CN104062411A - Method for determining crude fiber content in citrus by texture determination - Google Patents
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Abstract
Description
技术领域technical field
本发明涉及柑橘中粗纤维含量的测定方法，尤其涉及一种用质构仪测定柑橘中粗纤维含量的方法。The invention relates to a method for measuring the crude fiber content in citrus, in particular to a method for measuring the crude fiber content in citrus with a texture analyzer.
背景技术Background technique
膳食纤维是柑橘类水果中的一种重要营养素，这类营养素是健康饮食不可缺少的，它在保持人体消化系统健康上扮演者重要的角色，同时可以预防多种疾病。膳食纤维中的纤维素和半纤维素可以清洁消化壁，增强消化功能，同时可以稀释和加速食物中的致癌物质和有毒物质的移除，保护脆弱的消化道和预防结肠癌。因此，食物中粗纤维素的测定就显得十分重要。柑橘类产品中的膳食纤维包括纤维素、半纤维素、木质素和原果胶等，其中纤维素、半纤维素和木质素为粗纤维的主要组成部分。目前我国主要是采用洗涤剂法测定柑橘中的粗纤维含量，这种测定方法过程极为繁琐，且会不可避免的产生误差，比如试剂的量取、温度控制、残渣冲洗过程中产生的误差。因此，需要找到一种客观、简单、快速、准确地测定柑橘粗纤维含量的方法。Dietary fiber is an important nutrient in citrus fruits. This nutrient is indispensable for a healthy diet. It plays an important role in maintaining the health of the human digestive system and can prevent many diseases. The cellulose and hemicellulose in dietary fiber can clean the digestive wall and enhance digestive function. At the same time, it can dilute and accelerate the removal of carcinogens and toxic substances in food, protect the fragile digestive tract and prevent colon cancer. Therefore, the determination of crude cellulose in food is very important. Dietary fiber in citrus products includes cellulose, hemicellulose, lignin and protopectin, among which cellulose, hemicellulose and lignin are the main components of crude fiber. At present, the detergent method is mainly used in my country to determine the crude fiber content in citrus. This determination method is extremely cumbersome and inevitably produces errors, such as errors in the amount of reagents, temperature control, and residue washing. Therefore, it is necessary to find an objective, simple, fast and accurate method for determining the crude fiber content of citrus.
发明内容Contents of the invention
为了克服上述现有技术的不足，本发明专利的目的在于提供一种用质构试验测定柑橘中粗纤维含量的方法，该方法快速便捷，可用于工业化连续操作。In order to overcome the above-mentioned deficiencies in the prior art, the purpose of the patent of the present invention is to provide a method for measuring crude fiber content in citrus with texture test, which is fast and convenient, and can be used for industrial continuous operation.
本发明提供的一种柑橘粗纤维含量的测定方法，包括如下步骤：A kind of assay method of citrus crude fiber content provided by the invention comprises the steps:
1)柑橘预处理；1) citrus pretreatment;
2)对所述步骤1)所得到的柑橘进行TPA试验和剪切试验，得到柑橘质构特征信息；2) Carry out TPA test and shear test to the citrus that described step 1) obtains, obtain the citrus texture characteristic information;
3)对所述步骤2)得到的质构特征信息进行预处理，得到柑橘质构特征信息数据；3) Preprocessing the texture characteristic information obtained in the step 2) to obtain citrus texture characteristic information data;
4)对所述步骤2)得到的柑橘用范氏法测定粗纤维含量，得到其化学测定值；4) the citrus that described step 2) obtains is measured crude fiber content with Fan's method, obtains its chemical measurement value;
5)回归模型的建立：5) Establishment of regression model:
将所述步骤3)所得的质构特征信息数据作为自变量，步骤4)所得的粗纤维含量作为因变量，用统计算法建立所述自变量与所述因变量之间的回归模型(也即粗纤维含量与质构特征信息数据之间的映射关系)；The texture characteristic information data obtained in the step 3) is used as an independent variable, and the crude fiber content obtained in the step 4) is used as a dependent variable, and a statistical algorithm is used to establish a regression model between the independent variable and the dependent variable (that is, The mapping relationship between crude fiber content and texture feature information data);
6)未知粗纤维含量的柑橘样品的测定：6) Determination of citrus samples with unknown crude fiber content:
另外还可取一些待测柑橘样品，重复所述步骤1)至步骤3)，将步骤3)所得到的质构特征信息数据输入所述步骤5)的回归模型，得到所述待测柑橘样品中的粗纤维的含量。In addition, some citrus samples to be tested can be taken, and the steps 1) to 3) are repeated, and the texture characteristic information data obtained in step 3) is input into the regression model of the step 5), to obtain the citrus samples to be tested. content of crude fiber.
