CN106706545A - Method for analyzing functional group atlas of potato powder and flour mixture - Google Patents
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- 235000002595 Solanum tuberosum Nutrition 0.000 title claims abstract description 32
- 244000061456 Solanum tuberosum Species 0.000 title claims abstract description 32
- 235000013312 flour Nutrition 0.000 title claims abstract description 30
- 239000000843 powder Substances 0.000 title claims abstract description 17
- 125000000524 functional group Chemical group 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 title claims abstract description 13
- 239000000203 mixture Substances 0.000 title claims abstract description 11
- 238000001228 spectrum Methods 0.000 claims abstract description 56
- 238000002329 infrared spectrum Methods 0.000 claims abstract description 20
- 229920001592 potato starch Polymers 0.000 claims abstract description 18
- 230000001360 synchronised effect Effects 0.000 claims abstract description 14
- 238000004458 analytical method Methods 0.000 claims abstract description 7
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- 238000010219 correlation analysis Methods 0.000 claims abstract description 4
- 230000003595 spectral effect Effects 0.000 claims description 14
- 238000005102 attenuated total reflection Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
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- 235000013305 food Nutrition 0.000 abstract description 10
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- 235000016709 nutrition Nutrition 0.000 abstract description 5
- 230000035764 nutrition Effects 0.000 abstract description 3
- 230000003993 interaction Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 238000005457 optimization Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 9
- 230000008859 change Effects 0.000 description 7
- 229920002472 Starch Polymers 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 235000019698 starch Nutrition 0.000 description 5
- 239000008107 starch Substances 0.000 description 5
- 238000005100 correlation spectroscopy Methods 0.000 description 4
- 238000004497 NIR spectroscopy Methods 0.000 description 3
- 238000005360 mashing Methods 0.000 description 3
- 235000012015 potatoes Nutrition 0.000 description 3
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- 238000004566 IR spectroscopy Methods 0.000 description 2
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- 238000004445 quantitative analysis Methods 0.000 description 2
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- 101710172072 Kexin Proteins 0.000 description 1
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- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 235000005911 diet Nutrition 0.000 description 1
- 230000037213 diet Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000006694 eating habits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
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- 102000004169 proteins and genes Human genes 0.000 description 1
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- 238000001845 vibrational spectrum Methods 0.000 description 1
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- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
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Abstract
本发明公开了一种马铃薯全粉与面粉共混物的官能团图谱分析方法。包括：制备多个品种的马铃薯全粉和面粉的混合样品，并采集温度外扰下各马铃薯全粉和面粉的混合样品的红外光谱；计算混合样品红外光谱的受温度外扰诱发的动态光谱；对各样品的动态光谱进行二维相关分析，获得对应的同步二维相关光谱；对各样品的同步二维相关光谱进行官能团图谱分析。本发明研究马铃薯全粉与面粉共混物的分子结构变化以及它们之间的相互作用，揭示了不同品种马铃薯全粉与面粉在不同混合比例下它们之间相应各官能团的变化规律，为优化完善马铃薯主粮的制作加工过程，评价马铃薯主粮的营养和功效提供参考。
The invention discloses a functional group map analysis method of potato whole powder and flour blend. Including: preparing mixed samples of multiple varieties of potato flour and flour, and collecting the infrared spectrum of each mixed sample of potato flour and flour under external disturbance of temperature; calculating the dynamic spectrum of the infrared spectrum of the mixed sample induced by external disturbance of temperature; Carry out two-dimensional correlation analysis on the dynamic spectrum of each sample to obtain the corresponding synchronous two-dimensional correlation spectrum; perform functional group map analysis on the synchronous two-dimensional correlation spectrum of each sample. The present invention studies the molecular structure changes of potato flour and flour blends and the interaction between them, and reveals the variation rules of the corresponding functional groups between different varieties of potato flour and flour under different mixing ratios, and provides a basis for optimization and improvement. The production and processing process of potato staple food provides a reference for evaluating the nutrition and efficacy of potato staple food.
Description
技术领域technical field
本发明涉及利用红外光来测试或分析材料的检测方法，具体涉及一种马铃薯全粉与面粉共混物的官能团图谱分析方法。The invention relates to a detection method for testing or analyzing materials by using infrared light, in particular to a functional group spectrum analysis method for a blend of whole potato powder and flour.
