CN118090690A - Detection method of amylose in grains - Google Patents
Detection method of amylose in grains Download PDFInfo
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- 229920000856 Amylose Polymers 0.000 title claims abstract description 55
- 238000001514 detection method Methods 0.000 title abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000007864 aqueous solution Substances 0.000 claims abstract description 14
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 12
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 90
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 claims description 48
- 239000002244 precipitate Substances 0.000 claims description 34
- 239000011259 mixed solution Substances 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 229920002472 Starch Polymers 0.000 claims description 13
- 235000019698 starch Nutrition 0.000 claims description 13
- 239000008107 starch Substances 0.000 claims description 13
- 239000012043 crude product Substances 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 12
- 238000000605 extraction Methods 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- 230000005284 excitation Effects 0.000 claims description 4
- SNMVRZFUUCLYTO-UHFFFAOYSA-N n-propyl chloride Chemical compound CCCCl SNMVRZFUUCLYTO-UHFFFAOYSA-N 0.000 claims description 4
- 229910016644 EuCl3 Inorganic materials 0.000 claims description 3
- KTUQUZJOVNIKNZ-UHFFFAOYSA-N butan-1-ol;hydrate Chemical compound O.CCCCO KTUQUZJOVNIKNZ-UHFFFAOYSA-N 0.000 claims description 3
- NNMXSTWQJRPBJZ-UHFFFAOYSA-K europium(iii) chloride Chemical compound Cl[Eu](Cl)Cl NNMXSTWQJRPBJZ-UHFFFAOYSA-K 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims 3
- 238000001816 cooling Methods 0.000 claims 2
- 229910004664 Cerium(III) chloride Inorganic materials 0.000 claims 1
- 229910017544 NdCl3 Inorganic materials 0.000 claims 1
- 229910019328 PrCl3 Inorganic materials 0.000 claims 1
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- ATINCSYRHURBSP-UHFFFAOYSA-K neodymium(iii) chloride Chemical compound Cl[Nd](Cl)Cl ATINCSYRHURBSP-UHFFFAOYSA-K 0.000 claims 1
- LHBNLZDGIPPZLL-UHFFFAOYSA-K praseodymium(iii) chloride Chemical compound Cl[Pr](Cl)Cl LHBNLZDGIPPZLL-UHFFFAOYSA-K 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 235000013305 food Nutrition 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 150000002910 rare earth metals Chemical class 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 description 10
- 238000000746 purification Methods 0.000 description 10
- 235000013339 cereals Nutrition 0.000 description 7
- 241000209094 Oryza Species 0.000 description 4
- 235000007164 Oryza sativa Nutrition 0.000 description 4
- 235000009566 rice Nutrition 0.000 description 4
- 241000209140 Triticum Species 0.000 description 2
- 235000021307 Triticum Nutrition 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229920000945 Amylopectin Polymers 0.000 description 1
- 229920002261 Corn starch Polymers 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 239000008120 corn starch Substances 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- 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
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Abstract
Description
技术领域Technical Field
本发明属于食品检测领域,具体涉及一种谷物中直链淀粉的检测方法。The invention belongs to the field of food detection, and in particular relates to a method for detecting amylose in cereals.
背景技术Background technique
淀粉是一种混合物,是由不同类型的淀粉组成,一种是直链淀粉,另一种是支链淀粉。Starch is a mixture that is made up of different types of starch, one is amylose and the other is amylopectin.
其中直链淀粉是小麦、玉米、大米等农作物的主要营养成分,对食品的品质和口感有很大的影响。具有高直链淀粉含量的大米在蒸煮过程中会吸收较多的水分,导致饭粒蓬松色暗。小麦直链淀粉的含量直接影响最终面粉的软度、粘性、光滑性。同时玉米淀粉是直链淀粉的主要来源之一。Among them, amylose is the main nutrient component of crops such as wheat, corn, and rice, and has a great impact on the quality and taste of food. Rice with a high amylose content will absorb more water during the cooking process, resulting in fluffy and dark rice grains. The content of wheat amylose directly affects the softness, viscosity, and smoothness of the final flour. At the same time, corn starch is one of the main sources of amylose.
