CN103529170B - A kind of on-line checking automatic control system of starch saccharification finishing point - Google Patents
A kind of on-line checking automatic control system of starch saccharification finishing point Download PDFInfo
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Abstract
本发明公开了一种淀粉糖化终点的在线检测方法及自动控制系统，该方法为：测定糖化液的葡萄糖以及还原糖含量；通过公式E＝CG/CR计算，当E达到0.98‑0.99区间，则可判定到达糖化终点，E表述糖化终点，CG表示葡萄糖含量，CR表示还原糖含量；该系统包括：主控处理器、全自动还原糖测定仪、生物传感分析仪、糖化条件执行单元。本发明通过测定糖化液中葡萄糖、还原糖的含量，计算葡萄糖和还原糖比值，确定糖化终点；固定化酶葡萄糖生物传感分析仪和还原糖测定仪可进行葡萄糖和还原糖的测定，方法简单，快速、准确，而且不需测定干物质含量，具备了在实际生产中的可行性和实用性，较好的解决了现有的测定方法操作复杂，工作效率低，限制了制糖工业的发展的问题。
The invention discloses an online detection method and an automatic control system for the end point of starch saccharification. The method comprises: measuring the glucose and reducing sugar content of the saccharification liquid; calculating by the formula E=C G /C R , when E reaches the range of 0.98-0.99 , it can be determined that the saccharification end point has been reached, E represents the saccharification end point, C G represents the glucose content, and C R represents the reducing sugar content; the system includes: main control processor, automatic reducing sugar tester, biosensor analyzer, saccharification condition execution unit. The present invention determines the end point of saccharification by measuring the content of glucose and reducing sugar in the saccharification liquid, calculating the ratio of glucose and reducing sugar; the immobilized enzyme glucose biosensing analyzer and reducing sugar measuring instrument can measure glucose and reducing sugar, and the method is simple , fast, accurate, and does not need to measure the dry matter content, it has the feasibility and practicability in actual production, and better solves the complicated operation and low work efficiency of the existing determination methods, which limit the development of the sugar industry The problem.
Description
技术领域 technical field
本发明属于淀粉糖化终点检测技术领域，尤其涉及一种淀粉糖化终点的在线检测方法及自动控制系统。 The invention belongs to the technical field of starch saccharification end point detection, and in particular relates to an on-line detection method and an automatic control system for the starch saccharification end point.
背景技术 Background technique
目前，淀粉制糖多采用酶法工艺，经过液化和糖化过程，将淀粉水解成葡萄糖，在液化工序中，淀粉经a-淀粉酶水解成糊精和低聚糖范围较小分子产物；糖化工序则是利用葡萄糖淀粉酶进一步将这些产物水解成葡萄糖。 At present, starch sugar production mostly adopts enzymatic process. After liquefaction and saccharification process, starch is hydrolyzed into glucose. In the liquefaction process, starch is hydrolyzed by a-amylase into dextrin and oligosaccharide range smaller molecular products; saccharification process These products are then further hydrolyzed into glucose using glucoamylase.