背景技术Background technique
2015年初我国启动了马铃薯主粮化战略，以新鲜马铃薯为原料，经挑选、清洗、去皮、切片、漂洗、预煮、冷却、蒸煮、捣泥、脱水干燥等工艺过程制得马铃薯全粉。马铃薯全粉易贮藏，且保持了马铃薯特有的营养和风味，将其与面粉按一定比例混合后加工制成馒头、面条等适合中国人饮食习惯的主食，这将大大改善和丰富我国居民的膳食营养结构，满足人体对营养配比的需要。但目前马铃薯主粮化推进过程中存在马铃薯全粉专用品种缺乏，马铃薯主粮中马铃薯全粉混合比例较低，马铃薯主粮产品价格高昂等问题。At the beginning of 2015, my country launched the potato staple food strategy, using fresh potatoes as raw materials, through the process of selection, cleaning, peeling, slicing, rinsing, precooking, cooling, steaming, mashing, dehydration and drying to produce whole potato powder. Potato powder is easy to store, and maintains the unique nutrition and flavor of potatoes. It is mixed with flour in a certain proportion and processed into steamed buns, noodles and other staple foods suitable for Chinese eating habits, which will greatly improve and enrich the diet of Chinese residents. Nutritional structure to meet the needs of the human body for nutritional ratio. However, in the process of promoting potato as a staple food, there are problems such as the lack of special varieties of potato whole flour, the low mixing ratio of potato whole flour in potato staple food, and the high price of potato staple food.
近年来出现了一些针对马铃薯淀粉、马铃薯全粉及其制品进行检测的技术，如近红外光谱建模分析。基于近红外光谱的研究主要针对马铃薯全粉中还原糖、蛋白质等营养成分进行了定量分析，还有学者对干物质、淀粉等进行了定量分析。很多近红外模型预测结果精准，但建模所需样本量大，而且模型失效有待解决。In recent years, some technologies for the detection of potato starch, potato flour and their products have emerged, such as near-infrared spectroscopy modeling analysis. The research based on near-infrared spectroscopy mainly focuses on the quantitative analysis of reducing sugar, protein and other nutrients in potato flour, and some scholars have carried out quantitative analysis on dry matter and starch. The prediction results of many near-infrared models are accurate, but the sample size required for modeling is large, and the model failure needs to be solved.
二维相关光谱技术是将原本在一维空间的光谱拓展到二维空间，以达到增强光谱分辨率的效果，二维相关光谱技术常结合红外光谱检测技术一起使用，红外光谱图分为特征频率区和指纹区，特征频率区的吸收峰数目不多，但具有很强的特征性，在基团鉴定工作上很有价值。指纹区峰多而复杂，没有强的特征性，但当分子结构稍有不同时，该区吸收峰就会产生细微差异，指纹区对于区别结构类似的化合物很有帮助。所以二维相关光谱技术结合红外光谱技术后，就可通过测定分子内各基团相应微扰所导致红外振动光谱的影响，运用数学相关分析技术对获得的动态光谱进行处理得到二维相关红外谱图，利用更高分辨率的二维谱图上自动峰及相关峰峰簇的位置、数量和强度等的不同，不仅能鉴别出各谱峰的具体归属，还提供了各物质分子之间微观变化的信息，进而获得分子结构变化的信息。对于复杂体系的鉴别研究，具有一定的实际意义。目前该方法已经被广泛的应用于物理、化学、材料、生物、医学等各个领域，但是在马铃薯主粮化领域还未见应用。Two-dimensional correlation spectroscopy technology is to expand the spectrum originally in one-dimensional space to two-dimensional space to achieve the effect of enhancing spectral resolution. Two-dimensional correlation spectroscopy technology is often used in combination with infrared spectrum detection technology. The infrared spectrum is divided into characteristic frequency The number of absorption peaks in the characteristic frequency region and the fingerprint region is small, but it has strong characteristics and is very valuable in group identification. There are many and complex peaks in the fingerprint area, and there is no strong characteristic. However, when the molecular structure is slightly different, the absorption peaks in this area will have subtle differences. The fingerprint area is very helpful for distinguishing compounds with similar structures. Therefore, after the two-dimensional correlation spectroscopy technology is combined with the infrared spectroscopy technology, the influence of the infrared vibration spectrum caused by the corresponding perturbation of each group in the molecule can be measured, and the obtained dynamic spectrum can be processed by mathematical correlation analysis technology to obtain the two-dimensional correlation infrared spectrum. Figure, using the position, number and intensity of automatic peaks and related peak clusters on the higher-resolution two-dimensional spectrum, not only can identify the specific attribution of each spectrum peak, but also provide microscopic information on the relationship between the molecules of each substance. Change information, and then obtain information on molecular structure changes. It has certain practical significance for the identification research of complex systems. At present, this method has been widely used in various fields such as physics, chemistry, materials, biology, and medicine, but it has not been applied in the field of potato staple food.
