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CN101349638A - Spectral rapid non-destructive detection method for vitamin C content in fruits and vegetables - Google Patents

Spectral rapid non-destructive detection method for vitamin C content in fruits and vegetables Download PDF

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CN101349638A
CN101349638A CNA2007101303143A CN200710130314A CN101349638A CN 101349638 A CN101349638 A CN 101349638A CN A2007101303143 A CNA2007101303143 A CN A2007101303143A CN 200710130314 A CN200710130314 A CN 200710130314A CN 101349638 A CN101349638 A CN 101349638A
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vitamin
content
vegetables
fruits
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刘燕德
孙旭东
陈兴苗
周培聪
饶洪辉
文建萍
蒋育华
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Jiangxi Agricultural University
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Abstract

本发明为果蔬维生素C含量的光谱快速无损检测方法，涉及一种应用可见光和近红外漫反射光谱分析技术快速无损检测水果、蔬菜维生素C含量的方法，目前所采用的检测方法为破坏性检测，检测速度慢、效率低、成本高，本发明提供的技术方案具体步骤包括：样品采集、建模样品集选择、建模样品光谱采集、建模样品参考化学值测定、校正数学模型建立、校正数学模型验证和未知样品预测，本发明主要用于快速、高效地实现各类水果、蔬菜内部维生素C含量的无损检测，具有检测速度快，检测精度高，人为误差小，不需化学试剂，不污染环境，检测成本低的有益效果。

The invention discloses a spectral rapid nondestructive detection method for vitamin C content of fruits and vegetables, and relates to a method for rapid nondestructive detection of vitamin C content of fruits and vegetables by applying visible light and near-infrared diffuse reflectance spectral analysis technology. The detection method currently used is destructive detection, which has slow detection speed, low efficiency and high cost. The technical scheme provided by the invention specifically comprises the following steps: sample collection, modeling sample set selection, modeling sample spectrum collection, modeling sample reference chemical value determination, correction mathematical model establishment, correction mathematical model verification and unknown sample prediction. The invention is mainly used for rapidly and efficiently realizing nondestructive detection of vitamin C content in various fruits and vegetables, and has the beneficial effects of fast detection speed, high detection accuracy, small human error, no need for chemical reagents, no environmental pollution and low detection cost.

Description

The optical spectrum rapid nondestructive detection method of fruit and vegetable vitamin C content
Technical field
The present invention relates to the lossless detection method field, relate in particular to the method that a kind of application of spectral analytical technology quick nondestructive detects.
Background technology
In recent years, along with the continuous increase of fruit, yield of vegetables and improving constantly of people's living standard, consumer's requirement to the inside quality index of fruits and vegetables when choosing fruits and vegetables is more and more higher, and vitamin C is as a kind of important nutritional labeling, the main reference index the when consumer selects fruits and vegetables beyond doubt.And at present to the mensuration of fruit and vegetable vitamin C often based on destructive chemical analysis or use the expensive experimental instrumental analysis, the method for common detection fruit and vegetable vitamin C mainly contains:
2,6-dichloroindophenol titrimetry: by 2 of blueness, 6-dichloroindophenol solution carries out redox titration to containing ascorbic fruits and vegetables sample acid solution, during beginning 2,6-dichloroindophenol blue solution is reduced to colourless, when reaching titration end-point, unnecessary 2,6-dichloroindophenol blue solution presents light red in acid medium, by 2, and the ascorbic content of reduced form in the 6-dichloroindophenol solution usage calculation sample.2, though 6-dichloroindophenol titrimetry is the national standard method (GB/T6195-1986) that China's fruit, vegetables Vit C contents are measured, but measuring process need be carried out processing such as fruit making beating, constant volume, filtration, titration, demarcation, it is bigger that measurement result is influenced by human factor, detection speed is slow, detection efficiency is low, and needs to buy expensive chemical reagent, detects the cost height.