糖化操作过程是将淀粉液化液引入糖化罐中，调节到适当的温度和pH值，加入需要量的糖化酶制剂，保持一定时间，使达到最高的葡萄糖含量，即得糖化液； The saccharification operation process is to introduce the starch liquefaction solution into the saccharification tank, adjust to an appropriate temperature and pH value, add the required amount of glucoamylase preparation, and keep it for a certain period of time to achieve the highest glucose content, that is, the saccharification solution;
当糖化液达到最高的葡萄糖含量以后，应当停止反应，否则，葡萄糖含量趋向降低，这是因为葡萄糖发生复合反应，一部分葡萄糖又重新结合生成异麦芽糖等复合糖类，这种反应在较高的酶浓度和底物浓度的情况下更为显著，葡萄糖淀粉酶对于葡萄糖的复合反应具有催化作用； When the saccharification solution reaches the highest glucose content, the reaction should be stopped, otherwise, the glucose content tends to decrease, this is because the glucose undergoes a compound reaction, and a part of the glucose is recombined to form complex sugars such as isomaltose, which is reacted at a higher enzyme It is more significant in the case of concentration and substrate concentration, glucoamylase has a catalytic effect on the complex reaction of glucose;
在糖化反应终点及时终止糖化反应对提高糖化效率、缩短生产周期、保证糖化液质量有重要的作用，在实际生产中一般使用DE值(也称葡萄糖值)或DX值(葡萄糖)表示淀粉水解的程度或糖化程度，控制糖化终点， Terminating the saccharification reaction in time at the end of the saccharification reaction plays an important role in improving the saccharification efficiency, shortening the production cycle, and ensuring the quality of the saccharification solution. In actual production, DE value (also called glucose value) or DX value (glucose) is generally used to indicate the hydrolysis rate of starch. degree or degree of glycation, control the end point of glycation,
DE值：糖化液中还原性糖(以葡萄糖计)占干物质的百分比， DE value: the percentage of reducing sugar (calculated as glucose) in the dry matter in the saccharification solution,
DE值＝{还原糖(C″)/干物质(W′)×糖液比重(d)}×100％ DE value = {reducing sugar (C″)/dry matter (W′) × specific gravity of sugar solution (d)} × 100%
其中：还原糖用裴林氏法或碘量法测定，浓度表示：葡萄糖g/100ml糖液；干物质用阿贝折光仪测定，浓度表示：干物质g/100g糖液； Among them: reducing sugar is measured by Perrin's method or iodometric method, and the concentration is expressed as: glucose g/100ml sugar solution; dry matter is measured by Abbe refractometer, and the concentration is expressed as: dry matter g/100g sugar solution;
DX值：糖液中葡萄糖含量占干物质的百分比， DX value: the percentage of glucose content in the sugar solution to the dry matter,
DX值＝{葡萄糖(C″)/干物质(W′)×糖液比重(d)}×100％； DX value = {glucose (C")/dry matter (W') × specific gravity of sugar solution (d)} × 100%;
糖化过程中葡萄糖的实际含量低于葡萄糖值(还原糖)，因为还有还原性低聚糖存在，随着糖化程度的增高，二者的差别逐渐减少，因此，采用葡萄糖和还原糖比值，即DX/DE比值，可以确定糖化工艺进程和糖化终点，目前国内稳定的生产工艺中，糖化液的葡萄糖含量DX大于95.5％，葡萄糖值DE一般大于98％，DX/DE比值大于97.5％。 The actual content of glucose in the saccharification process is lower than the glucose value (reducing sugar), because there are reducing oligosaccharides. As the degree of saccharification increases, the difference between the two gradually decreases. Therefore, the ratio of glucose to reducing sugar is used, that is The DX/DE ratio can determine the saccharification process and the saccharification end point. In the current domestic stable production process, the glucose content DX of the saccharification liquid is greater than 95.5%, the glucose value DE is generally greater than 98%, and the DX/DE ratio is greater than 97.5%.
现有的测定方法操作复杂，工作效率低，限制了制糖工业的发展。 The existing determination method is complex in operation and low in efficiency, which limits the development of the sugar industry.
发明内容 Contents of the invention
本发明实施例的目的在于提供一种淀粉糖化终点的在线检测方法及自动控制系统，旨在解决现有的测定方法操作复杂，工作效率低，限制了制糖工业的发展的问题。 The purpose of the embodiments of the present invention is to provide an on-line detection method and automatic control system for the end point of starch saccharification, aiming at solving the problems that the existing measurement methods are complicated in operation, low in work efficiency, and limit the development of the sugar industry.