由于直链淀粉对食品的品质影响大,对直链淀粉含量的检测具有重要的理论价值和实际意义。Since amylose has a great influence on the quality of food, the detection of amylose content has important theoretical value and practical significance.
发明内容Summary of the invention
本发明目的在于提供一种谷物中直链淀粉的检测方法。The present invention aims to provide a method for detecting amylose in cereals.
本发明通过下述技术方案实现:The present invention is achieved through the following technical solutions:
一种谷物中直链淀粉的检测方法,包括以下步骤:A method for detecting amylose in cereals comprises the following steps:
粗产物的提取:待测样品,经粉碎后,加入到稀土元素水溶液中,将溶液加热至60℃,在60℃下保持90min;然后加入100mL正丁醇和异戊醇的混合溶液;然后加热至100℃,并搅拌10min;降温至4℃,并在4℃下维持24h;最后在室温下离心20min中,得到直链淀粉粗产物;Extraction of crude product: The sample to be tested is crushed and added to a rare earth element aqueous solution, the solution is heated to 60°C and maintained at 60°C for 90 minutes; then 100 mL of a mixed solution of n-butanol and isoamyl alcohol is added; then heated to 100°C and stirred for 10 minutes; cooled to 4°C and maintained at 4°C for 24 hours; finally centrifuged at room temperature for 20 minutes to obtain a crude amylose product;
纯化:取100mL正丁醇水混合溶液加入到直链淀粉粗产物中,其中;将溶液加热到100℃直到淀粉完全溶解,然后冷却至25℃,然后置于4℃环境中存放24h,离心得到沉淀,沉淀重复处理3~4次;然后将沉淀物浸于无水乙醇中24h,用无水乙醇洗涤沉淀后,真空干燥得到直链淀粉;Purification: 100 mL of a mixed solution of n-butanol and water is added to the crude amylose product, wherein; the solution is heated to 100°C until the starch is completely dissolved, then cooled to 25°C, and then stored in a 4°C environment for 24 hours, centrifuged to obtain a precipitate, and the precipitation treatment is repeated 3 to 4 times; then the precipitate is immersed in anhydrous ethanol for 24 hours, the precipitate is washed with anhydrous ethanol, and vacuum dried to obtain amylose;
再使用荧光分光光度计对直链淀粉含量进行检测。The amylose content was then detected using a fluorescence spectrophotometer.
进一步地,所述丁醇和异戊醇混合溶液中丁醇和异戊醇的体积比为1:3。Furthermore, the volume ratio of butanol to isoamyl alcohol in the mixed solution of butanol and isoamyl alcohol is 1:3.
进一步地,所述正丁醇水混合溶液中正丁醇和水的体积比为1:9。Furthermore, the volume ratio of n-butanol to water in the n-butanol-water mixed solution is 1:9.
进一步地,所述稀土元素水溶液中稀土元素选自PrCl3、CeCl3、PrCl3、NdCl3、EuCl3中的一种。Furthermore, the rare earth element in the rare earth element aqueous solution is selected from one of PrCl 3, CeCl 3, PrCl 3, NdCl 3, and EuCl 3 .
进一步地,所述稀土元素水溶液中稀土元素选自EuCl3。Furthermore, the rare earth element in the rare earth element aqueous solution is selected from EuCl3.
进一步地,EuCl3溶液的浓度为0.5M~1.0M。Further, the concentration of the EuCl 3 solution is 0.5M~1.0M.
进一步地,EuCl3溶液的浓度为0.5M。Further, the concentration of EuCl 3 solution is 0.5M.
进一步地,EuCl3溶液的体积为70~150mL。Furthermore, the volume of the EuCl 3 solution is 70 to 150 mL.
进一步地,EuCl3溶液的体积为100mL。Further, the volume of EuCl 3 solution is 100 mL.
进一步地,在使用荧光分光光度计对直链淀粉含量进行检测时,在300~500nm波长范围内扫描确定最大激发波长和发射波长。Furthermore, when the amylose content is detected using a fluorescence spectrophotometer, the maximum excitation wavelength and emission wavelength are determined by scanning in the wavelength range of 300-500 nm.