2, the 4-dinitro phenyl hydrazine method: total ascorbic acid comprises the ancient happy saccharic acid of reduced form, dehydrogenation type and diketone, by activated charcoal reduced form ascorbic acid (vitamin C) in the fruit sample is oxidized to hydroascorbic acid, again with 2, the effect of 4-dinitrophenylhydrazine generates red osazone, be directly proportional with total ascorbic acid content according to the content of osazone in sulfuric acid solution, carry out colorimetric assay.2, though the 4-dinitro phenyl hydrazine method is the national standard method (GB/T12392-1990) that total ascorbic acid is measured in China vegetables, fruit and the goods thereof, but measuring process need be carried out processing such as fruit making beating, constant volume, filtration, water-bath, colorimetric, curve plotting, it is bigger that measurement result is influenced by human factor, detection speed is slow, detection efficiency is low, and needs to buy expensive chemical reagent, detects the cost height.
High performance liquid chromatography: by high performance liquid chromatograph the fruits and vegetables samples of juice is analyzed, the vitamin C in the fruits and vegetables sample after oxalic acid solution extracts rapidly, separation determination on reverse-phase chromatographic column.Though high performance liquid chromatography be multiple component content is measured in China's food, the feed national standard method (for example: GB/T 19861-2005: the detection method of tonyred dyestuff in the food; GB/T 17817-1999: the assay method of vitamin A in the feed), but measuring process needs processing such as making beating, constant volume, filtration, stratographic analysis, and must be equipped with equipment such as high performance liquid chromatograph, UV-detector, integraph, so the method complicated operation, the instrument costliness of using, detection cost height, sense cycle is long.
Summary of the invention
In order to overcome the existing various defectives of above-mentioned detection method, the invention provides a kind of method that detects fruit, vegetables Vit C contents with the spectral analysis technique quick nondestructive.The method can not only realize that quick nondestructive detects the content of fruit and vegetable vitamin C, and does not need sample is carried out Chemical Pretreatment, does not need to buy expensive chemical reagent.From testing result, the present invention can carry out fast fruit and vegetable vitamin C content, harmless, effective and easy detection.
The optical spectrum rapid nondestructive detection method of fruit and vegetable vitamin C content may further comprise the steps:
(1) sample collecting: collect representational sample in the fruits and vegetables, comprise from now on desired sample chemical character in the actual analysis as far as possible;
(2) the modeling sample collection is selected: select the sample sets of the wider sample of concentration range as mathematical modeling from representational sample;
(3) modeling sample spectra collection: fruit and vegetable surfaces is after simple process, and each sample position is under the line gathered a spectrum every 120 degree, gets three spectrum and asks average;
(4) measure with reference to chemical score: use the national standard assay method carries out the inside quality Vit C contents to the fruits and vegetables sample of having gathered mensuration;
(5) mathematical model is set up: use the multivariate calibration methods in the Chemical Measurement, set up the mathematical model between the Vit C contents and absorption spectrum in the tested fruits and vegetables sample;
(6) calibration model checking: get the sample of known fruit and vegetable vitamin C content, under the same conditions, measure its absorption spectrum, the Vit C contents according to the concentrated fruits and vegetables sample of having set up of correction calculated with mathematical model checking requires the checking error less than 10%;
(7) unknown sample prediction: behind the scanning unknown sample spectrum, fruits and vegetables sample Vit C contents is predicted comparison with building mathematical model and spectrum thereof.
(8) mathematical model after establishment is proofreaied and correct.
(9) testing sample is carried out spectroscopic assay.
(10) spectroscopic data that records is imported the mathematical model of determining.
(11) obtain ascorbic content.
Has fibre-optical probe in the pick-up unit according to such scheme foundation, in fibre-optical probe, has light source, fibre-optical probe is contained in movably on the erecting frame, handle is housed on fibre-optical probe, handle and light source irradiation are 45 degree to the depression angle of fruits and vegetables glazed thread, be equipped with in the handle and accept catoptrical optical fiber transmission line, optical fiber transmission line is connected with spectrometer, spectrometer is connected with the computing machine with spectral manipulation software by the data cable line, and described light source, spectrometer and computing machine are connected with external power supply through supporting power lead.
