CN102519900A - Method for measuring nonprotein nitrogen content in plants and plant products - Google Patents

Method for measuring nonprotein nitrogen content in plants and plant products Download PDF

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CN102519900A
CN102519900A CN 201110460000 CN201110460000A CN102519900A CN 102519900 A CN102519900 A CN 102519900A CN 201110460000 CN201110460000 CN 201110460000 CN 201110460000 A CN201110460000 A CN 201110460000A CN 102519900 A CN102519900 A CN 102519900A
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digestion
plants
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nitrogen
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孔浩辉
张心颖
程志颖
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广东中烟工业有限责任公司
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Abstract

The invention provides a method for measuring nonprotein nitrogen content in plants and plant products, which includes the following steps: separating protein nitrogen from a plant and a plant product to obtain a to-be-measured sample containing nonprotein nitrogen; adding potassium persulfate into the to-be-measured sample to obtain a mixed solution under the heating condition; performing ultraviolet catalysis and high-temperature heating to the mixed solution sequentially, so as to obtain a digestion product; detecting the digestion product to obtain ultraviolet spectrum data; and obtaining the nonprotein nitrogen content in the plant and the plant product as per the ultraviolet spectrum data and a predetermined standard curve. The method provided by the invention has excellent digestion effect, the digestion of the nonprotein nitrogen ingredient as well as the digestion of the reductive ingredient in the to-be-measured sample can be realized, the reductive function of the to-be-measured sample is lost, the interference in the nonprotein nitrogen ingredient digestion is reduced, so that the digestion effect becomes more uniform, the recovery rate of the nonprotein nitrogen measurement is improved, and the accuracy of the measurement result is improved.

Description

一种植物及植物制品中非蛋白质氮含量的测定方法 A plant and method for measuring nitrogen content in plant products nonprotein

技术领域 FIELD

[0001] 本发明涉及氮的分析测定技术领域,尤其涉及一种植物及植物制品中非蛋白质氮含量的测定方法。 [0001] The present invention relates to the technical field Determination of nitrogen, particularly to a method for measuring nitrogen content of plants and plant products is nonprotein.

背景技术 Background technique

[0002] 氮是植物生长发育不可缺少的营养元素,被称为生命元素,氮素代谢在植物的新陈代谢中占主导地位。 [0002] Nitrogen is the development of essential nutrients for plant growth, known as life element and nitrogen metabolism dominates in the metabolism of plants. 植物中的氮可分为蛋白质氮和非蛋白质氮,蛋白质氮是植物正在利用的氮含量;非蛋白质氮主要包括氨基酸、生物碱、硝酸盐、亚硝酸盐和氨盐等,是一种储藏形式的氮;总氮则代表植物总的氮元素的吸收情况。 Nitrogen in plants of proteins can be divided into non-protein nitrogen and nitrogen, protein nitrogen content of the plant is being utilized by a nitrogen; non-protein nitrogen include amino acids, alkaloids, nitrates, nitrites and ammonium salts and the like, a storage form of nitrogen; TN represents the total absorption of nitrogen plant. 植物中氮的含量随着其生理状况及环境条件的不同而发生变化,所以测定其中不同形式氮的含量对研究植物的氮素吸收、运输和代谢规律,了解植物的生长状况,以及确定植物制品的品质、营养价值等都具有重要的意义;对于植物制品,测定其中非蛋白质氮含量还有助于确定其中蛋白质氮的真实含量,有利于对其品质进行评价。 The nitrogen content in plants with different physiological conditions and environmental conditions change, the measured content of nitrogen in which different forms of nitrogen in plants of the absorption, transport and metabolism of the law, to understand how the plants and plant products determined quality, nutritional value and so is of great significance; for plant products, determination of non-protein nitrogen content which also helps determine where the real content of protein nitrogen, help evaluate its quality.

[0003] 对于氮含量的测定,通常采用的方法是将样品中的含氮化合物消解,得到硝酸盐, 然后将得到的硝酸盐还原为亚硝酸盐,利用亚硝酸盐与磺胺和N-萘基乙二胺盐酸盐显色的性质,采用分光光度法对其进行测定。 [0003] For the determination of nitrogen content, generally employed is a method of nitrogen-containing compounds in the sample digestion, to give the nitrate, nitrate reduction and then the resulting nitrite by nitrite and naphthyl sulfonamide and N- ethylenediamine hydrochloride color development properties, and it was determined by spectrophotometry. 如邹琳等采用流动注射分析仪测定了水中的总氮和总磷的含量(邹琳,周圣东,陈卫.高压消解\流动注射光度法同时测定水中总氮与总磷.中国给水排水,2009,25 (22) :93〜97.),其过程为:在110°C下,将水样经过碱性过硫酸钾和硫酸两次消解,得到的消解产物分别进入流动注射分析仪中的总氮、总磷分析系统, 得到水样中总氮、总磷的含量。 Lin et Zou as to determine the content of total nitrogen and total phosphorus in water (Zou Lin, Zhousheng Dong, Chen Wei flow injection analyzer high pressure digestion \ Determination of total nitrogen and total phosphorus in water by flow injection method. China Water & Wastewater, 2009 , 25 (22): 93~97), the process is: at 110 ° C, the water sample through two alkaline and acid digestion, the digestion products were obtained entering total flow injection analyzer nitrogen, total phosphorus analysis system, to obtain water samples total nitrogen, total phosphorus content. 在总氮分析系统中,消解产物通过一个镀铜的镉圈后,硝酸根被定量还原为亚硝酸根,在酸性条件下,亚硝酸根与磺胺和N-萘基乙二胺盐酸盐在45°C 恒温条件下反应生成紫红色物质,其最佳吸收波长为550nm,采用分光光度法对得到的紫红色物质进行测定,得到水中的总氮含量。 Analysis of total nitrogen in the system, by digestion product was a copper ring cadmium nitrate is quantitatively reduced to nitrite under acidic conditions, nitrite with sulfanilamide and N- naphthyl ethylenediamine hydrochloride purple reaction material at a constant temperature of 45 ° C, the optimal absorption wavelength of 550 nm, using spectrophotometry purple substance obtained was measured to obtain the total nitrogen content in the water.

[0004] 高压消解对非蛋白质氮中的无机氮消解效果较好,但是对于植物碱、氨基酸类的非蛋白质氮,如烟碱、茶碱、亮氨酸等来说,由于其结构较为复杂,采用高压消解时存在消解不完全、不彻底的现象,从而造成对非蛋白质氮测定的回收率低,得到的测量结果不准确。 [0004] better high pressure digestion of non-protein nitrogen inorganic nitrogen digestion, but for a plant alkaloid, a non-protein nitrogen-amino acids, such as nicotine, theophylline, leucine and the like, because of its complex structure, the presence of incomplete digestion, incomplete digestion of the high-pressure phenomena, resulting in low recovery of the non-protein nitrogen determination, the measurements obtained are not accurate. 尤其对于植物及植物制品来说,其大部分非蛋白质氮属于植物碱或氨基酸类,而且植物及植物制品中还含有还原性成分,如糖类,这些还原性成分会与氧化剂反应,从而影响对含氮组分的消解,造成其消解不完全和不彻底,采用上述方法对其中的非蛋白质氮含量进行测定时,得到的消解产物不够完全和彻底,导致测定结果不准确。 Especially for plants and plant products is that most non-protein nitrogen base or amino acids belonging to the plant, and plants and plant products also contain a reducing component, such as sugars, reducing component which will react with the oxidant thereby Effect Digestion nitrogen compounds, which cause incomplete or complete digestion, when non-protein nitrogen content which was measured by the above method, the product obtained is incomplete and complete digestion, leading to inaccurate measurement results.

发明内容 SUMMARY

[0005] 本发明的目的在于提供一种植物及植物制品中非蛋白质氮含量的测定方法,本发明提供的方法对非蛋白质氮的测定具有较高的回收率,得到的植物及植物制品中非蛋白质氮含量的测定结果准确。 [0005] The object of the present invention is to provide a plant and a method for measuring nitrogen content of nonprotein plant products, the present invention provides a method having a higher recovery of non-protein nitrogen was measured, resulting plants and plant products in Central Africa accurate determination of the nitrogen content of the protein results.

[0006] 本发明提供一种植物及植物制品中非蛋白质氮含量的测定方法,包括以下步骤:[0007] a)分离植物及植物制品中的蛋白质氮,得到含有非蛋白质氮的待测试样; [0006] The present invention provides a method for measuring nitrogen content of plants and plant products of nonprotein, comprising the steps of: [0007] a) separation plants and plant products in the N protein, to obtain the sample to be tested containing non-protein nitrogen ;

[0008] b)在加热条件下,向所述待测试样中加入过硫酸钾,得到混合溶液; [0008] b) under heating conditions, to the potassium persulfate was added in the test sample, to give a mixed solution;

[0009] c)将所述混合溶液依次经过紫外催化和高温加热,得到消解产物; [0009] c) the mixed solution sequentially through UV catalysis and heated to high temperature digestion product obtained;

[0010] d)检测所述消解产物,得到紫外光谱数据; [0010] d) detecting the digestion product was UV spectral data;

[0011] e)根据所述紫外光谱数据和预定的标准曲线,得到植物及植物制品中非蛋白质氮含量。 [0011] e) The UV spectra data and the predetermined standard curve to obtain a protein nitrogen content of plants and plant products Africa.