本发明与现有技术相比,具有如下的优点和有益效果:见实施例。Compared with the prior art, the present invention has the following advantages and beneficial effects: see the embodiments.
具体实施方式Detailed ways
为使本发明的目的、技术方案和优点更加清楚明白,下面结合实施例,对本发明作进一步的详细说明,本发明的示意性实施方式及其说明仅用于解释本发明,并不作为对本发明的限定。In order to make the purpose, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with embodiments. The illustrative embodiments of the present invention and their description are only used to explain the present invention and are not intended to limit the present invention.
实施例1Example 1
粗产物的提取:取10g待测样品,经粉碎后,加入到100mL 0.5M CeCl3水溶液中,将溶液加热至60℃,在60℃下保持90min;然后加入100mL正丁醇和异戊醇的混合溶液,其中丁醇和异戊醇的体积比为1:3;然后加热至100℃,并搅拌10min;降温至4℃,并在4℃下维持24h;最后在室温下离心20min,得到直链淀粉粗产物;Extraction of crude product: Take 10g of the sample to be tested, crush it, add it to 100mL of 0.5M CeCl 3 aqueous solution, heat the solution to 60℃, and keep it at 60℃ for 90min; then add 100mL of a mixed solution of n-butanol and isoamyl alcohol, where the volume ratio of butanol to isoamyl alcohol is 1:3; then heat to 100℃ and stir for 10min; cool to 4℃ and keep it at 4℃ for 24h; finally centrifuge at room temperature for 20min to obtain crude amylose;
纯化:取100mL正丁醇水混合溶液加入到直链淀粉粗产物中,其中正丁醇和水的体积比为1:9;将溶液加热到100℃直到淀粉完全溶解,然后冷却至25℃,然后置于4℃环境中存放24h,离心得到沉淀,沉淀重复处理3~4次;然后将沉淀物浸于无水乙醇中24h,用无水乙醇洗涤沉淀后,真空干燥得到直链淀粉。Purification: Take 100 mL of a mixed solution of n-butanol and water and add it to the crude amylose product, wherein the volume ratio of n-butanol to water is 1:9; heat the solution to 100°C until the starch is completely dissolved, then cool it to 25°C, and then store it in a 4°C environment for 24 hours, centrifuge it to obtain a precipitate, and repeat the precipitation process 3 to 4 times; then immerse the precipitate in anhydrous ethanol for 24 hours, wash the precipitate with anhydrous ethanol, and vacuum dry it to obtain amylose.
实施例2Example 2
粗产物的提取:取10g待测样品,经粉碎后,加入到100mL 0.5M PrCl3水溶液中,将溶液加热至60℃,在60℃下保持90min;然后加入100mL正丁醇和异戊醇的混合溶液,其中丁醇和异戊醇的体积比为1:3;然后加热至100℃,并搅拌10min;降温至4℃,并在4℃下维持24h;最后在室温下离心20min,得到直链淀粉粗产物;Extraction of crude product: Take 10g of the sample to be tested, crush it, add it to 100mL of 0.5M PrCl 3 aqueous solution, heat the solution to 60℃, and keep it at 60℃ for 90min; then add 100mL of a mixed solution of n-butanol and isoamyl alcohol, where the volume ratio of butanol to isoamyl alcohol is 1:3; then heat to 100℃ and stir for 10min; cool to 4℃ and keep it at 4℃ for 24h; finally centrifuge at room temperature for 20min to obtain crude amylose;
纯化:取100mL正丁醇水混合溶液加入到直链淀粉粗产物中,其中正丁醇和水的体积比为1:9;将溶液加热到100℃直到淀粉完全溶解,然后冷却至25℃,然后置于4℃环境中存放24h,离心得到沉淀,沉淀重复处理3~4次;然后将沉淀物浸于无水乙醇中24h,用无水乙醇洗涤沉淀后,真空干燥得到直链淀粉。Purification: Take 100 mL of a mixed solution of n-butanol and water and add it to the crude amylose product, wherein the volume ratio of n-butanol to water is 1:9; heat the solution to 100°C until the starch is completely dissolved, then cool it to 25°C, and then store it in a 4°C environment for 24 hours, centrifuge it to obtain a precipitate, and repeat the precipitation process 3 to 4 times; then immerse the precipitate in anhydrous ethanol for 24 hours, wash the precipitate with anhydrous ethanol, and vacuum dry it to obtain amylose.