The acquisition range of spectrum is 350-1800nm, belongs to visible light and near infrared spectrum district, and light source adopts the 50W halogen tungsten lamp.
Near infrared spectrum (Near Infrared Spectroscopy, NIRS) being electromagnetic wave between visible light (VIS) and mid-infrared light (MIR), is 780-2526nm (12820-3959cm according to the wavelength coverage in the near infrared spectrum district of American Society for Tests and Materials (ASTM) definition -1).Near infrared spectrum mainly is because the anharmonicity of molecular vibration makes molecular vibration produce when the high level transition from ground state, what write down mainly is the frequency multiplication and the sum of fundamental frequencies absorption of hydrogeneous radicals X-H (X=C, N, O) vibration, different groups (as methyl, methylene, phenyl ring etc.) or near infrared absorption wavelength and the intensity of same group in the different chemical environment all have significant difference, near infrared spectrum has abundant structures and composition information, and the composition and the character that are suitable for very much carbon-hydrogen organic are measured.The spectral signature of visible-range can reflect visual signatures such as the color and luster, shape, texture of fruit sample.The essential characteristic of visible light and near-infrared diffuse reflection spectrum is that quick nondestructive detection fruit and vegetable vitamin C content has been established theoretical foundation.The fruits and vegetables sample of known vitamin C chemical measurement value and its visible light and near-infrared diffuse reflection spectrum are carried out the correlativity mathematical modeling, after model adaptability and reliability demonstration, as long as record the visible light and the near-infrared diffuse reflection spectrum of unknown fruits and vegetables sample, spectrum is directed into the mathematical model of building, just can realizes that quick nondestructive detects the testing goal of fruit sample Vit C contents.
The present invention solves the testing scheme that its technical matters adopts:
A kind of fruit of mutual relationship between fruit, vegetables vitamin C and the spectrum, fast non-destructive detection method of vegetables Vit C contents of being based upon; Spectrometer links to each other with computing machine by two-way parallel interface cable data line, links to each other with external power supply through supporting power lead simultaneously; Visible light and near-infrared diffuse reflection fibre are connected on spectrometer and the light source handle, make the light that comes out through the inner diffuse reflection of fruits and vegetables be transmitted through the fiber to detecting device in the spectrometer; Light source is fixed in the fibre-optical probe, and the light source depression angle is 45 degree; Fix the relative position of fruits and vegetables, light source, optical fiber and spectrometer, light source irradiation is at the fruit and vegetable surfaces with the optical fiber probe support, through fruits and vegetables internal reflection and scattering, by the detecting device of Optical Fiber Transmission to the spectrometer, collect the spectrum picture of fruits and vegetables sample, convert the spectrum master data to by spectral manipulation software again, by multivariate calibration methods in the Chemical Measurement software ascorbic chemical measurement value of fruit and spectrum master data are carried out mathematical then, set up model, through overcorrect, the mathematical model after determining at last to proofread and correct.The sample that needs are measured carries out spectroscopic assay, and the spectrum that records is imported the mathematical model of determining, obtains the Vit C contents of sample at last.
The fruit that is fit to the method for spectrum quick nondestructive detection fruit and vegetable vitamin C content can be tangerine orange, navel orange, apple, pears, strawberry etc., and vegetables can be cucumber, eggplant, tomato, taro, potato, radish, sponge gourd etc.
The present invention's beneficial effect that has of comparing with background technology is:
(1) analysis speed is fast, and the spectroscopic assay process can be finished in 1 second;
(2) the fruits and vegetables sample does not need pre-service, reaches nondestructive measurement;
(3) have higher degree of accuracy, reduce personal error;
(4) analysis result accuracy is approached standard method;
(5) do not need chemical reagent, reduce and detect cost, free from environmental pollution;
(6) can measure multiple composition and index simultaneously.