[0012] 优选的,所述紫外催化为在非硫酸酸性环境中进行紫外催化。 [0012] Preferably, the UV catalyst is sulfuric acid in an acidic environment, a non-UV catalysis.

[0013] 优选的,所述紫外催化的温度为90°C〜110°C。 [0013] Preferably, the temperature of the UV-catalyzed 90 ° C~110 ° C.

[0014] 优选的,所述高温加热的温度为95°C〜150°C。 [0014] Preferably, the high-temperature heating temperature of 95 ° C~150 ° C.

[0015] 优选的,所述高温加热为加压高温加热。 [0015] Preferably, the heating temperature of the high temperature pressing.

[0016] 优选的,所述加压高温加热的压力为5Psi〜8Psi。 [0016] Preferably, the pressure of the pressurized high-temperature heating 5Psi~8Psi.

[0017] 优选的,所述步骤b)中的加热温度为90°C〜110°C。 The heating temperature [0017] Preferably, the step b) is 90 ° C~110 ° C.

[0018] 优选的,所述步骤a)具体为: [0018] Preferably, the step a) is specifically:

[0019] 向植物及植物制品中加入蛋白质变性试剂,加热得到的混合物,分离后得到含有非蛋白质氮的待测试样。 [0019] Plants and plant products was added to the protein denaturing reagent, the mixture was heated, to give a test sample to be separated comprises non-protein nitrogen. 优选的,所述蛋白质变性试剂为有机酸。 Preferably, the protein denaturing agent is an organic acid.

[0020] 优选的,所述步骤b)前还包括: [0020] Preferably, said step b) before further comprises:

[0021] 向所述待测试样中加入过氧化氢,除去所述待测试样中的还原性组分; [0021] Hydrogen peroxide was added to the sample to be tested, the test sample is removed in the reducing component;

[0022] 和/或向所述待测试样中加入活性炭,除去所述待测试样中的无机色素; [0022] and / or in the test sample to the activated carbon is added to remove the test sample of the inorganic pigments;

[0023] 和/或向所述待测试样中加入乙二胺四乙酸二钠,除去所述待测试样中的金属离子。 [0023] and / or to the sample to be tested was added disodium edetate, removing the metal ions to be in the test sample.

[0024] 本发明提供的植物及植物制品中非蛋白质氮含量的测定方法,包括以下步骤:分离植物及植物制品中的蛋白质氮,得到含有非蛋白质氮的待测试样;在加热条件下,向所述待测试样中加入过硫酸钾,得到混合溶液;将所述混合溶液依次经过紫外催化和高温加热, 得到消解产物;检测所述消解产物,得到紫外光谱数据;根据所述紫外光谱数据和预定的标准曲线,得到植物及植物制品中非蛋白质氮含量。 [0024] Determination of the nitrogen content of plants and plant products of the present invention provides a nonprotein, comprising the steps of: separating plants and plant products in the N protein, to obtain the sample to be tested containing non-protein nitrogen; under heating conditions, the sample to be tested was added potassium persulfate, to give a mixed solution; the mixed solution sequentially through an ultraviolet catalyst and heated to high temperatures, resulting digestion product; detecting the digestion product was UV spectral data; according to the UV spectra data and a predetermined standard curve to obtain a protein nitrogen content of plants and plant products Africa. 在本发明中,过硫酸钾在加热条件下产生活性氧原子[0],对植物及植物制品进行初步消解;然后在紫外催化条件下,部分活性氧原子[0]与水反应生成自由基,该自由基使样品中的非蛋白质氮组分进一步消解;接着, 高温条件下,活性氧原子[0]对植物及植物制品中的非蛋白质氮的组分进行更进一步的消解,最终使各类非蛋白质氮组分消解完全。 In the present invention, potassium persulfate produced active oxygen atom under heating [0], the plants and plant products preliminary digestion; then ultraviolet catalysis, part of reactive oxygen atoms [0] is reacted with water to generate free radicals, the radical non-protein nitrogen components in the sample is further digestion; next, under high temperature conditions, active oxygen atom [0] non-protein nitrogen component of plants and plant products is still further digestion, and finally to all kinds of non-protein nitrogen components complete digestion. 本发明提供的方法具有良好的消解效果,在将待测试样中的非蛋白质氮组分完全和彻底消解的同时,将其中的还原性组分消解,使其失去还原作用,减少对非蛋白质氮组分消解的干扰,从而提高得到的消解结果的均一性,提高对非蛋白质氮测定的回收率,提高测定结果的准确性。 The method of the present invention provides a good digestion results in the non-protein nitrogen components in the test sample is completely and simultaneously complete digestion, wherein the reducing component digestion, loss reduction, reduction of non-protein nitrogen component digestion interference, thereby improving the uniformity of digestion results obtained, increase the recovery rate of non-protein nitrogen determination to improve the accuracy of measurement results. 另外,本发明提供的测定方法具有良好的稳定性和重复性。 Further, the present invention provides a measurement method having good stability and reproducibility.

[0025] 实验结果表明,本发明提供的方法对植物及植物制品中非蛋白质氮组分之一的烟碱检测的回收率为98. 76 %〜100. 9 %,茶碱的回收率达到100. 8 %,亮氨酸的回收率为99.0% ;采用本发明提供的方法测定了烟草中的非蛋白质氮含量,得到了准确的结果。 [0025] Experimental results show that the present invention provides a method for detecting nicotine recovery of plants and plant products one nonprotein nitrogen components was 98.76% ~ 100 9% recovery of theophylline 100 8% leucine recovery 99.0%; the method of the present invention provides a non-protein nitrogen content measured in tobacco, to obtain accurate results. 另外,本发明提供的方法采用连续消解的方式,操作简单、省时,步骤简便,且消解条件温和, 本发明提供的方法批量处理样品能力较强,处理周期较短,大大提高了检测效率。 Further, the present invention provides a method of digestion continuous manner, the operation is simple, time-saving, simple steps, and the digestion mild conditions, the present invention provides methods of batch processing capability sample strong, short processing cycle, greatly improving the detection efficiency. 附图说明 BRIEF DESCRIPTION

[0026] 图1为本发明实施例1得到的紫外光谱图; [0026] FIG 1 UV spectrum obtained in Example 1 of the present invention;

[0027] 图2为本发明实施例1得到的非线性二级标准曲线; [0027] FIG 2 two linear calibration curve obtained in Example 1 of the embodiment of the present invention;

[0028] 图3为本发明实施例1得到的线性标准曲线。 [0028] FIG. 3 linear calibration curve obtained in Example 1 of the embodiment of the present invention.

具体实施方式 detailed description

[0029] 本发明提供了一种植物及植物制品中非蛋白质氮含量的测定方法,包括以下步骤: [0029] The present invention provides a method for measuring nitrogen content of plants and plant products of nonprotein, comprising the steps of:

[0030] a)分离植物及植物制品中的蛋白质氮,得到含有非蛋白质氮的待测试样; [0030] a) separation plants and plant products in the N protein, to obtain the sample to be tested containing non-protein nitrogen;

[0031] b)在加热条件下,向所述待测试样中加入过硫酸钾,得到混合溶液; [0031] b) under heating conditions, to the potassium persulfate was added in the test sample, to give a mixed solution;

[0032] c)将所述混合溶液依次经过紫外催化和高温加热,得到消解产物; [0032] c) the mixed solution sequentially through UV catalysis and heated to high temperature digestion product obtained;

[0033] d)检测所述消解产物,得到紫外光谱数据; [0033] d) detecting the digestion product was UV spectral data;

[0034] e)根据所述紫外光谱数据和预定的标准曲线,得到植物及植物制品中非蛋白质氮含量。 [0034] e) The UV spectra data and the predetermined standard curve to obtain a protein nitrogen content of plants and plant products Africa.

[0035] 为了便于对植物及植物制品中非蛋白质氮含量的测定,本发明优选对得到的植物及植物制品进行前处理,具体包括以下步骤: [0035] In order to facilitate determination of nonprotein nitrogen content of plants and plant products, and the present invention is preferably obtained on plants and plant products pretreatment, comprises the steps of:

[0036] 将植物及植物制品烘干、粉碎,得到植物及植物制品粉末。 [0036] The plants and plant products, drying, grinding, to give a powder of plants and plant products. 所述烘干温度优选为250C〜40°C,更优选为280C〜38°C,最优选为30°C〜35°C,所述植物及植物制品粉末的粒度优选为60目〜120目,更优选为65目〜110目,最优选为80目〜100目。 The drying temperature is preferably 250C~40 ° C, more preferably 280C~38 ° C, and most preferably 30 ° C~35 ° C, the plants and plant products, powder particle size is preferably 60 mesh ~ 120 mesh, more preferably 65 mesh ~110 mesh, and most preferably 80 mesh ~ 100 mesh.