实施例3Example 3
粗产物的提取:取10g待测样品,经粉碎后,加入到100mL 0.5M NdCl3水溶液中,将溶液加热至60℃,在60℃下保持90min;然后加入100mL正丁醇和异戊醇的混合溶液,其中丁醇和异戊醇的体积比为1:3;然后加热至100℃,并搅拌10min;降温至4℃,并在4℃下维持24h;最后在室温下离心20min,得到直链淀粉粗产物;Extraction of crude product: Take 10g of the sample to be tested, crush it, add it to 100mL of 0.5M NdCl 3 aqueous solution, heat the solution to 60℃, and keep it at 60℃ for 90min; then add 100mL of a mixed solution of n-butanol and isoamyl alcohol, where the volume ratio of butanol to isoamyl alcohol is 1:3; then heat to 100℃ and stir for 10min; cool to 4℃ and keep it at 4℃ for 24h; finally centrifuge at room temperature for 20min to obtain crude amylose;
纯化:取100mL正丁醇水混合溶液加入到直链淀粉粗产物中,其中正丁醇和水的体积比为1:9;将溶液加热到100℃直到淀粉完全溶解,然后冷却至25℃,然后置于4℃环境中存放24h,离心得到沉淀,沉淀重复处理3~4次;然后将沉淀物浸于无水乙醇中24h,用无水乙醇洗涤沉淀后,真空干燥得到直链淀粉。Purification: Take 100 mL of a mixed solution of n-butanol and water and add it to the crude amylose product, wherein the volume ratio of n-butanol to water is 1:9; heat the solution to 100°C until the starch is completely dissolved, then cool it to 25°C, and then store it in a 4°C environment for 24 hours, centrifuge it to obtain a precipitate, and repeat the precipitation process 3 to 4 times; then immerse the precipitate in anhydrous ethanol for 24 hours, wash the precipitate with anhydrous ethanol, and vacuum dry it to obtain amylose.
实施例4Example 4
粗产物的提取:取10g待测样品,经粉碎后,加入到100mL 0.5M EuCl3水溶液中,将溶液加热至60℃,在60℃下保持90min;然后加入100mL正丁醇和异戊醇的混合溶液,其中丁醇和异戊醇的体积比为1:3;然后加热至100℃,并搅拌10min;降温至4℃,并在4℃下维持24h;最后在室温下离心20min,得到直链淀粉粗产物;Extraction of crude product: Take 10g of the sample to be tested, crush it, add it to 100mL of 0.5M EuCl 3 aqueous solution, heat the solution to 60℃, and keep it at 60℃ for 90min; then add 100mL of a mixed solution of n-butanol and isoamyl alcohol, where the volume ratio of butanol to isoamyl alcohol is 1:3; then heat to 100℃ and stir for 10min; cool to 4℃ and keep it at 4℃ for 24h; finally centrifuge at room temperature for 20min to obtain crude amylose;
纯化:取100mL正丁醇水混合溶液加入到直链淀粉粗产物中,其中正丁醇和水的体积比为1:9;将溶液加热到100℃直到淀粉完全溶解,然后冷却至25℃,然后置于4℃环境中存放24h,离心得到沉淀,沉淀重复处理3~4次;然后将沉淀物浸于无水乙醇中24h,用无水乙醇洗涤沉淀后,真空干燥得到直链淀粉。Purification: Take 100 mL of a mixed solution of n-butanol and water and add it to the crude amylose product, wherein the volume ratio of n-butanol to water is 1:9; heat the solution to 100°C until the starch is completely dissolved, then cool it to 25°C, and then store it in a 4°C environment for 24 hours, centrifuge it to obtain a precipitate, and repeat the precipitation process 3 to 4 times; then immerse the precipitate in anhydrous ethanol for 24 hours, wash the precipitate with anhydrous ethanol, and vacuum dry it to obtain amylose.