Description of drawings
Fig. 1 is the spectrum quick nondestructive pick-up unit figure of fruit and vegetable vitamin C content of the present invention;
Fig. 2 is a process flow diagram of the present invention;
Fig. 3 is the original averaged spectrum curve map of the typical modeling sample of three kinds of different cultivars of Nanfeng orange;
Fig. 4 is that 90 Nanfeng orange modeling samples are proofreaied and correct and inner validation-cross model scatter diagram fully;
Fig. 5 is the outside prediction of 20 a Nanfeng oranges scatter diagram.
Embodiment
With Nanfeng orange fruit sample is the method that example explanation spectrum quick nondestructive detects Vit C contents.
Three kinds of different cultivars of Nanfeng orange (Jiangxi provinces and cities mountain town fruitlet system, the big fruit in Jiangxi provinces and cities mountain town system, Jiangxi Province's POLO town fruitlet system) are used to set up calibration model, and detection procedure as shown in Figure 2.
(1) sample collecting: totally 110 and guarantee that these fruit sample surfaces and inside do not have open defect of three kinds of Nanfeng orange of plucking the maturity stage from Jiangxi provinces and cities mountain town, POLO town;
(2) the modeling sample collection is selected: select the sample sets of wide and 90 samples being evenly distributed of Vit C contents scope as mathematical modeling from 110 representational fruit samples;
(3) modeling sample spectra collection: fruit surface is after simple process, utilize the Indico V4.0 of U.S. ASD company or the Unsorambler V9.5 spectra collection software of Norway CAMO company that each sample is spent spectrum of collection in interval, position 120 under the line, get three spectrum and ask average.The typical mean absorption spectrum of three kinds of different cultivars of Nanfeng orange as shown in Figure 3;
(4) measure with reference to chemical score: use 2,6-dichloroindophenol titrimetry (GB/T 6195-1986) is carried out the mensuration of inside quality Vit C contents to 90 Nanfeng orange samples having gathered;
(5) mathematical model is set up: utilize the PLS1 method in the Unscrambler V9.5 multivariate statistics software of Norway CAMO company, set up the correction mathematical model between the vitamin C chemical assay value and visible light and near-infrared diffuse reflectance absorption spectrum in the sample, the results are shown in Figure 4;
(6) calibration model checking: in Unscrambler V9.5 multivariate statistics software, adopt inner cross verification (leave-one-out proof method) fully when setting up the correction mathematical model, model to be verified, the results are shown in Figure 4, its checking square error is 1.6284mg/100g;
(7) unknown sample prediction: behind the Nanfeng orange unknown sample scanning visible light and near-infrared diffuse reflection spectrum of 20 different cultivars, using positive mathematical model for school building and spectrum thereof predicts the sample Vit C contents, the results are shown in Figure 5, the mathematical model after determining to proofread and correct;
(8) sample to be measured is carried out spectroscopic assay, the spectroscopic data that records is imported the mathematical model of determining, obtain ascorbic content at last.
Fig. 1 has shown a kind of pick-up unit, tangerine orange 1 is placed on the rubber washer 2 on the fibre-optical probe 3, in fibre-optical probe, has light source 4, be the 50W halogen tungsten lamp, fibre-optical probe is contained in movably on the erecting frame 5, is equipped with to accept catoptrical optical fiber transmission line 6 in the fibre-optical probe handle, adopts the standard reflection probe of U.S. ASD company, optical fiber transmission line is connected with spectrometer 7, and spectrometer adopts the Quality Spec of U.S. ASD company
Figure A20071013031400071
The pro spectrometer, spectrometer is connected with the computing machine 9 with spectral manipulation software by data cable line 8, data processing software is the Indico V4.0 of U.S. ASD company, detecting device is silicon detecting device (350-1000nm) and indium gallium arsenic detecting device (1000-1800cm), and optical fiber adopts the standard reflection fibre-optical probe of U.S. ASD company.Multivariate calibration methods is partial least square method (PLS) in the mathematical modeling.20 tangerine orange are listed in the table 1 through the ascorbic value that chemical measurement and spectral measurement obtain.