发明内容Contents of the invention
针对背景技术中存在的问题和不足，本发明的目的在于提供一种马铃薯全粉与面粉共混物的官能团图谱分析方法，在衰减全反射采集模式下采集样品在温度外扰下的一系列红外光谱，进一步获得同步二维相关光谱，然后对不同样品二维相关同步谱间差异进行分析，揭示不同品种马铃薯全粉与面粉在不同混合比例下它们之间相应各官能团的变化规律，既解决了传统湿法化学方法检测成本高，环境不友好等缺点，也有效弥补了近红外光谱建模分析法模型失效的不足。In view of the problems and deficiencies in the background technology, the purpose of the present invention is to provide a method for functional group spectrum analysis of potato flour and flour blends, which collects a series of infrared images of samples under external disturbance of temperature in the attenuated total reflection collection mode. Spectrum, to further obtain the synchronous two-dimensional correlation spectrum, and then analyze the difference between the two-dimensional correlation synchronous spectra of different samples, revealing the change law of the corresponding functional groups between different varieties of potato whole flour and flour at different mixing ratios, which solves the problem of The shortcomings of traditional wet chemical methods, such as high detection cost and unfriendly environment, also effectively make up for the shortcomings of the model failure of near-infrared spectroscopy modeling and analysis.
本发明采用的技术方案的步骤如下：The steps of the technical solution adopted in the present invention are as follows:
1)制备多个品种的马铃薯全粉和面粉的混合样品，多个品种的马铃薯全粉和面粉的混合样品比例分别为30％、35％、40％、45％或50％；然后采集温度外扰下多个品种的马铃薯全粉和面粉的混合样品的红外光谱；1) Prepare the mixed samples of whole potato powder and flour of multiple varieties, the proportion of mixed samples of whole potato flour and flour of multiple varieties is respectively 30%, 35%, 40%, 45% or 50%; Infrared spectra of mixed samples of whole potato powder and flour of various varieties;
2)计算步骤1)中混合样品的红外光谱的受温度外扰t诱发的动态光谱，动态光谱表示为：2) Calculate the dynamic spectrum of the infrared spectrum of the mixed sample in step 1) induced by the temperature disturbance t, the dynamic spectrum Expressed as:
式中，y(v，t)是在整个微扰过程(从t＝-T/2到t＝T/2)中微扰为t时变量v处的光谱强度；是参考光谱，参考光谱的选择由静态光谱或时间平均光谱设定，定义为：In the formula, y(v, t) is the spectral intensity at the variable v when the perturbation is t in the whole perturbation process (from t=-T/2 to t=T/2); is the reference spectrum, the choice of reference spectrum is set by static spectrum or time-averaged spectrum, defined as:
3)对各样品的动态光谱进行二维相关分析，获得对应的同步二维相关光谱；3) Perform two-dimensional correlation analysis on the dynamic spectra of each sample to obtain corresponding synchronous two-dimensional correlation spectra;
在微扰t作用下，等间距的测得m个数据点(如在相等温度间隔时测量样品的红外光谱)则从t＝-T/2到t＝T/2的动态光谱可表示为：Under the action of perturbation t, m data points measured at equal intervals (such as measuring the infrared spectrum of the sample at equal temperature intervals) then the dynamic spectrum from t=-T/2 to t=T/2 can be expressed as:
同步二维相关光谱代表两个变量v1和v2处光谱强度随微扰t而产生的变化的相似性，同步二维相关光谱的同步光谱强度φ(v1，v2)的计算公式为：The synchronous two-dimensional correlation spectrum represents the similarity of the variation of the spectral intensity at the two variables v 1 and v 2 with perturbation t, and the calculation formula of the synchronous spectral intensity φ(v 1 , v 2 ) of the synchronous two-dimensional correlation spectrum is :
4)对各混合样品的同步二维相关光谱进行官能团变化的图谱分析。4) Perform spectral analysis of functional group changes on the simultaneous two-dimensional correlation spectra of each mixed sample.
所述步骤1)中，马铃薯全粉制备方法为：新鲜马铃薯-清洗去皮-切片厚度8mm-在70℃下预煮20min-冷却-在100℃下蒸煮15min-捣碎制泥-真空干燥-粉碎100目过筛-取筛下物。In the step 1), the preparation method of whole potato powder is as follows: fresh potatoes-cleaning and peeling-slice thickness 8mm-precooking at 70°C for 20min-cooling-cooking at 100°C for 15min-mashing and mashing-vacuum drying- Crush the 100 mesh sieve - get the undersize.