[0037] 得到植物及植物制品粉末后,获得所述植物及植物制品粉末的干重。 [0037] After the powder obtained plants and plant products, to obtain a dry powder of the plants and plant products weight. 所述植物及植物制品粉末的干重优选按照以下方法获得: Plants and plant products the dry weight of the powder is preferably obtained by the following method:

[0038] 测定所述植物及植物制品粉末中的水分含量,用称量得到的植物及植物制品粉末的质量扣除得到的植物及植物制品粉末中的水分含量,得到所述植物及植物制品粉末的干重。 [0038] Determination of moisture content of the plants and plant products in the powder, the moisture content of the plants and plant products, plants and plant products, powder mass of powder obtained by weighing the obtained subtracted, to give the plants and plant products in powder dry weight. 本发明优选采用烘箱法测定所述植物及植物制品粉末中的水分含量,对所述烘箱法没有特殊限制。 Preferably the present invention was measured by oven method the moisture content of the plant and plant products in the powder, there is no particular restriction on the oven method. 植物及植物制品粉末的质量根据测定结果的精确度而定,本发明中,测定结果的准确度优选为0. OOOlg〜0. Olg,更优选为0. OOlg〜0. Olgo Plants and plant products quality powder according to the accuracy of the measurement result may be, in the present invention, the measurement accuracy of the results is preferably 0. OOOlg~0. Olg, more preferably 0. OOlg~0. Olgo

[0039] 得到植物及植物制品粉末的干重后,本发明分离所述植物及植物制品粉末中的蛋白质氮,得到含有非蛋白质氮的待测试样。 [0039] After the obtained dry powder of plants and plant products, protein of the present invention, the nitrogen separation plants and plant products in the powder, to obtain the sample to be tested containing non-protein nitrogen.

[0040] 本发明可以采用向植物及植物制品粉末中加入蛋白质变性试剂,加热得到的混合物,或紫外烘烤所述植物及植物制品粉末的方法,固化其中的蛋白质,分离固化后的蛋白质,得到含有非蛋白质氮的待测试样;本发明优选向植物及植物制品粉末中加入蛋白质变性试剂,将得到的混合物加热,分离固化后的蛋白质,得到含有非蛋白质氮的待测试样,所述蛋白质变性试剂优选为有机酸,更优选为醋酸水溶液;所述醋酸水溶液的体积分数优选为0. 1 %〜5 %,更优选为0. 3 %〜4 %,最优选为0. 5 %〜3 % ;所述蛋白质变性试剂的体积与植物及植物制品粉末的质量比优选为25mL : (0. 1〜3)g,更优选为25mL : (0. 3〜1) g ;优选将得到的混合物加热至沸腾;所述加热时间优选为5分钟〜50分钟,更优选为8分钟〜40分钟,最优选为20分钟〜30分钟。 [0040] The present invention can be added using a protein denaturing agent to plants and plant products in the powder, heating the resulting mixture, or the ultraviolet plants and plant products, baking powder method, wherein curing the protein, protein separated after curing, to give test sample containing non-protein nitrogen; the present invention is preferably added to the protein denaturing agent to plants and plant products in the powder, and the mixture was heated, cured after the separation of protein, to obtain the sample to be tested containing non-protein nitrogen, the protein denaturing agent is preferably an organic acid, more preferably acetic acid aqueous solution; volume fraction of the aqueous solution of acetic acid is preferably 0.1% ~ 5%, more preferably 0.3% ~ 4%, and most preferably 0.5% ~ 3%; mass and volume of the plants and plant products the protein denaturation agent powder is preferably from 25mL: (0. 1~3) g, more preferably 25mL: (0. 3~1) g; preferably obtained the mixture was heated to boiling; the heating time is preferably 5 minutes ~ 50 minutes ~ 40 minutes and more preferably 8 minutes, most preferably 20 minutes ~ 30 minutes.

[0041] 停止加热后,优选将得到的溶液趁热过滤,用所述蛋白质变性试剂优选淋洗1 次〜10次,更优选为2次〜8次,最优选为3〜5次,合并每次得到的滤液,冷却后定容,得到含有非蛋白质氮的待测试样。 [0041] After the heating was stopped, the resulting solution is preferably filtered hot, rinsed once with 1 ~ 10 times the protein denaturing agent is preferred, more preferably 2 ~ 8 times, and most preferably three to five times, per combined the resulting secondary filtrate, after cooling volume, to obtain samples to be tested contain non-protein nitrogen.

[0042] 为了减小植物及植物制品中还原性组分对其中非蛋白质氮含量测定的干扰,本发明在对所述待测试样进行消解前优选除去所述待测试样中的还原性组分。 [0042] In order to reduce interference measurement wherein the non-protein nitrogen content of plants and plant products in the reducing component of the present invention in removing the sample to be tested to be in the test sample prior to digestion preferred reducing components. 本发明中所述植物及植物制品中主要的还原组分为糖类化合物,优选当所述待测样品中总糖含量> 15% 时,更优选>20%时,优选向所述待测样品中加入过氧化氢,除去所述待测试样中的还原性组分。 In the present invention, plants and plant products in the primary reducing saccharide component, preferably the sample is measured when the total sugar content> 15%, more preferably> 20%, preferably the sample to be tested hydrogen peroxide was added, the test sample is removed in the reducing component. 所述过氧化氢与待测样品中的糖进行氧化还原反应,糖中的醛基被过氧化氢氧化为羧基,失去还原作用,所述过氧化氢的质量浓度优选为3 %〜50 %,更优选为10 %〜30 %, 本发明对所述氧化还原反应中原料的配比,反应条件等没有特殊限制,为本领域技术人员熟知的糖与过氧化氢之间的氧化还原反应。 The hydrogen peroxide with a test sample through the redox reaction of the sugar, the sugar aldehyde group into a carboxyl group by hydrogen peroxide, loss reduction, the hydrogen peroxide concentration is preferably 3% ~ 50%, more preferably 10% ~ 30%, the ratio is not particularly limited, the reaction conditions in the starting material the present invention is reducing the oxide, among well known to those skilled in the sugar reduction reaction with hydrogen peroxide.

[0043] 为了减小杂质对非蛋白质氮测定的干扰,本发明在对所述待测试样进行消解前优选除去所述待测试样中的杂质,将得到的滤液定容,得到含有非蛋白质氮的待测试样,如所述待测样品中含有无机色素时,可以采用以下方法处理:优选向所述滤液中加入活性炭,过滤得到的混合溶液,除去其中的无机色素;所述待测样品含有金属离子时,可以采用以下方法处理:优选向所述滤液中加入乙二胺四乙酸二钠溶液,过滤得到的混合溶液,除去其中的金属离子,所述乙二胺四乙酸二钠溶液的浓度优选为0. lg/L〜5g/L,更优选为0. 2g/L〜 3g/L,最优选为0. 8g/L〜2g/L ;所述待测样品含有无机色素和金属离子时,可以先用上述方法除去无机色素再除去金属离子,也可以先用上述方法除去金属离子再除去无机色素。 [0043] In order to reduce the contaminants of non-protein nitrogen determination, in the present invention, the test sample is preferably removed prior to digestion for the impurities in the test sample, the obtained filtrate volume, containing a non give nitrogen-like protein to be tested, when the test sample as containing an inorganic pigment, the processing method may be employed: activated carbon is preferably added to the filtrate, and the resulting mixed solution was filtered to remove inorganic pigments therein; said to be when measuring a sample containing a metal ion, may be employed the following methods: preferably disodium EDTA solution was added to the filtrate, the mixed solution obtained was filtered to remove the metal ions wherein the disodium edetate concentration of the solution is preferably 0. lg / L~5g / L, more preferably 0. 2g / L~ 3g / L, and most preferably 0. 8g / L~2g / L; the sample to be tested containing an inorganic pigment and metal ions, the method described above can first remove metal ions and then removing the inorganic pigments, the method described above may be first removed and then removing the metal ions of inorganic pigments.