上述步骤1)中，所述预处理为柑橘采摘后，在8℃-15℃下保存36小时后剥去果皮。In the above step 1), the pretreatment is peeling off the peel after the citrus is picked at 8°C-15°C for 36 hours.
所述步骤2)中，所述的TPA试验质构特征信息为：硬度和弹性；所述的剪切试验质构特征信息为：最大剪切力和剪切功。In the step 2), the TPA test texture feature information is: hardness and elasticity; the shear test texture feature information is: maximum shear force and shear work.
所述步骤2)中，所述的TPA试验中，质构仪采用P100/R的探头，测前速率为1mm/s、测试速率为0.5mm/s、测后速率均为2mm/s，测试时间间隔为1s，压缩百分比为30％；所述的剪切试验中，质构仪采用燕尾型不锈钢剪刀进行试验，测前速率、测后速率为1mm/s，测试速率为0.5mm/s，剪切距离为15mm。In the step 2), in the TPA test, the texture analyzer adopts the probe of P100/R, the pre-test rate is 1mm/s, the test rate is 0.5mm/s, and the post-test rate is 2mm/s. The time interval is 1s, and the compression percentage is 30%. In the shear test, the texture analyzer adopts dovetail stainless steel scissors to test, the pre-test speed and post-test speed are 1mm/s, and the test speed is 0.5mm/s. The shear distance is 15mm.
所述步骤3)所述预处理包括：将所述步骤2)得到的质构特征信息变换为4-6个互不相关的变量。The preprocessing in the step 3) includes: transforming the texture feature information obtained in the step 2) into 4-6 mutually uncorrelated variables.
所述步骤4)中，所述的粗纤维包括纤维素、半纤维素和木质素；所述的柑橘粗纤维含量的化学测定值是使用范氏法测得的。In the step 4), the crude fiber includes cellulose, hemicellulose and lignin; the chemical determination value of the citrus crude fiber content is measured by the Fan method.
所述步骤5)中，所述的统计算法为多元线性回归算法。In the step 5), the statistical algorithm is a multiple linear regression algorithm.
另外，可按照如下步骤对步骤5)所得回归模型进行实验：另外取一些待测柑橘样品，重复所述步骤1)至步骤3)，将步骤3)所得到的质构特征信息数据输入所述步骤5)的回归模型，得到所述待测柑橘样品中的粗纤维的含量。In addition, the regression model obtained in step 5) can be tested according to the following steps: take some citrus samples to be tested, repeat the steps 1) to 3), and input the texture feature information data obtained in step 3) into the The regression model of step 5) obtains the content of crude fiber in the citrus fruit sample to be tested.
本发明收集了一批具有代表性的柑橘样品例如：奥林达柑橘、伏令柑橘、无核柑橘、红柑橘、康贝尔柑橘、蜜奈柑橘、斯加哥斯柑橘、大果柑橘、福罗斯特柑橘等9个柑橘品种。以这批柑橘作为建立回归模型的样品，提出了一种利用质构仪对柑橘进行TPA试验和剪切试验测定其中的粗纤维含量的方法，该方法应用多元统计方法对柑橘质构特征信息数据和粗纤维含量进行关联研究，可以确定这两者之间的定性或定量关系，即回归模型。建立回归模型后，只要测量出未知样品的质构特征信息数据，根据回归模型就可以确定柑橘的粗纤维的含量。该方法具有分析速度快、分析效率高，不适用任何化学试剂，分析成本低，且对环境不造成任何污染的优点。The present invention collects a batch of representative citrus samples such as: Olinda citrus, Fuling citrus, seedless citrus, red citrus, Campbell citrus, Minai citrus, Skagos citrus, Big Fruit citrus, Foros 9 citrus varieties including special citrus. Taking this batch of citrus as a sample to establish a regression model, a method for determining the crude fiber content in citrus by TPA test and shear test using a texture analyzer is proposed. The association study between the crude fiber content and the crude fiber content can determine the qualitative or quantitative relationship between the two, that is, the regression model. After the regression model is established, as long as the texture characteristic information data of the unknown sample is measured, the crude fiber content of citrus can be determined according to the regression model. The method has the advantages of fast analysis speed and high analysis efficiency, does not apply any chemical reagents, has low analysis cost, and does not cause any pollution to the environment.
具体实施方式Detailed ways
下面结合具体的实施例，并参照数据进一步详细地描述本发明。应理解，这些实施例只是为了举例说明本发明，而并非以任何方式限制本发明的范围。The present invention will be described in further detail below in conjunction with specific examples and with reference to data. It should be understood that these examples are only for illustration of the present invention and are not intended to limit the scope of the present invention in any way.