所述步骤1)中，光谱采集模式为衰减全反射，所有样品采集红外光谱时的采集条件一致：光谱范围为4000～400cm-1，光谱分辨率8cm-1，采集时间3s，每一条光谱为16次扫描的平均光谱。In the step 1), the spectrum collection mode is attenuated total reflection, and the collection conditions of all samples are the same when collecting infrared spectra: the spectral range is 4000-400cm -1 , the spectral resolution is 8cm -1 , the collection time is 3s, and each spectrum is Average spectrum of 16 scans.
本发明具有的有益效果是：The beneficial effects that the present invention has are:
1)本发明采用的二维相关光谱法结合红外光谱检测技术，通过比较马铃薯全粉与面粉不同混合比例样品的二维相关红外光谱间的差异情况，对样品在外扰下各物质分子之间微观变化信息进行分析。该方法不仅简便，快速，无需对待测样品进行分离，纯化等预处理，而且环境友好，无化学试剂污染，对操作人员要求不高，同时还弥补了近红外光谱建模方法中遇到的模型失效的问题。1) The two-dimensional correlation spectroscopy method that the present invention adopts combines the infrared spectrum detection technology, by comparing the difference between the two-dimensional correlation infrared spectra of samples of different mixing ratios of potato flour and flour, the microcosm of each substance molecule under the external disturbance of the sample Change information is analyzed. This method is not only simple and fast, and does not require pretreatment such as separation and purification of the sample to be tested, but also is environmentally friendly, free from chemical reagent pollution, and has low requirements for operators. failure problem.
2)本发明利用二维相关红外光谱研究马铃薯全粉与面粉共混物的分子结构变化以及它们之间的相互作用，揭示了不同品种马铃薯全粉与面粉在不同混合比例下它们之间相应各官能团的变化规律，为更好的优化完善马铃薯主粮的制作加工过程，更有效的评价马铃薯主粮的营养和功效提供了参考。2) The present invention uses two-dimensional correlation infrared spectroscopy to study the molecular structure changes of potato flour and flour blends and the interaction between them, revealing the corresponding differences between different varieties of potato flour and flour under different mixing ratios. The change law of functional groups provides a reference for better optimizing and improving the production and processing process of potato staple food, and more effectively evaluating the nutrition and efficacy of potato staple food.
附图说明Description of drawings
图1是马铃薯全粉制备方法。Fig. 1 is the preparation method of whole potato flour.
图2是二维相关光谱的获得示意图。Fig. 2 is a schematic diagram of obtaining a two-dimensional correlation spectrum.
图3是大西洋含量从30％增至50％的马铃薯全粉及面粉共混物的二维相关图谱。Figure 3 is a two-dimensional correlation map of whole potato flour and flour blends with increasing Atlantic content from 30% to 50%.
具体实施方式detailed description
下面结合附图和实施例对本发明作进一步的说明。The present invention will be further described below in conjunction with the accompanying drawings and embodiments.
本实施例中，所制备的样本包括：In this embodiment, the prepared samples include:
马铃薯：共4个品种，分别为大西洋、夏波蒂、冀张薯8号和克新，均采收自河北坝上张北县。Potatoes: There are 4 varieties in total, namely Atlantic, Xiabodi, Jizhangshu No. 8 and Kexin, all harvested from Zhangbei County, Bashang, Hebei.
如图1所示，马铃薯全粉制备方法为：新鲜马铃薯-清洗去皮-切片厚度8mm-在70℃下预煮20min-冷却-在100℃下蒸煮15min-捣碎制泥-真空干燥-粉碎100目过筛-取筛下物。As shown in Figure 1, the preparation method of whole potato powder is as follows: fresh potatoes-cleaning and peeling-slicing thickness 8mm-precooking at 70°C for 20min-cooling-cooking at 100°C for 15min-mashing to make puree-vacuum drying-crushing 100 mesh sieve - take the undersize.
马铃薯全粉和面粉的共混物：混合马铃薯全粉比例分别为30％、35％、40％、45％、50％Blends of whole potato flour and flour: 30%, 35%, 40%, 45%, 50% of mixed whole potato flour
如图2所示，是二维相关光谱的获得示意图。As shown in FIG. 2 , it is a schematic diagram of obtaining a two-dimensional correlation spectrum.