实施例5Example 5
粗产物的提取:取10g待测样品,经粉碎后,加入到100mL 0.5M LaCl3水溶液中,将溶液加热至60℃,在60℃下保持90min;然后加入100mL正丁醇和异戊醇的混合溶液,其中丁醇和异戊醇的体积比为1:3;然后加热至100℃,并搅拌10min;降温至4℃,并在4℃下维持24h;最后在室温下离心20min,得到直链淀粉粗产物;Extraction of crude product: Take 10g of the sample to be tested, crush it, add it to 100mL of 0.5M LaCl 3 aqueous solution, heat the solution to 60℃, and keep it at 60℃ for 90min; then add 100mL of a mixed solution of n-butanol and isoamyl alcohol, where the volume ratio of butanol to isoamyl alcohol is 1:3; then heat to 100℃ and stir for 10min; cool to 4℃ and keep it at 4℃ for 24h; finally centrifuge at room temperature for 20min to obtain crude amylose;
纯化:取100mL正丁醇水混合溶液加入到直链淀粉粗产物中,其中正丁醇和水的体积比为1:9;将溶液加热到100℃直到淀粉完全溶解,然后冷却至25℃,然后置于4℃环境中存放24h,离心得到沉淀,沉淀重复处理3~4次;然后将沉淀物浸于无水乙醇中24h,用无水乙醇洗涤沉淀后,真空干燥得到直链淀粉。Purification: Take 100 mL of a mixed solution of n-butanol and water and add it to the crude amylose product, wherein the volume ratio of n-butanol to water is 1:9; heat the solution to 100°C until the starch is completely dissolved, then cool it to 25°C, and then store it in a 4°C environment for 24 hours, centrifuge it to obtain a precipitate, and repeat the precipitation process 3 to 4 times; then immerse the precipitate in anhydrous ethanol for 24 hours, wash the precipitate with anhydrous ethanol, and vacuum dry it to obtain amylose.
实施例6Example 6
粗产物的提取:取10g待测样品,经粉碎后,加入到70mL 0.5M EuCl3水溶液中,将溶液加热至60℃,在60℃下保持90min;然后加入100mL正丁醇和异戊醇的混合溶液,其中丁醇和异戊醇的体积比为1:3;然后加热至100℃,并搅拌10min;降温至4℃,并在4℃下维持24h;最后在室温下离心20min,得到直链淀粉粗产物;Extraction of crude product: Take 10g of the sample to be tested, crush it, add it to 70mL of 0.5M EuCl 3 aqueous solution, heat the solution to 60℃, and keep it at 60℃ for 90min; then add 100mL of a mixed solution of n-butanol and isoamyl alcohol, where the volume ratio of butanol to isoamyl alcohol is 1:3; then heat to 100℃ and stir for 10min; cool to 4℃ and keep it at 4℃ for 24h; finally centrifuge at room temperature for 20min to obtain crude amylose;
纯化:取100mL正丁醇水混合溶液加入到直链淀粉粗产物中,其中正丁醇和水的体积比为1:9;将溶液加热到100℃直到淀粉完全溶解,然后冷却至25℃,然后置于4℃环境中存放24h,离心得到沉淀,沉淀重复处理3~4次;然后将沉淀物浸于无水乙醇中24h,用无水乙醇洗涤沉淀后,真空干燥得到直链淀粉。Purification: Take 100 mL of a mixed solution of n-butanol and water and add it to the crude amylose product, wherein the volume ratio of n-butanol to water is 1:9; heat the solution to 100°C until the starch is completely dissolved, then cool it to 25°C, and then store it in a 4°C environment for 24 hours, centrifuge it to obtain a precipitate, and repeat the precipitation process 3 to 4 times; then immerse the precipitate in anhydrous ethanol for 24 hours, wash the precipitate with anhydrous ethanol, and vacuum dry it to obtain amylose.