本发明实施例是这样实现的，一种淀粉糖化终点的在线检测方法，该淀粉糖化终点的在线检测方法包括以下步骤： The embodiment of the present invention is achieved in this way, an online detection method for the end point of starch saccharification, the online detection method for the end point of starch saccharification comprises the following steps:
步骤一，测定糖化液的葡萄糖以及还原糖含量； Step 1, measuring the glucose and reducing sugar content of the saccharification solution;
步骤二，通过公式E＝CG/CR计算，当E达到0.98-0.99区间，则可判定到达糖化终点，E表述糖化终点，CG表示葡萄糖含量，CR表示还原糖含量。 Step 2, calculated by the formula E=C G /C R , when E reaches the range of 0.98-0.99, it can be judged that the end point of saccharification has been reached, E represents the end point of saccharification, C G represents the content of glucose, and C R represents the content of reducing sugar.
进一步，在步骤一中，葡萄糖测定采用SBA-40C生物传感分析仪和0.1％葡萄糖标准液，磷酸缓冲液。 Further, in the first step, the glucose is measured using a SBA-40C biosensor analyzer, 0.1% glucose standard solution, and phosphate buffer solution.
进一步，葡萄糖测定方法为：从糖化罐中提取糖化液，稀释后待测，用微量进样器取稀释后样品，注入仪器反应池，仪器自动完成反应过程，并显示测定值，测定值乘以稀释倍数就是样品中葡萄糖的含量。 Further, the method of glucose determination is: extract the saccharification liquid from the saccharification tank, dilute it to be tested, take the diluted sample with a micro-sampler, inject it into the reaction pool of the instrument, and the instrument will automatically complete the reaction process and display the measured value. The measured value is multiplied by The dilution factor is the amount of glucose in the sample.
进一步，在步骤一中，还原糖快速测定采用SGD-IV全自动还原糖测定仪和1.0％葡萄糖溶液，1.0％次甲基蓝溶液，费林甲液，费林乙液。 Further, in step 1, the rapid determination of reducing sugars is carried out using an SGD-IV automatic reducing sugar analyzer, 1.0% glucose solution, 1.0% methylene blue solution, Fehling A solution, and Fehling B solution.
进一步，还原糖快速测定的方法为：从糖化罐中提取糖化液，稀释后待测， 用微量进样器取稀释后样品，注入仪器反应池，仪器自动完成反应过程，并显示测定值，测定值乘以稀释倍数就是样品中葡萄糖的含量。 Further, the method for rapid determination of reducing sugar is: extract the saccharification liquid from the saccharification tank, dilute it for testing, take the diluted sample with a micro-sampler, inject it into the reaction pool of the instrument, and the instrument will automatically complete the reaction process and display the measured value. The value multiplied by the dilution factor is the amount of glucose in the sample.
进一步，在步骤二中，取糖化液进行测定，以糖化时间为X轴，葡萄糖及还原糖含量为Y轴制图，根据葡萄糖和还原糖浓度变化，通过计算葡萄糖/还原糖比值，确定糖化终点。 Further, in step 2, the saccharification liquid is taken for measurement, and the saccharification time is taken as the X-axis, and the glucose and reducing sugar content is used as the Y-axis to draw a graph, and the saccharification end point is determined by calculating the ratio of glucose/reducing sugar according to the concentration changes of glucose and reducing sugar.
本发明实施例的另一目的在于提供一种淀粉糖化终点的在线检测自动控制系统，该淀粉糖化终点的在线检测自动控制系统包括：主控处理器、全自动还原糖测定仪、生物传感分析仪、糖化条件执行单元； Another object of the embodiments of the present invention is to provide an automatic control system for on-line detection of the end point of starch saccharification. instrument, saccharification condition execution unit;
主控处理器，用于控制全自动还原糖测定仪和生物传感分析仪在线检测糖化液中的还原糖和葡萄糖的含量； The main control processor is used to control the automatic reducing sugar analyzer and the biosensor analyzer to detect the content of reducing sugar and glucose in the saccharification liquid online;
全自动还原糖测定仪，与主控处理器连接，用于检测糖化液中的还原糖的含量； A fully automatic reducing sugar tester, connected to the main control processor, used to detect the content of reducing sugar in the saccharification solution;
生物传感分析仪，与主控处理器连接，用于测糖化液中的葡萄糖含量； A biosensing analyzer connected to the main control processor for measuring the glucose content in the saccharification solution;
糖化条件执行单元，与主控处理器连接，用于确定糖化的终点。 The saccharification condition execution unit is connected with the main control processor and used for determining the end point of saccharification.