[0044] 得到含有非蛋白质氮的待测试样后,本发明在加热条件下,向所述待测试样中加入过硫酸钾,得到混合溶液。 After [0044] Test Sample to be obtained containing non-protein nitrogen, the present invention under heating conditions, to the test sample of potassium persulfate was added to obtain a mixed solution. 所述过硫酸钾在加热条件下释放出活性氧原子[0],得到的活性氧原子[0]会对待测试样中的非蛋白质氮化合物进行消解,得到消解产物。 The release of potassium persulfate under heating in the active oxygen [0], the obtained active oxygen [0] non-protein nitrogen compound treated test samples were digested to obtain digestion product. 所述过硫酸钾与所述植物及植物制品干重的质量比优选为1 : (1〜20),更优选为1 : O〜15),最优选为1 : (3〜10);所述过硫酸钾优选为过硫酸钾溶液,所述过硫酸钾溶液的摩尔浓度优选为0. lmol/L 〜lmol/L,更优选为0. 15mol/L 〜0. 8mol/L,最优选为0. 25mol/L 〜0. 5mol/ L ;所述加热温度优选为90°C〜110°C,更优选为95°C〜105°C。 The potassium persulfate and the dry weight of plants and plant products in the mass ratio is preferably 1: (1~20), more preferably from 1: O~15), and most preferably 1: (3~10); the potassium persulfate is preferably potassium persulfate solution, the molar concentration of the potassium persulfate solution is preferably 0. lmol / L ~lmol / L, more preferably 0. 15mol / L ~0. 8mol / L, and most preferably 0 .. 25mol / L ~0 5mol / L; the heating temperature is preferably 90 ° C~110 ° C, more preferably 95 ° C~105 ° C.

[0045] 得到混合溶液后,本发明将所述混合溶液进行紫外催化,得到紫外催化的消解产物。 After [0045] The resulting mixed solution, the mixed solution of the present invention UV catalysis, to give the product an ultraviolet catalyzed digestion. 在紫外催化过程中,上述得到的部分活性氧原子[0]在紫外催化的条件下与水反应, 优选在紫外灯照射条件下,生成自由基,所述自由基可对待测试样中的各类有机氮等还原性组分进行消解,得到紫外催化的消解产物。 Ultraviolet catalytic processes, part of the above obtained active oxygen atom [0] under the condition of UV-catalyzed reaction with water, preferably under UV light irradiation conditions, generate free radicals, the radical treatment of various types of test samples organic nitrogen reducing component for digestion, digestion product obtained by UV catalysis. 所述紫外催化优选在非硫酸酸性环境中进行紫外催化,更优选为在盐酸酸性环境中进行紫外催化;所述紫外催化的温度优选为90°C〜 110°c,更优选为95°C 〜105 °C。 The UV catalyzed preferably sulfuric acid in an acidic environment of a non-catalyzed ultraviolet, UV and more preferably in an acidic hydrochloric acid catalytic environment; said UV catalyst temperature is preferably 90 ° C~ 110 ° c, more preferably 95 ° C ~ 105 ° C.

[0046] 得到紫外催化的消解产物后,本发明将所述紫外催化的消解产物继续进行高温加热,得到所述待测试样的消解产物。 After [0046] to give the product an ultraviolet catalyzed digestion, the digestion product of the present invention, ultraviolet catalytic high-temperature heating is continued, the test sample to obtain the digestion product. 在高温加热过程中,上述得到的活性氧原子[0]在高温条件下对所述紫外催化的消解产物进行进一步地消解,得到所述待测样品的消解产物。 In the high-temperature heating process, the above obtained active oxygen [0] at a high temperature of digestion of the product of the UV-catalyzed further digestion, the resulting digestion product samples tested. 所述高温加热的温度优选为95°C〜150°C,更优选为100°C〜140°C,最优选为110°C〜130°C; 所述高温加热优选为加压高温加热,所述加压高温加热的压力优选为5Psi〜8Psi,更优选为5. 5Psi 〜7. 5Psi。 The heating temperature is preferably a temperature of 95 ° C~150 ° C, more preferably from 100 ° C~140 ° C, and most preferably from 110 ° C~130 ° C; temperature of the pressurized heating is preferably heated to high temperatures, the pressurizing said pressure is preferably high-temperature heating 5Psi~8Psi, more preferably 5. 5Psi ~7. 5Psi.

[0047] 得到所述待测试样的消解产物后,检测所述消解产物,本发明优选采用紫外分光光度法检测所述消解产物,得到所述消解产物的紫外光谱数据。 [0047] The sample to be tested to obtain the product after digestion, the digestion product is detected, the present invention is preferably UV spectrophotometry the digestion product was digested UV spectral data of the product. 首先将得到的消解产物还原,得到亚硝酸盐,然后将所述亚硝酸盐优选与磺胺和Ν-α-萘基)乙二胺二盐酸盐反应,得到紫红色产物,采用紫外分光光度法测定得到的紫红色产物,得到所述消解产物的紫外光谱数据。 The resulting digestion product was first reduced to give the nitrite and the nitrite is preferably a sulfonamide and Ν-α- naphthyl) ethylenediamine dihydrochloride salt, obtained as a purple product by ultraviolet spectrophotometry the resulting purple product was measured to obtain the ultraviolet spectrum data digestion product. 优选用镉将得到的消解产物还原,得到亚硝酸盐;所述磺胺的浓度优选为Ig/ L〜50g/L,更优选为10g/L〜40g/L,最优选为20g/L〜30g/L ;所述N-萘基乙二胺盐酸盐的浓度优选为0. lg/L〜10g/L,更优选为0. 5g/L〜8g/L,最优选为lg/L〜5g/L ;所述测定波长优选为520nm〜560nm,更优选为530nm〜550nm,最优选为5;35nm〜M5nm。 Preferably cadmium resulting digestion product is reduced to afford nitrite; preferably the concentration of the sulfonamide Ig / L~50g / L, more preferably 10g / L~40g / L, and most preferably 20g / L~30g / L; the concentration of hydrochloride N- naphthyl ethylenediamine is preferably 0. lg / L~10g / L, more preferably 0. 5g / L~8g / L, and most preferably from lg / L~5g / L; the measurement wavelength is preferably 520nm~560nm, more preferably 530nm~550nm, and most preferably 5; 35nm~M5nm.

[0048] 根据上述技术方案得到的紫外光谱数据和预定的标准曲线,即可得到植物及植物制品中非蛋白质氮含量。 [0048] The UV spectrum data obtained in the above technical solutions and a predetermined standard curve to obtain a protein nitrogen content of plants and plant products Africa.

[0049] 在本发明中,所述标准曲线优选按照以下方法获得: [0049] In the present invention, preferably the standard curve obtained in the following manner:

[0050] 配制系列浓度的标准溶液; [0050] The preparation of standard solution concentration series;

[0051] 在加热条件下,向所述标准溶液中加入过硫酸钾,得到混合溶液; [0051] under heating, potassium persulfate was added to the standard solution to obtain a mixed solution;

[0052] 将所述混合溶液依次经过紫外催化和高温加热,得到消解产物; [0052] After the mixed solution was successively heated to high temperatures and UV catalysis, to obtain digestion product;

[0053] 检测所述消解产物,得到系列浓度标准溶液的紫外光谱数据; [0053] The digestion product was detected, the UV spectral data to obtain a series of concentrations of the standard solution;

[0054] 根据所述紫外光谱数据及系列浓度绘制得到标准曲线。 [0054] Draw standard curve based on the UV spectral data and concentration series.

[0055] 本发明中所述标准溶液优选为硝酸钠水溶液,采用国家标准物质研究中心的硝酸盐氮标准,配制系列浓度的标准溶液。 [0055] The standard solution of the present invention is preferably a nitrate solution, nitrate nitrogen using standard National Research Center, concentration series of the standard solution preparation. 首先,配制标准物质的储备液,将得到的储备液稀释至标准溶液的浓度。 First, a stock solution of a standard substance formulation, resulting stock solution was diluted to a concentration of the standard. 所述标准溶液的质量浓度优选为0.001%〜10%,更优选为0. 01%〜 5%,最优选为0. 〜;优选用醋酸溶液将标准物质储备液稀释到标准溶液的浓度,所述醋酸溶液的体积分数优选为0. 1 %〜10 %,更优选为0. 25 %〜8 %,最优选为0. 5 %〜 5%。 The mass concentration of the standard solution is preferably 0.001% ~ 10%, more preferably from 0.01% to 5%, and most preferably 0. ~; preferably acetic acid solution was diluted with stock solution to a concentration of the standard substance standard solution, the acetic acid solution of said volume fraction is preferably 0.1% ~ 10%, more preferably from 0.25% ~ 8%, and most preferably from 0.5% to 5%.