实施例7Example 7
粗产物的提取:取10g待测样品,经粉碎后,加入到80mL 0.5M EuCl3水溶液中,将溶液加热至60℃,在60℃下保持90min;然后加入100mL正丁醇和异戊醇的混合溶液,其中丁醇和异戊醇的体积比为1:3;然后加热至100℃,并搅拌10min;降温至4℃,并在4℃下维持24h;最后在室温下离心20min,得到直链淀粉粗产物;Extraction of crude product: Take 10g of the sample to be tested, crush it, add it to 80mL of 0.5M EuCl 3 aqueous solution, heat the solution to 60℃, and keep it at 60℃ for 90min; then add 100mL of a mixed solution of n-butanol and isoamyl alcohol, where the volume ratio of butanol to isoamyl alcohol is 1:3; then heat to 100℃ and stir for 10min; cool to 4℃ and keep it at 4℃ for 24h; finally centrifuge at room temperature for 20min to obtain crude amylose;
纯化:取100mL正丁醇水混合溶液加入到直链淀粉粗产物中,其中正丁醇和水的体积比为1:9;将溶液加热到100℃直到淀粉完全溶解,然后冷却至25℃,然后置于4℃环境中存放24h,离心得到沉淀,沉淀重复处理3~4次;然后将沉淀物浸于无水乙醇中24h,用无水乙醇洗涤沉淀后,真空干燥得到直链淀粉。Purification: Take 100 mL of a mixed solution of n-butanol and water and add it to the crude amylose product, wherein the volume ratio of n-butanol to water is 1:9; heat the solution to 100°C until the starch is completely dissolved, then cool it to 25°C, and then store it in a 4°C environment for 24 hours, centrifuge it to obtain a precipitate, and repeat the precipitation process 3 to 4 times; then immerse the precipitate in anhydrous ethanol for 24 hours, wash the precipitate with anhydrous ethanol, and vacuum dry it to obtain amylose.
实施例8Example 8
粗产物的提取:取10g待测样品,经粉碎后,加入到120mL 0.5M EuCl3水溶液中,将溶液加热至60℃,在60℃下保持90min;然后加入100mL正丁醇和异戊醇的混合溶液,其中丁醇和异戊醇的体积比为1:3;然后加热至100℃,并搅拌10min;降温至4℃,并在4℃下维持24h;最后在室温下离心20min,得到直链淀粉粗产物;Extraction of crude product: Take 10g of the sample to be tested, crush it, add it to 120mL of 0.5M EuCl 3 aqueous solution, heat the solution to 60℃, and keep it at 60℃ for 90min; then add 100mL of a mixed solution of n-butanol and isoamyl alcohol, where the volume ratio of butanol to isoamyl alcohol is 1:3; then heat to 100℃ and stir for 10min; cool to 4℃ and keep it at 4℃ for 24h; finally centrifuge at room temperature for 20min to obtain crude amylose;
纯化:取100mL正丁醇水混合溶液加入到直链淀粉粗产物中,其中正丁醇和水的体积比为1:9;将溶液加热到100℃直到淀粉完全溶解,然后冷却至25℃,然后置于4℃环境中存放24h,离心得到沉淀,沉淀重复处理3~4次;然后将沉淀物浸于无水乙醇中24h,用无水乙醇洗涤沉淀后,真空干燥得到直链淀粉。Purification: Take 100 mL of a mixed solution of n-butanol and water and add it to the crude amylose product, wherein the volume ratio of n-butanol to water is 1:9; heat the solution to 100°C until the starch is completely dissolved, then cool it to 25°C, and then store it in a 4°C environment for 24 hours, centrifuge it to obtain a precipitate, and repeat the precipitation process 3 to 4 times; then immerse the precipitate in anhydrous ethanol for 24 hours, wash the precipitate with anhydrous ethanol, and vacuum dry it to obtain amylose.