进一步，主控处理器利用控制器内置软件算法进行提前预算出糖化状态，当糖化终点到来时，控制糖化执行装置。 Further, the main control processor uses the built-in software algorithm of the controller to predict the saccharification state in advance, and controls the saccharification execution device when the saccharification end point arrives.
本发明提供的淀粉糖化终点的在线检测方法及自动控制系统，通过测定糖化液中葡萄糖、还原糖的含量，计算葡萄糖和还原糖比值，确定糖化终点，计算方法如下：DX/DE＝葡萄糖/还原糖在常规糖化工艺中，当DX/DE比值大于97.5％，即可确定为糖化终点，在不同的糖化工艺中，可根据实际生产工艺控制特点，选定DX/DE控制范围；本发明固定化酶葡萄糖生物传感分析仪和还原糖测定仪可进行葡萄糖和还原糖的测定，实现了糖化过程的自动化、无人化和智能化。节约了人力物力，提高了产品的可靠性和质量，增强了企业的市场竞争力。此外，本发明方法简单，快速、准确，而且不需测定干物质含量，具备了在实际生产中的可行性和实用性，较好的解决了现有的测定方法操作复杂，工作效率低，限制了制糖工业的发展的问题。 The online detection method and automatic control system for the starch saccharification end point provided by the present invention, by measuring the content of glucose and reducing sugar in the saccharification liquid, calculating the ratio of glucose and reducing sugar, and determining the saccharification end point, the calculation method is as follows: DX/DE=glucose/reduction In the conventional saccharification process, when the DX/DE ratio is greater than 97.5%, it can be determined as the saccharification end point. In different saccharification processes, the control range of DX/DE can be selected according to the actual production process control characteristics; the immobilization of the present invention The enzyme glucose biosensing analyzer and reducing sugar analyzer can measure glucose and reducing sugar, realizing the automation, unmanned and intelligent saccharification process. It saves manpower and material resources, improves the reliability and quality of products, and enhances the market competitiveness of enterprises. In addition, the method of the present invention is simple, fast and accurate, and does not need to measure the dry matter content, which has feasibility and practicability in actual production, and better solves the complicated operation, low work efficiency and limitations of the existing measuring methods. The problem of the development of the sugar industry.
附图说明 Description of drawings
图1是本发明实施例提供的淀粉糖化终点的在线检测方法的流程图； Fig. 1 is the flow chart of the online detection method of the starch saccharification end point provided by the embodiment of the present invention;
图2是本发明实施例提供的淀粉糖化终点的在线检测自动控制系统的结构示意图； Fig. 2 is a schematic structural view of the on-line detection automatic control system of the starch saccharification end point provided by the embodiment of the present invention;
图中：1、主控处理器；2、全自动还原糖测定仪；3、生物传感分析仪；4、糖化条件执行单元； In the figure: 1. Main control processor; 2. Automatic reducing sugar analyzer; 3. Biosensing analyzer; 4. Saccharification condition execution unit;
图3是本发明实施例提供的糖化过程还原糖及葡萄糖含量检测曲线图。 Fig. 3 is a curve diagram of detection of reducing sugar and glucose content in the saccharification process provided by the embodiment of the present invention.
具体实施方式 detailed description
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。 In order to make the object, technical solution and advantages of the present invention more clear, the present invention will be further described in detail below in conjunction with the examples. It should be understood that the specific embodiments described here are only used to explain the present invention, not to limit the present invention.
下面结合附图及具体实施例对本发明的应用原理作进一步描述。 The application principle of the present invention will be further described below in conjunction with the accompanying drawings and specific embodiments.