[0056] 得到系列浓度的标准溶液后,本发明在加热条件下,向所述标准溶液中加入过硫酸钾,得到混合溶液。 After the [0056] concentration of the standard solution series, under heating in the present invention, potassium persulfate was added to the standard solution to obtain a mixed solution. 所述过硫酸钾在加热条件下释放出活性氧原子[0],得到的活性氧原子[0]会对所述标准溶液进行消解,得到消解产物。 The release of potassium persulfate under heating in the active oxygen [0], the obtained active oxygen [0] The standard solution will be digested to obtain digestion product. 所述过硫酸钾与所述标准溶液中标准物质的质量比优选为1 : (1〜20),更优选为1 : O〜15),最优选为1 : (3〜10);所述过硫酸钾优选为过硫酸钾溶液,所述过硫酸钾溶液的摩尔浓度优选为0. lmol/L〜lmol/ L,更优选为0. 15mol/L〜0. 8mol/L,最优选为0. 25mol/L〜0. 5mol/L ;所述加热温度优选为90°C〜110°C,更优选为95°C〜105°C。 The standard solution of potassium persulfate and the mass ratio of the standard substance is preferably 1: (1~20), more preferably from 1: O~15), and most preferably 1: (3~10); said through preferably potassium persulfate solution, the molar concentration of the potassium persulfate solution is preferably 0. lmol / L~lmol / L, more preferably 0. 15mol / L~0. 8mol / L, and most preferably 0. . 25mol / L~0 5mol / L; the heating temperature is preferably 90 ° C~110 ° C, more preferably 95 ° C~105 ° C.

[0057] 得到混合溶液后,将所述混合溶液依次经过紫外催化和高温加热,得到消解产物。 [0057] After the obtained mixed solution, the mixed solution sequentially through an ultraviolet catalyst and heated to high temperatures, resulting digestion product. 所述紫外催化和高温加热过程与上述技术方案中的紫外催化和高温加热过程相同。 The ultraviolet and catalytic processes with high-temperature heating and high temperature heating above-described ultraviolet catalytic aspect of the process the same.

[0058] 按照上述技术方案中的紫外催化和高温加热过程,得到消解产物后,检测所述消解产物,得到系列浓度标准溶液的紫外光谱数据。 After the [0058] UV catalyst according to the above technical solution and heated at high temperature, digestion product was obtained, the digestion product was detected, the UV spectral data to obtain a series of concentrations of the standard solution. 所述检测过程与上述技术方案中的检测过程相同。 The detection process of the above-described aspect same detection process.

[0059] 根据上述技术方案中的检测过程,得到系列浓度标准溶液的紫外光谱数据后,根据所述紫外光谱数据及其对应的浓度绘制标准曲线。 After [0059] According to the above aspect of the detection process, the UV spectral data to obtain a series of concentrations of the standard solutions, standard curve, according to the UV spectral data and its corresponding concentration. 所述标准曲线优选为非线性二级标准曲线或线性标准曲线。 The standard curve preferably is a linear or non-linear calibration curve two standard curve.

[0060] 根据上述技术方案得到的植物及植物制品消解产物的紫外光谱数据和标准曲线, 经过计算即可得到植物及植物制品中非蛋白质氮的质量,再将所述非蛋白质氮的质量除以上述植物及植物制品的干重,得到植物及植物制品中非蛋白质氮含量。 [0060] UV spectral data and standard curve digestion product obtained according to the above aspect of plants and plant products, obtained after mass calculated nonprotein nitrogen to plants and plant products, the quality of the non-protein nitrogen and then divided by It said plant and plant dry weight of the article, to give a protein nitrogen content of plants and plant products Africa.

[0061] 本发明中,对植物及植物制品含有的非蛋白质氮化合物中的烟碱、茶碱和亮氨酸进行了测定,测定了烟草中非蛋白质氮含量,均得到了准确的结果。 [0061] In the present invention, non-protein nitrogen compounds to plants and plant products containing nicotine, theophylline, and leucine were measured, protein nitrogen content measured tobacco Africa, accurate results were obtained. [0062] 烟碱,俗称尼古丁,是一种存在于茄科植物中的生物碱,具有式(I)结构: [0062] nicotine, commonly known as nicotine, present in a Solanaceae plant alkaloids having the formula (I) Structure:

[0063] [0063]

[0064] 茶碱是氮杂环类化合物,为植物及植物制品中植物碱的一种,具有式(II)结构: [0064] Theophylline is a nitrogen heterocyclic compound, as a plant and plant products, plant alkaloids, and has the structure of formula (II):

[0066] 亮氨酸可用来配制植物生长促进剂,是植物及植物制品中重要的非蛋白质氮化合物之一,具有式(III)结构: [0066] leucine used to formulate the plant growth-promoting agent, one non-protein nitrogen compounds in plants and plant products is important, having the formula (III) Structure:

[0067] [0067]

[0068] 本发明提供的植物及植物制品中非蛋白质氮含量的测定方法,过硫酸钾释放出的活性氧原子[0]首先对植物及植物制品进行初步消解,然后依次在紫外催化和高温加热条件下对植物及植物制品进行进一步的消解,最终使植物及植物制品中的非蛋白质氮化合物得到相对完全、彻底的消解,而且消除了其中还原性组分对消解产物的影响,具有良好的消解效果,得到的消解产物具有良好的均一性,本发明提供的方法对植物及植物制品中非蛋白质氮测定的回收率高,结果准确。 [0068] Determination of the nitrogen content of plants and plant products of the present invention provides a nonprotein, potassium persulfate released active oxygen atoms [0] First, the plants and plant products preliminary digestion, followed by heating at high temperature and UV catalysis plants and plant products, for further digestion under the conditions of the final non-protein nitrogen compounds in plants and plant products obtained relative total, complete digestion, but which eliminates the influence of the reducing component of the digestion product with good digestion effect, resulting digestion product having good uniformity, the present invention provides a method for the recovery of plants and plant products is high nonprotein nitrogen determination, accurate results. 实验结果表明,本发明提供的方法对植物及植物制品中非蛋白质氮化合物烟碱测定的回收率为98. 76%〜100. 9%,茶碱的回收率达到100. 8%, 亮氨酸的回收率达到99.0%。 Experimental results show that the present invention provides a method for the recovery of plants and plant products nicotine measured nonprotein nitrogen compound is 98.76% ~ 100 9% and the recovery reaches 100.8% theophylline, leucine the recovery rate of 99.0%. 采用本发明提供的方法测定了烟草中的非蛋白质氮的含量, 结果准确。 The present invention provides a method to determine the content of non-protein nitrogen in tobacco, accurate results. 另外,本发明提供的方法具有良好的稳定性和重复性。 Further, the present invention provides a method having a good stability and reproducibility.

[0069] 为了进一步说明本发明,以下结合实施例对本发明提供的植物及植物制品中非蛋白质氮含量测定方法进行详细描述,但不能将它们理解为对本发明保护范围的限定。 [0069] In order to further illustrate the present invention, the following embodiments of the plant in conjunction with the present invention provides methods for protein determination and nitrogen content of the plant product Africa described in detail, but they should not be construed as limiting the scope of the present invention.

[0070] 实施例1 [0070] Example 1

[0071] 将Ilg硝酸钠溶解于IOOmL蒸馏水中,得到质量浓度为10. 0 %的硝酸钠储备液。 [0071] The sodium Ilg IOOmL dissolved in distilled water to give a concentration of 10.0% by mass of sodium nitrate stock solution. 准确移取1. OmL,2. OmL,4. OmL,6. OmL,8. OmLUO. OmL所述标准储备液,用体积分数为0. 5% 的醋酸溶液分别定容到lOOmL,得到系列浓度的硝酸钠标准待测溶液。 Accurate pipetting 1. OmL, 2. OmL, 4. OmL, 6. OmL, 8. OmLUO. OmL The standard stock solution, a volume fraction of 0.5% acetic acid solution are made up to lOOmL, to give a series of concentrations standard sodium nitrate solution to be measured. 分别取所述标准待测溶液2mL,倾入连续流动分析仪样品管中分别平行测定三次。 The standard test solution were taken 2mL, poured into a continuous flow analyzer sample tube was measured three times respectively in parallel. 在连续流动分析仪中,样品进样量为0. lmL/min,进样时间为100s,冲洗时间为120s。 In the continuous flow analyzer, the sample injection volume was 0. lmL / min, the injection time is 100s, the flushing time is 120s. 首先在90°C下,向所述标准待测溶液中加入2mL摩尔浓度为0. 3mol/L的过硫酸钾溶液,过硫酸钾溶液的进样量为0. 8mL/min, 然后得到的混合溶液在90°C、盐酸提供的酸性条件下进行紫外灯照射:3min,接着在6Psi压力下高温加热得到的紫外催化的消解产物2. 5min,加热温度为110°C,得到样品的消解产物。 First at 90 ° C, was added to 2mL molar concentration of the standard test solution was 0. 3mol / L solution of potassium persulfate, potassium persulfate solution injection volume was 0. 8mL / min, and the resulting mixture the solution was irradiated with UV light at 90 ° C, to provide the acidic conditions of hydrochloric acid: 3min, followed by UV-catalyzed digestion product obtained in the high-temperature heating 2. 5min 6Psi pressure, the heating temperature was 110 ° C, to obtain the digestion product samples. 得到的消解产物经过镉柱被还原为亚硝酸盐,进入检测器进行紫外分光光度法测定,检 The resulting digestion product was cadmium column is reduced to nitrite, into the detector UV spectrophotometry, detection

(III )。 (III). 测波长为MOnm,得到标准物质的紫外光谱图。 Measuring wavelength MOnm, UV spectrum to obtain the standard substances.