实施例9Example 9
粗产物的提取:取10g待测样品,经粉碎后,加入到150mL 0.5M EuCl3水溶液中,将溶液加热至60℃,在60℃下保持90min;然后加入100mL正丁醇和异戊醇的混合溶液,其中丁醇和异戊醇的体积比为1:3;然后加热至100℃,并搅拌10min;降温至4℃,并在4℃下维持24h;最后在室温下离心20min,得到直链淀粉粗产物;Extraction of crude product: Take 10g of the sample to be tested, crush it, add it to 150mL of 0.5M EuCl 3 aqueous solution, heat the solution to 60℃, and keep it at 60℃ for 90min; then add 100mL of a mixed solution of n-butanol and isoamyl alcohol, where the volume ratio of butanol to isoamyl alcohol is 1:3; then heat to 100℃ and stir for 10min; cool to 4℃ and keep it at 4℃ for 24h; finally centrifuge at room temperature for 20min to obtain crude amylose;
纯化:取100mL正丁醇水混合溶液加入到直链淀粉粗产物中,其中正丁醇和水的体积比为1:9;将溶液加热到100℃直到淀粉完全溶解,然后冷却至25℃,然后置于4℃环境中存放24h,离心得到沉淀,沉淀重复处理3~4次;然后将沉淀物浸于无水乙醇中24h,用无水乙醇洗涤沉淀后,真空干燥得到直链淀粉。Purification: Take 100 mL of a mixed solution of n-butanol and water and add it to the crude amylose product, wherein the volume ratio of n-butanol to water is 1:9; heat the solution to 100°C until the starch is completely dissolved, then cool it to 25°C, and then store it in a 4°C environment for 24 hours, centrifuge it to obtain a precipitate, and repeat the precipitation process 3 to 4 times; then immerse the precipitate in anhydrous ethanol for 24 hours, wash the precipitate with anhydrous ethanol, and vacuum dry it to obtain amylose.
测试例1Test Example 1
将实施例1~9中方法用于对同种大米中的直链淀粉的检测,检测方法为以水作为溶剂,采用荧光分光光度计对直链淀粉含量进行检测,在300~500nm范围内确定最大激发波长和发射波长,标准曲线浓度范围为0.1μg/mL~1.0μg/mL。同时使用NY/T 55-1987的检测值作为标准。每次测量进行两次,取平均值。The methods in Examples 1 to 9 were used to detect the amylose in the same rice. The detection method was to use water as a solvent, use a fluorescence spectrophotometer to detect the amylose content, determine the maximum excitation wavelength and emission wavelength in the range of 300 to 500 nm, and the standard curve concentration range was 0.1 μg/mL to 1.0 μg/mL. At the same time, the detection value of NY/T 55-1987 was used as a standard. Each measurement was performed twice and the average value was taken.
表1性能测试Table 1 Performance test
由表1中数据可以看出,不同稀土元素的提取液都有一定作用,但实施例4中效果最好,与国标NY/T 55-1987所测定的结果最接近。It can be seen from the data in Table 1 that the extracts of different rare earth elements all have certain effects, but the effect in Example 4 is the best, which is closest to the results measured by the national standard NY/T 55-1987.
测试例2Test Example 2
将实施例4的方法用于不同谷物含量的检测,检测方法为以水作为溶剂,采用荧光分光光度计对直链淀粉含量进行检测,在300~500nm范围内确定最大激发波长和发射波长,标准曲线浓度范围为0.1μg/mL~1.0μg/mL。同时使用NY/T 55-1987的检测值作为标准。每次测量进行两次,取平均值。The method of Example 4 was used to detect the contents of different cereals. The detection method was to use water as a solvent, use a fluorescence spectrophotometer to detect the content of amylose, determine the maximum excitation wavelength and emission wavelength in the range of 300-500 nm, and the concentration range of the standard curve was 0.1 μg/mL-1.0 μg/mL. At the same time, the detection value of NY/T 55-1987 was used as a standard. Each measurement was performed twice and the average value was taken.
表2不同谷物中直链淀粉含量测定。Table 2 Determination of amylose content in different cereals.
由表2中数据可以看出,本申请中的检测方法可以用于不同种类谷物的测定。It can be seen from the data in Table 2 that the detection method in this application can be used for the determination of different types of grains.
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.
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