Show the contrast of 1:20 unknown sample predicted value and chemical reference value numerical value
Table 1 has shown spectrum predicted value and the chemical reference value that each sample records, and the checking square error that difference has between the two met mathematical model is 1.6248mg/100g.

Claims (4)

1、果蔬维生素C含量的光谱快速无损检测方法，其特征在于：它包括以下几个步骤：1. The method for rapid and non-destructive detection of vitamin C content in fruits and vegetables, characterized in that it comprises the following steps: (1)样品采集：收集果蔬中有代表性的样品，尽量包括今后实际分析中所要求的样品化学性质；(1) Sample collection: collect representative samples of fruits and vegetables, and try to include the chemical properties of the samples required in the actual analysis in the future; (2)建模样品集选择：从有代表性的样品中选择浓度范围较广的样品作为数学建模的样品集；(2) Modeling sample set selection: select samples with a wide concentration range from representative samples as the sample set for mathematical modeling; (3)建模样品光谱采集：果蔬表面经简单处理后，每个样品在赤道部位每隔120度采集一次光谱，取三次光谱求平均；(3) Spectrum collection of modeling samples: After simple treatment of the surface of fruits and vegetables, each sample collects a spectrum every 120 degrees at the equator, and takes the average of three spectra; (4)参考化学值测定：应用国家标准测定方法对已采集的果蔬样品进行内部品质维生素C含量的测定；(4) Determination of reference chemical value: Determination of internal quality vitamin C content of collected fruit and vegetable samples by national standard determination method; (5)数学模型建立：使用化学计量学中的多元校正方法，建立被测果蔬样品中维生素C含量与吸收光谱之间的数学模型；(5) Mathematical model establishment: use the multivariate calibration method in chemometrics to establish a mathematical model between the vitamin C content and absorption spectrum in the tested fruit and vegetable samples; (6)校正模型验证：取已知果蔬维生素C含量的样品，在相同条件下，测定其吸收光谱，根据已建立的校正数学模型计算验证集中果蔬样品的维生素C含量，要求验证误差小于10％；(6) Calibration model verification: Take samples with known vitamin C content of fruits and vegetables, measure their absorption spectra under the same conditions, and calculate the vitamin C content of fruit and vegetable samples in the verification set according to the established calibration mathematical model, and the verification error is required to be less than 10%. ; (7)未知样品预测：扫描未知样品光谱后，用已建数学模型及其光谱对果蔬样品维生素C含量进行预测比较。(7) Prediction of unknown samples: After scanning the spectra of unknown samples, use the established mathematical model and its spectra to predict and compare the vitamin C content of fruit and vegetable samples. (8)确立校正后的数学模型。(8) Establish the corrected mathematical model. (9)对待测样品进行光谱测定。(9) Spectrum measurement is carried out on the sample to be tested. (10)将测得的光谱数据导入确定的数学模型。(10) Import the measured spectral data into a determined mathematical model. (11)得到维生素C的含量。(11) Get the content of vitamin C. 2、根据权利要求1所述的果蔬维生素C含量的光谱快速无损检测方法，其特征在于检测装置中具有光纤探头，在光纤探头内具有光源，光纤探头装在可移动的安装架上，在光纤探头上装有手柄，手柄与光源照射到果蔬上光线的俯视角为45度，手柄内装有接受反射光的的光纤传输线，光纤传输线与光谱仪连接，光谱仪通过数据电缆线与具有光谱处理软件的计算机连接，所述光源、光谱仪和计算机经配套电源线与外接电源连接。2. The spectral rapid non-destructive detection method of vitamin C content in fruits and vegetables according to claim 1, characterized in that the detection device has an optical fiber probe, a light source is provided in the optical fiber probe, the optical fiber probe is mounted on a movable mounting frame, The probe is equipped with a handle, and the angle of view between the handle and the light source irradiated on the fruits and vegetables is 45 degrees. The handle is equipped with an optical fiber transmission line to receive reflected light. The optical fiber transmission line is connected to the spectrometer, and the spectrometer is connected to the computer with spectral processing software through a data cable. , the light source, the spectrometer and the computer are connected to an external power supply via a supporting power cord. 3、根据权利要求1或2所述的果蔬维生素C含量的光谱快速无损检测方法，其特征在于：采用的光谱区间范围为350-1800nm。3. The rapid spectral non-destructive detection method for vitamin C content in fruits and vegetables according to claim 1 or 2, characterized in that: the spectral range used is 350-1800nm. 4、根据权利要求3所述的果蔬维生素C含量的光谱快速无损检测方法，其特征在于：光源采用50W卤钨灯。4. The spectral rapid nondestructive detection method for vitamin C content in fruits and vegetables according to claim 3, characterized in that: the light source is a 50W halogen tungsten lamp.