[0072] 标准物质的紫外光谱图如图1所示,图1为本发明实施例1得到的紫外光谱图,图中曲线上的信号叉从第五个开始紧接着的6个信号叉依次为系列浓度的标准溶液的电信号强度。 [0072] UV spectrum of a standard substance shown in FIG. 1, FIG. 1 shows UV spectrum of the embodiment of the invention obtained in Example 1, the signal on the fork from the fifth curve in FIG. 6 immediately start signals were fork the strength of the electric signal standard solution concentration series. 根据得到的系列浓度的标准物质的紫外光谱图及其对应的浓度绘制得到标准曲线,如图2和图3所示,图2为本发明实施例1得到的非线性二级标准曲线,图3为本发明实施例1得到的线性标准曲线,图3所示的线性标准曲线的硝酸根浓度线性范围为0. 〜 1%,线性方程为:A(吸光度)=-1076. 98+47750. 43C(% ),相关系数r为0.9981。 The UV spectrum and plotted to give the corresponding concentration of the standard substance to give a series of concentrations of the standard curve, as shown in FIG. 2 and FIG. 3, FIG. 2 two linear calibration curve obtained in Example 1 of the embodiment of the present invention, FIG 3 .. 1076 98 + 47750 43C - a (absorbance) =: Example 1 to obtain a linear calibration curve, nitrate linear range shown in FIG. 3 a linear standard curve is 0.5% to 1%, the present invention is the linear equation (%), the correlation coefficient r = 0.9981. 由图中可以看出,本发明提供的方法对非蛋白质氮氮含量测定的电信号强度得到明显的提高,而且电信号强度与其浓度之间存在良好的线性关系,本发明提供的方法具有良好的效果。 As can be seen from the figure, the present invention provides a method of significantly improving the strength of the electrical non-protein nitrogen content of a nitrogen determination, and there is a good linear relationship between the intensity of the electric signal and the concentration, the present invention provides a method has good effect.

[0073] 比较例1 [0073] Comparative Example 1

[0074] 将Ilg硝酸钠溶解于IOOmL蒸馏水中,得到质量浓度为10. O %的硝酸钠储备液。 [0074] The sodium Ilg IOOmL dissolved in distilled water to give a concentration of 10. O% stock solution of sodium nitrate. 准确移取1. OmL,2. OmL,4. OmL,6. OmL,8. OmLUO. OmL所述标准储备液,用体积分数为0. 5% 的醋酸溶液分别定容到lOOmL,得到系列浓度的硝酸钠标准溶液。 Accurate pipetting 1. OmL, 2. OmL, 4. OmL, 6. OmL, 8. OmLUO. OmL The standard stock solution, a volume fraction of 0.5% acetic acid solution are made up to lOOmL, to give a series of concentrations sodium nitrate standard solution. 分别取得到的标准溶液2mL,倾入连续流动分析仪样品管中分别平行测定三次。 Standard solutions were made to 2mL, poured into the continuous flow analyzer sample tube was measured three times respectively in parallel. 在连续流动分析仪中,样品进样量为0. lmL/min,进样时间为100s,冲洗时间为120s。 In the continuous flow analyzer, the sample injection volume was 0. lmL / min, the injection time is 100s, the flushing time is 120s. 首先在90°C下,向所述标准溶液中加入2mL摩尔浓度为0. 3mol/L的过硫酸钾溶液,过硫酸钾溶液的进样量为0. SmL/min,然后在6Psi压力高温加热得到的混合溶液2. 5min,加热温度为110°C,得到样品的消解产物。 First at 90 ° C, was added to 2mL molar concentration of the standard solution for 0. 3mol / L solution of potassium persulfate, potassium persulfate solution injection volume was 0. SmL / min, and then heated at a high temperature pressure 6Psi the resulting mixed solution 2. 5min, the heating temperature was 110 ° C, to obtain the digestion product samples. 得到的消解产物经过镉柱被还原为亚硝酸盐,进入检测器进行紫外分光光度法检测,检测波长为MOnm,得到标准物质的紫外光谱图。 The resulting digestion product was cadmium column is reduced to nitrite, into the detector UV spectrophotometry, detection wavelength MOnm, UV spectrum to obtain the standard substances.

[0075] 根据得到的系列浓度的标准物质的紫外光谱图绘制得到标准曲线。 [0075] The standard curve plotted spectra UV series of concentrations of the standard substance obtained.

[0076] 实施例2〜3 [0076] Example 2 or 3

[0077] 将3. 2446g烟碱用蒸馏水溶解并定容至200mL,得到质量浓度为1. 60%的烟碱储备液。 [0077] The nicotine 3. 2446g was dissolved in distilled water qs to 200 mL, to give a mass concentration of 1.60% stock solution of nicotine. 移取16. OmL,32. OmL所述烟碱储备液,用体积分数为0. 5 %的醋酸溶液定容到lOOmL,得到烟碱待测溶液。 Pipette 16. OmL, the 32. OmL nicotine stock solution, with the volume fraction of 0.5% acetic acid solution volume to lOOmL, nicotine resulting solution was measured. 移取2. OmL所述两种不同浓度的烟碱待测溶液,倾入流动分析仪样品管中分别平行测定三次。 2. Pipette the OmL two kinds of the test solutions of different concentrations of nicotine, three replicates was poured into the flow analyzer sample tube respectively. 在连续流动分析仪中,样品进样量为0. lmL/min,进样时间为100s,冲洗时间为120s。 In the continuous flow analyzer, the sample injection volume was 0. lmL / min, the injection time is 100s, the flushing time is 120s. 首先在90°C下,向所述烟碱待测溶液中加入2mL摩尔浓度为0. 3mol/L的过硫酸钾溶液,过硫酸钾溶液的进样量为0. SmL/min,然后得到的混合溶液在90°C、盐酸提供的酸性条件下进行紫外灯照射3min,接着在6Psi压力下高温加热得到的紫外催化的消解产物2. 5min,加热温度为110°C,得到烟碱样品的消解产物。 First at 90 ° C, the nicotine was added to the test solution 2mL molar concentration of 0. 3mol / L solution of potassium persulfate, potassium persulfate solution injection volume was 0. SmL / min, and the resulting the solution was mixed at 90 ° C, hydrochloric acid acidic conditions to provide an ultraviolet light irradiation 3min, followed by UV-catalyzed digestion product at a pressure high-temperature heating 6Psi obtained 2. 5min, the heating temperature was 110 ° C, to obtain a sample digestion nicotine product. 得到的消解产物经过镉柱被还原为亚硝酸盐,进入检测器进行紫外分光光度法检测,检测波长为540nm,得到烟碱的紫外光谱图。 The resulting digestion product was cadmium column is reduced to nitrite, into the detector UV spectrophotometry, detection wavelength was 540 nm, to obtain a UV spectrum of nicotine.

[0078] 根据得到的烟碱的紫外光谱图和实施例1得到的标准曲线,得到烟碱的氮含量, 计算得到烟碱的平均质量分别为5. 113mg, 10. 448mg,对烟碱测定的回收率为98. 76 %、 100. 90%,结果如表1所示,表1为本发明实施例2〜3与比较例2〜3得到的测定结果。 [0078] The UV spectrum of nicotine and obtained in Example 1 to obtain a standard curve, obtained nitrogen content of nicotine, nicotine calculated as the average mass 5. 113mg, 10. 448mg, respectively, of the nicotine assay recovery was 98.76%, 100.90%, as shown in table 1, table 2 or 3 in Example 1 of the present measurement results obtained in Comparative Example 2 or 3 of the embodiment of the invention.

