(23):368-372.
[16]杜晨朝,吴志生,赵娜,等.基于两类误差检测理论金银花提取过程的MEMS-NIR在线分析建模方法研究[J].中国中药杂志,2016,41(19):3563-3568.