如图1所示，本发明实施例的淀粉糖化终点的在线检测方法包括以下步骤： As shown in Figure 1, the online detection method of the starch saccharification end point of the embodiment of the present invention comprises the following steps:
S101：快速测定糖化液的葡萄糖以及还原糖含量； S101: rapid determination of glucose and reducing sugar content in the saccharification solution;
S102：通过公式E＝CG/CR计算，当E达到0.98-0.99区间，则可判定到达糖化终点； S102: Calculated by the formula E=C G /C R , when E reaches the range of 0.98-0.99, it can be determined that the saccharification end point has been reached;
在步骤S102中，CG表示葡萄糖含量，CR表示还原糖含量。 In step S102, C G represents the glucose content, and C R represents the reducing sugar content.
本发明的具体实施例： Specific embodiments of the present invention:
第一步，葡萄糖测定 First step, glucose determination
仪器：SBA-40C生物传感分析仪； Instrument: SBA-40C biosensing analyzer;
试剂：0.1％葡萄糖标准液，磷酸缓冲液。 Reagents: 0.1% glucose standard solution, phosphate buffer.
样品：从糖化罐中提取糖化液，稀释后待测。 Sample: extract the saccharification liquid from the saccharification tank, and dilute it for testing.
测定：用微量进样器取稀释后样品，注入仪器反应池，仪器自动完成反应过程，并显示测定值。测定值乘以稀释倍数就是样品中葡萄糖的含量； Determination: Use a micro-sampler to take the diluted sample, inject it into the reaction pool of the instrument, and the instrument will automatically complete the reaction process and display the measured value. The measured value multiplied by the dilution factor is the content of glucose in the sample;
第二步，还原糖快速测定： The second step, rapid determination of reducing sugar:
仪器：SGD-IV全自动还原糖测定仪； Instrument: SGD-IV automatic reducing sugar tester;
试剂：1.0％葡萄糖溶液，1.0％次甲基蓝溶液，费林甲液，费林乙液； Reagents: 1.0% glucose solution, 1.0% methylene blue solution, Fehling solution A, Fehling solution B;
样品：从糖化罐中提取糖化液，稀释后待测； Sample: extract the saccharification liquid from the saccharification tank, and dilute it to be tested;
测定：用微量进样器取稀释后样品，注入仪器反应池，仪器自动完成反应过程，并显示测定值。测定值乘以稀释倍数就是样品中葡萄糖的含量； Determination: Use a micro-sampler to take the diluted sample, inject it into the reaction pool of the instrument, and the instrument will automatically complete the reaction process and display the measured value. The measured value multiplied by the dilution factor is the content of glucose in the sample;
第三步，每隔一定时间取糖化液进行测定，以糖化时间为X轴，葡萄糖及还原糖含量为Y轴制图；在整个糖化过程中，还原糖及葡萄糖含量随糖化时间变化曲线示意图如附图3所示，其中曲线1为糖化过程中还原糖含量测定值，曲线2为糖化过程中葡萄糖含量测定值，3为糖化终点位置； The third step is to take the saccharification solution at regular intervals for measurement, and use the saccharification time as the X-axis, and the glucose and reducing sugar content as the Y-axis to draw a graph; during the entire saccharification process, the schematic diagram of the curve of reducing sugar and glucose content with saccharification time is shown in the attached As shown in Figure 3, curve 1 is the measured value of reducing sugar content during saccharification, curve 2 is the measured value of glucose content during saccharification, and curve 3 is the end point of saccharification;
第四步，根据葡萄糖和还原糖浓度变化，通过计算葡萄糖/还原糖比值，确定糖化终点。 The fourth step is to determine the end point of saccharification by calculating the ratio of glucose/reducing sugar according to the concentration changes of glucose and reducing sugar.