[0079] 比较例2〜3 [0079] Comparative Examples 2 to 3

[0080] 将3. 2446g烟碱用蒸馏水溶解并定容至200mL,得到质量浓度为1. 60%的烟碱储备液。 [0080] The nicotine 3. 2446g was dissolved in distilled water qs to 200 mL, to give a mass concentration of 1.60% stock solution of nicotine. 准确移取16. OmL,32. OmL所述烟碱储备液,用体积分数为0. 5%的醋酸溶液定容到IOOmL,得到烟碱待测溶液。 Accurate pipetting 16. OmL, the 32. OmL nicotine stock solution, with the volume fraction of 0.5% acetic acid solution volume to IOOmL, nicotine resulting solution was measured. 移取2. OmL所述两种不同浓度的烟碱待测溶液,倾入连续流动分析仪样品管中分别平行测定三次。 Pipette 2. OmL the two different concentrations of nicotine was measured, poured into a continuous flow analyzer sample tube was measured three times respectively in parallel. 在连续流动分析仪中,样品进样量为0. lmL/min,进样时间为100s,冲洗时间为120s。 In the continuous flow analyzer, the sample injection volume was 0. lmL / min, the injection time is 100s, the flushing time is 120s. 首先在90°C下,向所述烟碱待测溶液中加入2mL摩尔浓度为0. 3mol/L的过硫酸钾溶液,过硫酸钾溶液的进样量为0. SmL/min,然后在6Psi压力下高温加热得到的混合溶液2. 5min,加热温度为110°C,得到样品的消解产物。 First at 90 ° C, was added to 2mL molar concentration of the solution to be tested for nicotinic 0. 3mol / L solution of potassium persulfate, potassium persulfate solution injection volume was 0. SmL / min, then 6Psi high temperature heating under pressure the resulting mixed solution 2. 5min, the heating temperature was 110 ° C, to obtain the digestion product samples. 得到的消解产物经过镉柱被还原为亚硝酸盐,进入检测器进行紫外分光光度法检测,检测波长为540nm,得到烟碱的紫外光谱图。 The resulting digestion product was cadmium column is reduced to nitrite, into the detector UV spectrophotometry, detection wavelength was 540 nm, to obtain a UV spectrum of nicotine.

[0081] 根据得到的烟碱的紫外光谱图和比较例1得到的标准曲线,得到烟碱的氮含量, 计算得到烟碱的平均质量为3. 943mg,7. 18%ig,对烟碱测定的回收率为75. 95%,69. 19%, 结果如表1所示,表1为本发明实施例2〜3与比较例2〜3得到的测定结果。 [0081] The UV spectrum and the standard curve obtained in Comparative Example 1 was nicotine, nicotine to obtain nitrogen content, calculated as the average mass of nicotine 3. 943mg, 7. 18% ig, nicotine measured the recovery was 75.95%, 69.19%, as shown in table 1, table 2 or 3 in Example 1 of the present measurement results obtained in Comparative Example 2 or 3 of the embodiment of the invention.

[0082] 表1本发明实施例2〜3与比较例2〜3得到的测定结果 Comparative Example 2 or 3 with the measurement results obtained in Example 2 ~ 3 [0082] Table 1 Invention

[0083] [0083]

Figure CN102519900AD00101

[0084] 由表1可知,本发明提供的方法对烟碱测定的回收率为98. 76%〜100. 90%,测定结果准确度高。 [0084] As apparent from Table 1, the present invention provides a method for the recovery of nicotine was determined to be 98.76% ~ 100. 90%, high accuracy measurement result.

[0085] 实施例4 [0085] Example 4

[0086] 将3. 6032g茶碱用蒸馏水溶解并定容至IOOmL,得到质量浓度为3. 48%的茶碱储备液。 [0086] The dissolution of theophylline 3. 6032g distilled water and dilute to IOOmL, to give a mass concentration of 3.48% stock solution of theophylline. 移取5mL所述茶碱储备液,用体积分数为0. 5%的醋酸溶液定容到lOOmL,得到茶碱待测溶液。 The pipette 5mL stock theophylline solution, with the volume fraction of 0.5% acetic acid solution to lOOmL volume, to give theophylline tested solution. 移取2. OmL所述茶碱待测溶液,倾入流动分析仪的样品管中三次平行测定,检测过程与实施例2〜3的检测过程相同,得到茶碱的紫外光谱图。 2. OmL pipetting the test solution theophylline, was poured into the flow analyzer sample tube replicates of three, the same detection process of the detection process of Example 2 or 3 to give a UV spectrum of theophylline.

[0087] 根据茶碱的紫外光谱图和实施例1得到的标准曲线,得到茶碱的氮含量,计算得到茶碱的平均质量为3. 63;3mg,对茶碱测定的回收率为100. 8%,结果如表2所示,表2为本发明实施例4与比较例4得到的测定结果。 [0087] The UV spectrum of the standard curve and theophylline obtained in Example 1 to obtain nitrogen content of theophylline, theophylline mass calculated average of 3. 63; 3mg, recovery of the theophylline assay was 100. 8%, the results as shown in table 2 table 2 of the present invention, the measurement results obtained in Comparative Example 4 Example 4.

[0088] 比较例4 [0088] Comparative Example 4

[0089] 将3. 6032g茶碱用蒸馏水溶解并定容至IOOmL,得到质量浓度为3. 48%的茶碱储备液。 [0089] The dissolution of theophylline 3. 6032g distilled water and dilute to IOOmL, to give a mass concentration of 3.48% stock solution of theophylline. 移取5mL所述茶碱储备液,用体积分数为0. 5%的醋酸溶液定容到lOOmL,得到茶碱待测溶液。 The pipette 5mL stock theophylline solution, with the volume fraction of 0.5% acetic acid solution to lOOmL volume, to give theophylline tested solution. 移取2. OmL所述茶碱待测溶液,倾入流动分析仪的样品管中平行测定三次。 Three replicates were pipetted theophylline 2. OmL the test solution, was poured into the flow analyzer sample tube. 检测过程与比较例2〜3的检测过程相同,得到茶碱的紫外光谱图。 Detection process in Comparative Example 2 or 3 of the same process of detection, UV spectrum obtained theophylline.

[0090] 根据得到的茶碱的紫外光谱图和比较例1得到的标准曲线,得到茶碱的氮含量, 计算得到茶碱的平均质量分别为2. leang,对茶碱测定的回收率为59.0%,结果如表2所示,表2为本发明实施例4与比较例4得到的测定结果。 [0090] The UV spectrum and the standard curve obtained in Comparative Example 1 was theophylline, the theophylline to obtain nitrogen content, calculated average mass of theophylline were 2. leang, recovery of Theophylline 59.0 %, the results as shown in table 2 table 2 of the present invention, the measurement results obtained in Comparative Example 4 Example 4.

[0091] 表2本发明实施例4与比较例4得到的测定结果 [0091] Inventive Example 4 Table of measurement results obtained in Comparative Example 4 2

[0092] [0092]

Figure CN102519900AD00102

[0093] 由表2可知,本发明提供的方法对茶碱测定的回收率达到100. 8%,测定结果准确度尚。 [0093] As apparent from Table 2, the present invention provides a method for the recovery of theophylline measured reaches 100.8%, the accuracy of the measurement result yet.

[0094] 实施例5 [0094] Example 5

[0095] 将5. 2468g亮氨酸用蒸馏水溶解并定容至200mL,得到质量浓度为2. 56%的亮氨酸储备液。 [0095] The leucine 5. 2468g dissolved in distilled water and dilute to 200mL, to give a concentration of 2.56% by mass of the leucine stock solution. 准确移取10. OmL所述亮氨酸储备液,用体积分数为0. 5%的醋酸溶液定容到IOOmL,得到亮氨酸待测溶液。 10. OmL accurate pipetting of the leucine stock solution, with the volume fraction of 0.5% acetic acid solution volume to IOOmL, leucine resulting solution was measured. 移取2. OmL所述亮氨酸待测溶液,倾入连续流动分析仪样品管中平行测定三次。 2. OmL pipetting the test solution leucine, poured into measured three times continuous flow analyzer sample tube parallel. 检测过程与实施例2〜3所述的检测过程相同,得到亮氨酸的紫外光谱图。 Detection process similar to Example 2 or 3 of the detection process, resulting leucine UV spectrum.

[0096] 根据得到的亮氨酸的紫外光谱图和实施例1得到的标准曲线,得到亮氨酸的氮含量,计算得到亮氨酸的质量为5. 194mg,对亮氨酸测定的回收率为99. 0%,结果如表3所示, 表3为本发明实施例5与比较例5得到的测定结果。 [0096] leucine standard curve obtained and the UV spectrum obtained in Example 1 to obtain nitrogen content of leucine, leucine calculated mass of 5. 194mg, leucine recovery determination It was 99.0%, the results of the measurement results of Example 35 and Comparative Example 5 obtained in the present embodiment of the invention shown in table 3 and table.

[0097] 比较例5 [0097] Comparative Example 5

[0098] 将5. 2468g亮氨酸用蒸馏水溶解并定容至200mL,得到质量浓度为2. 56%的亮氨酸储备液。 [0098] The leucine 5. 2468g dissolved in distilled water and dilute to 200mL, to give a concentration of 2.56% by mass of the leucine stock solution. 准确移取10. OmL所述亮氨酸储备液,用体积分数为0. 5%的醋酸溶液定容到IOOmL,得到亮氨酸待测溶液。 10. OmL accurate pipetting of the leucine stock solution, with the volume fraction of 0.5% acetic acid solution volume to IOOmL, leucine resulting solution was measured. 移取2. OmL所述亮氨酸待测溶液,倾入连续流动分析仪样品管中平行测定三次。 2. OmL pipetting the test solution leucine, poured into measured three times continuous flow analyzer sample tube parallel. 检测过程与比较例2〜3的检测过程相同,得到亮氨酸的紫外光谱图。 Detection process in Comparative Example 2 or 3 of the same process of detection, the UV spectrum obtained leucine.