步骤1：采集一系列红外光谱Step 1: Acquire a series of infrared spectra
将马铃薯全粉和面粉的五种混合比例样品分别置于控温附件上，然后利用控温附件控制温度，从35～95℃每隔10℃采集一次红外光谱。所有样品采集红外光谱时的采集条件一致：采集模式为衰减全反射，空白对照光谱为不放置样本采集的空气的红外光谱，光谱范围为4000～400cm-1，光谱分辨率8cm-1，采集时间3s，每一条光谱为16次扫描的平均光谱。The five kinds of mixing ratio samples of whole potato powder and flour were placed on the temperature control attachment, and then the temperature was controlled by the temperature control attachment, and the infrared spectrum was collected every 10 °C from 35 to 95 °C. The collection conditions of all samples are the same when collecting infrared spectra: the collection mode is attenuated total reflection, the blank control spectrum is the infrared spectrum of the air collected without placing the sample, the spectral range is 4000～400cm -1 , the spectral resolution is 8cm -1 , the collection time 3s, each spectrum is the average spectrum of 16 scans.
步骤2：计算得到的红外光谱的动态光谱Step 2: Calculate the Dynamic Spectrum of the Resulting IR Spectrum
动态光谱可由下式计算得到：The dynamic spectrum can be calculated by the following formula:
式中，y(v，t)为在外扰作用下-T/2到T/2区域内的光谱强度；是参考光谱，参考光谱的选择通常由静态光谱或时间平均光谱设定，定义为：In the formula, y(v, t) is the spectral intensity in the region from -T/2 to T/2 under the external disturbance; is the reference spectrum, and the choice of the reference spectrum is usually set by a static spectrum or a time-averaged spectrum, defined as:
假如在外扰变量t作用下，获得的m组数据其动态光谱也可以由式3表达。If under the action of the external disturbance variable t, the dynamic spectrum of the obtained m sets of data can also be expressed by Equation 3.
步骤3：计算同步二维相关光谱：Step 3: Calculate the simultaneous 2D correlation spectrum:
同步二维相关光谱计算公式如式(4)所示；Synchronous two-dimensional correlation spectrum calculation formula is shown in formula (4);
步骤4：根据得到的同步二维相关光谱图(如图3所示)对马铃薯全粉和面粉的混合样品进行官能团变化分析。从图中可以看到在对角线相近的位置上均出现了自动峰，但是自动峰存在不同的组合方式且相对强度也各不同，也就是说马铃薯全粉和面粉不同混合比例体系中自动峰所对应的官能团所处的分子内部环境不同，相对应的分子结构对外部温度微扰的敏感程度也不同。此外，这些自动峰均在1047cm-1、1022cm-1以及994cm-1处出现最强峰，1047cm-1是淀粉结晶区的结构特征，对应于淀粉聚集态结构中的有序结构，1022cm-1则是淀粉无定型区的结构特征，对应于淀粉大分子的无规线团结构。在对角线两侧各个特征峰相互之间也都出现了交叉峰，而且均为正峰，表明在外部微扰的影响下，各个特征峰动态变化的方向是一致的。Step 4: According to the obtained synchronous two-dimensional correlation spectrum (as shown in FIG. 3 ), analyze the change of functional groups in the mixed sample of whole potato powder and flour. It can be seen from the figure that automatic peaks appear at positions close to the diagonals, but there are different combinations of automatic peaks and their relative intensities are also different, that is to say, automatic peaks in systems with different mixing ratios of whole potato flour and flour The corresponding functional groups have different internal molecular environments, and the corresponding molecular structures have different sensitivity to external temperature perturbations. In addition, these automatic peaks all appear at 1047cm -1 , 1022cm -1 and 994cm -1 as the strongest peaks, 1047cm -1 is the structural feature of the starch crystallization region, corresponding to the ordered structure in the starch aggregate structure, and 1022cm -1 It is the structural feature of the amorphous region of starch, corresponding to the random coil structure of starch macromolecules. The characteristic peaks on both sides of the diagonal also have cross peaks, and they are all positive peaks, indicating that under the influence of external perturbation, the direction of dynamic change of each characteristic peak is consistent.
上述具体实施方式用来解释说明本发明，而不是对本发明进行限制，在本发明的精神和权利要求的保护范围内，对本发明作出的任何修改和改变，都落入本发明的保护范围。The above specific embodiments are used to explain the present invention, rather than to limit the present invention. Within the spirit of the present invention and the protection scope of the claims, any modification and change made to the present invention will fall into the protection scope of the present invention.
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