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102768193A (en) * 2011-05-04 2012-11-07 中国科学技术大学 Infrared spectroscopic method for rapid determination of storage substance content in activated sludge cell
CN104359856A (en) * 2014-11-19 2015-02-18 天津市傲绿农副产品集团股份有限公司 Near-infrared nondestructive testing device for fruits
CN105004690A (en) * 2015-07-30 2015-10-28 合肥工业大学 Rapid and nondestructive testing method of sclereid content in pear pulp based on multi-spectral imaging technology
CN105486657A (en) * 2015-12-31 2016-04-13 深圳市芭田生态工程股份有限公司 Method for measuring main nutritional components of leaf vegetables through spectrometry
CN105512430A (en) * 2015-12-31 2016-04-20 深圳市芭田生态工程股份有限公司 Shared input and output system of spectroscopic data and chemical detection data
CN105628648A (en) * 2015-12-31 2016-06-01 深圳市芭田生态工程股份有限公司 Method for measuring vitamin C in agricultural product by utilization of spectroscopic method
CN105675515A (en) * 2015-12-31 2016-06-15 深圳市芭田生态工程股份有限公司 Method for determining main nutrition components in watermelons through using spectroscopy
CN111198168A (en) * 2020-03-06 2020-05-26 益海嘉里（兖州）粮油工业有限公司 Method for rapidly predicting vitamin C in flour sample

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102768193A (en) * 2011-05-04 2012-11-07 中国科学技术大学 Infrared spectroscopic method for rapid determination of storage substance content in activated sludge cell
CN104359856A (en) * 2014-11-19 2015-02-18 天津市傲绿农副产品集团股份有限公司 Near-infrared nondestructive testing device for fruits
CN104359856B (en) * 2014-11-19 2017-04-26 天津市傲绿农副产品集团股份有限公司 Near-infrared nondestructive testing device for fruits
CN105004690A (en) * 2015-07-30 2015-10-28 合肥工业大学 Rapid and nondestructive testing method of sclereid content in pear pulp based on multi-spectral imaging technology
CN105486657A (en) * 2015-12-31 2016-04-13 深圳市芭田生态工程股份有限公司 Method for measuring main nutritional components of leaf vegetables through spectrometry
CN105512430A (en) * 2015-12-31 2016-04-20 深圳市芭田生态工程股份有限公司 Shared input and output system of spectroscopic data and chemical detection data
CN105628648A (en) * 2015-12-31 2016-06-01 深圳市芭田生态工程股份有限公司 Method for measuring vitamin C in agricultural product by utilization of spectroscopic method
CN105675515A (en) * 2015-12-31 2016-06-15 深圳市芭田生态工程股份有限公司 Method for determining main nutrition components in watermelons through using spectroscopy
CN111198168A (en) * 2020-03-06 2020-05-26 益海嘉里（兖州）粮油工业有限公司 Method for rapidly predicting vitamin C in flour sample

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Open date: 20090121