如图2所示，本发明实施例的淀粉糖化终点的在线检测自动控制系统主要由主控处理器1、全自动还原糖测定仪2、生物传感分析仪3、糖化条件执行单元4组成； As shown in Figure 2, the online detection automatic control system of the starch saccharification end point in the embodiment of the present invention is mainly composed of a main control processor 1, a fully automatic reducing sugar analyzer 2, a biosensing analyzer 3, and a saccharification condition execution unit 4;
主控处理器1，用于控制全自动还原糖测定仪2和生物传感分析仪3在线检测糖化液中的还原糖和葡萄糖的含量； The main control processor 1 is used to control the automatic reducing sugar analyzer 2 and the biosensing analyzer 3 to detect the content of reducing sugar and glucose in the saccharification liquid on-line;
全自动还原糖测定仪2，与主控处理器1连接，用于检测糖化液中的还原糖的含量； A fully automatic reducing sugar analyzer 2, connected to the main control processor 1, for detecting the content of reducing sugar in the saccharification solution;
生物传感分析仪3，与主控处理器1连接，用于测糖化液中的葡萄糖含量； A biosensor analyzer 3 is connected to the main control processor 1 for measuring the glucose content in the saccharification solution;
糖化条件执行单元4，与主控处理器1连接，用于确定糖化的终点； The saccharification condition execution unit 4 is connected to the main control processor 1 and is used to determine the end point of saccharification;
全自动还原糖测定仪2和生物传感分析仪3把检测结果实时上传至主控处理器1，主控处理器1利用控制器内置软件算法进行提前预算出糖化状态，当糖化终点到来时，控制糖化执行装置，停止糖化条件以达到满足产品要求的前提下节能减排的效果； The automatic reducing sugar analyzer 2 and the biosensor analyzer 3 upload the test results to the main control processor 1 in real time. The main control processor 1 uses the built-in software algorithm of the controller to estimate the saccharification state in advance. When the saccharification end point arrives, Control the saccharification executive device and stop the saccharification conditions to achieve the effect of energy saving and emission reduction under the premise of meeting product requirements;
主控处理器1可以控制全自动还原糖测定仪2和生物传感分析仪3的各种 参数，控制器运行状态，在线采集到葡萄糖、还原糖的浓度，并实时在线显示在人际交互界面上，统计分析，趋势图，打印报表等功能； The main control processor 1 can control various parameters of the fully automatic reducing sugar analyzer 2 and the biosensing analyzer 3, and the running status of the controller can collect the concentration of glucose and reducing sugar online, and display it on the human interaction interface online in real time , Statistical analysis, trend chart, print report and other functions;
主控处理器1：LPC1788是恩智浦推出集成LCD图像控制器的ARM Cortex-M3微控制器，是NXP半导体针对各种高级通讯，高质量图像显示等应用场合而设计的一款具有高集成度，以Cortex-M3为内核的微控制器，该微控制器包含有LCD控制器，10/100的以太网EMAC，USB全速Device/Host/OTG控制器，CAN总线控制器，SPI，SSP，IIC，IIS以及外部存储控制器EMC等资源，特适用于工业控制和医疗系统的应用场合。 Main control processor 1: LPC1788 is an ARM Cortex-M3 microcontroller with an integrated LCD image controller launched by NXP. It is a high-integration design designed by NXP Semiconductors for various advanced communications, high-quality image display and other applications , a microcontroller with Cortex-M3 as the core, the microcontroller includes LCD controller, 10/100 Ethernet EMAC, USB full-speed Device/Host/OTG controller, CAN bus controller, SPI, SSP, IIC , IIS and external storage controller EMC and other resources, especially suitable for industrial control and medical system applications.
本发明形成了自动在线检测与反馈控制闭环系统，实现了糖化过程的自动化、无人化和智能化。节约了人力物力，提高了产品的可靠性和质量，增强了企业的市场竞争力。 The invention forms a closed-loop system of automatic online detection and feedback control, and realizes the automation, unmanned and intelligentization of the saccharification process. It saves manpower and material resources, improves the reliability and quality of products, and enhances the market competitiveness of enterprises.
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。 The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements and improvements made within the spirit and principles of the present invention should be included in the protection of the present invention. within range.
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