[0099] 根据得到的亮氨酸的紫外光谱图和比较例1得到的标准曲线,得到亮氨酸的氮含量,计算得到亮氨酸的质量为3. 940mg,对亮氨酸测定的回收率为75. 1 %,结果如表3所示, 表3为本发明实施例5与比较例5得到的测定结果。 [0099] The UV spectrum and the standard curve obtained in Comparative Example 1 was leucine, leucine obtained nitrogen content, calculated as the mass of leucine 3. 940mg, leucine recovery determination It was 75.1%, the results of the measurement results of Example 35 and Comparative Example 5 obtained in the present embodiment of the invention shown in table 3 and table.

[0100] 表3本发明实施例5与比较例5得到的测定结果 [0100] Table 5 Example 3 of the present invention and measurement results obtained in Comparative Example 5

Figure CN102519900AD00111

[0102] 由表3可知,本发明提供的方法对亮氨酸测定的回收率达到99.0%,测定结果准 [0102] apparent from Table 3, the present invention provides a method for the determination of leucine recovery reached 99.0%, the measurement result registration

确度高。 High indeed.

[0103] 实施例6〜21 [0103] Example 6~21

[0104] 按照中华人民共和国标准GB/T19616-2004选择16种烟草样品,选用的烟草样品由本公司技术中心原料检验室烟叶组提供的2006年、2007年和2008年国内外生产的烤烟烟叶样品,按照中华人民共和国烟草行业标准YC/T31-1996制备烟末试样,测定烟末中水分含量。 [0104] According to People's Republic of China standard GB / T19616-2004 selection of 16 samples of tobacco in 2006, selected tobacco samples provided by the company's technical center raw materials laboratory tobacco group, in 2007 and 2008, domestic and foreign production of flue-cured tobacco samples, People's Republic of China in accordance with the tobacco industry standards YC / T31-1996 end nicotinic sample, measuring the moisture content of tobacco powder. 将2g烟末试样溶解于IOOmL体积分数为0. 5%的乙酸溶液中,加热沸腾15分钟, 迅速用无氮定性滤纸过滤,用体积分数为0. 5%的乙酸溶液冲洗沉淀物,合并得到的滤液, 冷却后定容到200mL,准确移取2mL滤液倾入连续流动分析仪样品管中,对每种测定样品分别平行测定三次。 The end of the cigarette sample was dissolved in 2g IOOmL volume fraction of 0.5% acetic acid solution, boiled for 15 minutes, a nitrogen-free rapid qualitative filter paper, rinsing the precipitate was 0.5% acetic acid solution with a volume fraction of the combined the filtrate obtained was cooled to 200 mL volume, accurate pipetting 2mL filtrate was poured into a continuous flow analyzer sample tube, three replicates for each measurement sample, respectively. 检测过程与实施例2〜3的检测过程相同,得到烟草样品的紫外光谱图。 Detecting the same detection process procedure in Example 2 or 3 to give a sample of tobacco UV spectrum.

[0105] 根据得到的烟草样品的紫外光谱图和实施例1得到的标准曲线,得到烟草样品的非蛋白质氮含量,结果如表4所示,表4为本发明实施例6〜21得到的测定结果。 [0105] The UV spectrum of the standard curve obtained in the tobacco sample obtained in Example 1, to obtain a non-protein nitrogen content of tobacco samples, the results as shown in Table 4 Table Example 6~21 measured present embodiment of the invention obtained 4 result.

[0106] 表4本发明实施例6〜21得到的测定结果 [0106] The measurement results obtained in Example 6~21 embodiment of the present invention Table 4

[0107] [0107]

Figure CN102519900AD00121

[0108] 注:非蛋白质氮含量*为质量百分数。 [0108] Note: * is a non-protein nitrogen content percentage by mass.

[0109] 由表5可知,本发明提供的方法对烟草中非蛋白质氮的测定结果准确,得到的数据的变异系数皆小于5%,符合分析检测的要求。 [0109] As apparent from Table 5, the present invention provides a method for accurate measurement result Tobacco nonprotein nitrogen, coefficient of variation of the data obtained are less than 5%, as analytical testing requirements.

[0110] 由以上实施例可知,本发明提供的方法对非蛋白质氮化合物具有良好的消解效果,得到的回收率高,测定植物及植物制品中非蛋白质氮含量得到的结果准确。 [0110] Example apparent from the above embodiment, the present invention provides a method having a good effect on the digestion of non-protein nitrogen compounds, high recovery obtained, accurate measurement of plants and plant products obtained protein nitrogen content Africa.

[0111] 以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。 [0111] The above are only preferred embodiments of the present invention, it should be noted that those of ordinary skill in the art, in the present invention without departing from the principles of the premise, can make various improvements and modifications, such modifications and modifications should also be regarded as the protection scope of the present invention.

Claims (10)

  1. 1. 一种植物及植物制品中非蛋白质氮含量的测定方法,包括以下步骤:a)分离植物及植物制品中的蛋白质氮,得到含有非蛋白质氮的待测试样;b)在加热条件下,向所述待测试样中加入过硫酸钾,得到混合溶液;c)将所述混合溶液依次经过紫外催化和高温加热,得到消解产物;d)检测所述消解产物,得到紫外光谱数据;e)根据所述紫外光谱数据和预定的标准曲线,得到植物及植物制品中非蛋白质氮含量。 CLAIMS 1. A method for measuring nitrogen content in plants and plant products of nonprotein, comprising the steps of: a) separating the protein plants and plant products in nitrogen, to give a test sample containing non-protein nitrogen to be; b) under heating conditions , added to the persulfate in the test sample, to give a mixed solution; c) sequentially passes through the mixed solution UV catalysis and heated to high temperature digestion product obtained; D) detecting the digestion product was UV spectral data; e) the UV spectra data and the predetermined standard curve to obtain a protein nitrogen content of plants and plant products Africa.
  2. 2.根据权利要求1所述的测定方法,其特征在于,所述紫外催化为在非硫酸酸性环境中进行紫外催化。 The measuring method according to claim 1, wherein said UV catalyst is sulfuric acid in an acidic environment, a non-UV catalysis.
  3. 3.根据权利要求1所述的测定方法,其特征在于,所述紫外催化的温度为90°C〜 110°C。 3. The measuring method according to claim 1, wherein the temperature of the UV-catalyzed 90 ° C~ 110 ° C.
  4. 4.根据权利要求1所述的测定方法,其特征在于,所述高温加热的温度为95°C〜 150°C。 4. The measuring method according to claim 1, wherein said high-temperature heating temperature of 95 ° C~ 150 ° C.
  5. 5.根据权利要求1所述的测定方法,其特征在于,所述高温加热为加压高温加热。 The measuring method according to claim 1, wherein the heating temperature of the high temperature pressing.
  6. 6.根据权利要求5所述的测定方法,其特征在于,所述加压高温加热的压力为5Psi〜 SI3Si。 6. The measurement method according to claim 5, characterized in that the pressure of the pressurized high-temperature heating 5Psi~ SI3Si.
  7. 7.根据权利要求1所述的测定方法,其特征在于,所述步骤b)中的加热温度为90°C〜 110°C。 The measuring method according to claim 1, wherein the heating temperature of step b) is from 90 ° C~ 110 ° C.
  8. 8.根据权利要求1所述的测定方法,其特征在于,所述步骤a)具体为:向植物及植物制品中加入蛋白质变性试剂,加热得到的混合物,分离后得到含有非蛋白质氮的待测试样。 8. A measuring method according to claim 1, wherein said step a) is specifically: addition of a protein denaturing agent to plants and plant products, heating the resulting mixture, containing the test obtained after separation of non-protein nitrogen sample.
  9. 9.根据权利要求8所述的测定方法,其特征在于,所述蛋白质变性试剂为有机酸。 9. A measuring method according to claim 8, wherein the protein denaturing agent is an organic acid.
  10. 10.根据权利要求1所述的测定方法,其特征在于,所述步骤b)前还包括: 向所述待测试样中加入过氧化氢,除去所述待测试样中的还原性组分;和/或向所述待测试样中加入活性炭,除去所述待测试样中的无机色素; 和/或向所述待测试样中加入乙二胺四乙酸二钠,除去所述待测试样中的金属离子。 10. The measuring method according to claim 1, wherein said step b) before further comprises: adding to said sample to be tested hydrogen peroxide, the test sample to be removed reductively group points; and / or in the test sample to the activated carbon is added to remove the test sample of the inorganic pigments; and / or disodium edetate was added to the sample to be tested, removing the said metal ions in the sample to be tested.
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CN101349637A (en) * 2008-07-22 2009-01-21 广东中烟工业有限责任公司 Method for measuring non-protein nitrogen content in tobacco
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