以下实施例中统一采用SPSS软件进行数据分析。测定指标为柑橘的硬度(hardness，HN)、弹性(springiness，SN)、最大剪切力(shear force，SF)、剪切功(shear work，SW)和柑橘的纤维素、半纤维素、木质素。In the following examples, SPSS software was uniformly used for data analysis. The determination indexes are hardness (hardness, HN), elasticity (springiness, SN), maximum shear force (shear force, SF), shear work (shear work, SW) of citrus and citrus cellulose, hemicellulose, wood white.
试验仪器：美国FTC公司生产的TMS-CONSOLE型号的质构仪、榨汁机、水浴锅、温度计等。Test instruments: TMS-CONSOLE texture analyzer, juice extractor, water bath, thermometer, etc. produced by FTC Corporation of the United States.
实施例1：Example 1:
1)柑橘预处理：2012年5月上中旬采摘三峡库区秭归县柑橘，包括奥林达柑橘、伏令柑橘、无核柑橘、红柑橘、康贝尔柑橘、蜜奈柑橘、斯加哥斯柑橘、大果柑橘、福罗斯特柑橘等9个柑橘品种，每个品种在树冠中部外围分别采果30个，取圆球形、无损伤、无斑点，外表面光滑果实。将采摘后的柑橘在8℃-15℃下保存36小时，剥去柑橘的果皮。1) Citrus pretreatment: Citrus in Zigui County in the Three Gorges Reservoir area was picked in early and mid-May 2012, including Olinda citrus, Fuling citrus, seedless citrus, red citrus, Campbell citrus, Minai citrus, and Skagos citrus 9 citrus varieties, such as citrus, big fruit citrus, and frost citrus, each variety harvested 30 fruits in the middle of the canopy, taking spherical, no damage, no spots, smooth outer surface fruit. Preserve the picked citrus at 8°C-15°C for 36 hours, and peel off the peel of the citrus.
2)TPA试验和剪切试验：2) TPA test and shear test:
TPA试验：将步骤1)预处理后的柑橘置于实验台上，采用P100/R的探头，测前速率为1mm/s、测试速率为0.5mm/s、测后速率均为2mm/s，测试时间间隔为1s，压缩百分比为30％。方式为纵向压缩，压缩部位为柑橘顶部果梗区，每个品种随即选取10个进行试验，实验结果取平均值。TPA test: the citrus after step 1) pretreatment is placed on the test bench, using the probe of P100/R, the pre-test rate is 1mm/s, the test rate is 0.5mm/s, and the post-test rate is 2mm/s. The test time interval is 1s, and the compression percentage is 30%. The method is longitudinal compression, and the compression part is the top fruit stem area of citrus. 10 samples of each variety are randomly selected for testing, and the experimental results are averaged.
剪切试验：将步骤1预处理后的柑橘取一瓣置于质构仪平台，采取燕尾型不锈钢剪刀进行试验，测前速率、测后速率为1mm/s，测试速率为0.5mm/s，剪切距离为15mm。样品在室温条件下测定。每类品种选取6-8个果样，每个样品抽取4瓣进行平行试验。Shear test: Take a piece of citrus pretreated in step 1 and put it on the texture analyzer platform, and use dovetail stainless steel scissors for the test. The pre-test rate and post-test rate are 1mm/s, and the test rate is 0.5mm/s. The shear distance is 15mm. Samples were measured at room temperature. 6-8 fruit samples were selected for each variety, and 4 petals were selected from each sample for parallel testing.
3)将步骤2)和步骤3)TPA试验和剪切试验后得到的质构特征信息进行预处理，得到质构特征信息数据；3) Preprocessing the texture characteristic information obtained after the step 2) and step 3) TPA test and shear test to obtain texture characteristic information data;
4)粗纤维的测定：对所述步骤2)得到的柑橘用范氏法进行粗纤维含量的测定，步骤如下：4) mensuration of crude fiber: described step 2) the mandarin fruit that obtains carries out the mensuration of crude fiber content with Fan's method, and step is as follows:
测定粗纤维里3种主要成分：纤维素、半纤维素和木质素。实验之前将柑橘榨汁制成干样，将0.5g干样用3％中性洗涤剂(SDS)在沸水浴中水解lh，过滤后用蒸馏水和丙酮洗涤残渣3次，残渣用2M HCl 100℃保温50min，过滤，水洗残渣至pH6.5-7.0，将滤液定容至100ml用于半纤维素含量的测定，方法为地衣酚法，以木糖为标样，均重复测定3次。将洗涤后的残渣用72％H2SO4于35℃水解1h，然后加入4倍体积的蒸馏水，100℃水解1h，过滤后取滤液，用葱酮比色法测定纤维素含量。木质素是纤维素过滤后的残渣80℃至恒重的重量。以上均重复测定3次。纤维素、半纤维素和木质素含量的总和为柑橘粗纤维含量。Determination of 3 main components in crude fiber: cellulose, hemicellulose and lignin. Before the experiment, the citrus juice was squeezed to make a dry sample, and 0.5 g of the dry sample was hydrolyzed with 3% neutral detergent (SDS) in a boiling water bath for 1 hour, and after filtering, the residue was washed with distilled water and acetone for 3 times, and the residue was washed with 2M HCl at 100°C Incubate for 50 minutes, filter, wash the residue to pH 6.5-7.0, and dilute the filtrate to 100ml for the determination of hemicellulose content. The method is the orcinol method, with xylose as the standard sample, and the determination is repeated 3 times. The residue after washing was hydrolyzed with 72% H2SO4 at 35°C for 1h, then 4 times the volume of distilled water was added, hydrolyzed at 100°C for 1h, after filtration, the filtrate was taken, and the cellulose content was determined by the allthone colorimetric method. Lignin is the weight of the residue after cellulose filtration from 80°C to constant weight. The above measurements were repeated 3 times. The sum of cellulose, hemicellulose and lignin content is the citrus crude fiber content.
5)回归模型的建立：将所述步骤3)所得的质构特征信息数据作为自变量，步骤4)所得的粗纤维含量作为因变量，用多元线性回归算法建立所述自变量与所述因变量之间的回归模型(也即粗纤维素含量与质构特征信息数据之间的映射关系)；所得模型结果如表1所示：5) Establishment of a regression model: the texture feature information data obtained in the step 3) is used as an independent variable, and the crude fiber content obtained in the step 4) is used as a dependent variable, and the independent variable and the dependent variable are established with a multiple linear regression algorithm. The regression model between the variables (that is, the mapping relationship between the crude cellulose content and the texture characteristic information data); the obtained model results are shown in Table 1:
表1质构特征信息数据与粗纤维含量的相关分析Table 1 Correlation analysis between texture characteristic information data and crude fiber content
注：*.在0.05水平(双侧)上显著相关。**.在.01水平(双侧)上显著相关。Note: * . Significantly correlated at the 0.05 level (two-sided). ** . Significantly correlated at the .01 level (two-sided).
由表1可知：果实粗纤维主要与硬度、弹性相关，因此将果实粗纤维(CC)作为因变量，进行逐步回归分析，得到回归方程如下：It can be seen from Table 1 that the fruit crude fiber is mainly related to hardness and elasticity, so the fruit crude fiber (CC) is used as the dependent variable, and the stepwise regression analysis is carried out, and the regression equation is obtained as follows:
CC＝312.62+0.99HN-4.324SN+0.343SF+0.358SW (R＝0.917)CC＝312.62+0.99HN-4.324SN+0.343SF+0.358SW (R＝0.917)
据以上方程，质构特征信息数据与粗纤维含量之间均表现出一定相关性，硬度和弹性与粗纤维素存在负相关性，而最大剪切力和切断功与其存在显著的正相关性，剪切参数越大，粗纤维含量越高。According to the above equation, there is a certain correlation between the texture characteristic information data and the crude fiber content, there is a negative correlation between the hardness and elasticity and the crude cellulose, and there is a significant positive correlation between the maximum shear force and the work of cutting. The larger the shear parameter, the higher the crude fiber content.
果实粗纤维的回归方程决定系数达0.9以上，说明其拟合程度很高，可以通过将柑橘的质构特征信息数据代入此方程来得到柑橘粗纤维的含量。The coefficient of determination of the regression equation of fruit crude fiber is more than 0.9, indicating that its fitting degree is very high, and the content of citrus crude fiber can be obtained by substituting the texture characteristic information data of citrus into this equation.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104374887A (en) * | 2014-11-20 | 2015-02-25 | 江西农业大学 | Physical checking method for melting property of citrus fruit |
| CN106323803A (en) * | 2016-08-16 | 2017-01-11 | 天津市农业质量标准与检测技术研究所 | Method for rapidly determining coarse fiber content in plant-caused agricultural product |
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| CN202049082U (en) * | 2011-04-14 | 2011-11-23 | 济南海能仪器有限公司 | Crude fiber test instrument |
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| CN202049082U (en) * | 2011-04-14 | 2011-11-23 | 济南海能仪器有限公司 | Crude fiber test instrument |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104374887A (en) * | 2014-11-20 | 2015-02-25 | 江西农业大学 | Physical checking method for melting property of citrus fruit |
| CN106323803A (en) * | 2016-08-16 | 2017-01-11 | 天津市农业质量标准与检测技术研究所 | Method for rapidly determining coarse fiber content in plant-caused agricultural product |
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