CN102009964A - Method for extracting and detecting nitrate and nitrite in Chinese sauerkraut - Google Patents
Method for extracting and detecting nitrate and nitrite in Chinese sauerkraut Download PDFInfo
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- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 title claims abstract description 46
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910002651 NO3 Inorganic materials 0.000 title claims abstract description 43
- 235000021108 sauerkraut Nutrition 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 34
- 238000000605 extraction Methods 0.000 claims abstract description 19
- 238000001514 detection method Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 55
- HWYHZTIRURJOHG-UHFFFAOYSA-N luminol Chemical compound O=C1NNC(=O)C2=C1C(N)=CC=C2 HWYHZTIRURJOHG-UHFFFAOYSA-N 0.000 claims description 16
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000012488 sample solution Substances 0.000 claims description 12
- 238000004458 analytical method Methods 0.000 claims description 11
- 230000003068 static effect Effects 0.000 claims description 9
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 8
- XWNSFEAWWGGSKJ-UHFFFAOYSA-N 4-acetyl-4-methylheptanedinitrile Chemical compound N#CCCC(C)(C(=O)C)CCC#N XWNSFEAWWGGSKJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000004153 Potassium bromate Substances 0.000 claims description 7
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 7
- 229940094037 potassium bromate Drugs 0.000 claims description 7
- 235000019396 potassium bromate Nutrition 0.000 claims description 7
- 239000007853 buffer solution Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000001052 transient effect Effects 0.000 claims description 6
- 238000004020 luminiscence type Methods 0.000 claims description 5
- 238000005259 measurement Methods 0.000 claims description 5
- 229910021538 borax Inorganic materials 0.000 claims description 4
- 239000000276 potassium ferrocyanide Substances 0.000 claims description 4
- 239000012047 saturated solution Substances 0.000 claims description 4
- 239000004328 sodium tetraborate Substances 0.000 claims description 4
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 4
- XOGGUFAVLNCTRS-UHFFFAOYSA-N tetrapotassium;iron(2+);hexacyanide Chemical compound [K+].[K+].[K+].[K+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] XOGGUFAVLNCTRS-UHFFFAOYSA-N 0.000 claims description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000004246 zinc acetate Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 8
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 4
- 230000035945 sensitivity Effects 0.000 abstract description 3
- CEKJAYFBQARQNG-UHFFFAOYSA-N cadmium zinc Chemical compound [Zn].[Cd] CEKJAYFBQARQNG-UHFFFAOYSA-N 0.000 abstract description 2
- 230000009467 reduction Effects 0.000 description 6
- 235000013311 vegetables Nutrition 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 230000010355 oscillation Effects 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 238000005554 pickling Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 2
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
提取及检测酸菜中硝酸盐和亚硝酸盐的方法，涉及一种提取和检测的方法。本发明解决了解决现有提取酸菜中硝酸盐和亚硝酸盐方法存在时间长、效率低操作复杂问题，及检测方法存在工艺复杂、耗时长、线性范围窄等缺点。本发明利用微波法辅助提取酸菜中的硝酸盐、亚硝酸盐。利用锌-镉水浴振荡法还原硝酸盐，采用光化学方法检测硝酸盐和亚硝酸盐。本发明所述提取方法具有工艺简单、耗时短、提取率高、设备简单、适用范围广、重现性好、节省时间、节省试剂、污染小等特点。本发明所述检测方法具有工艺简单、耗时短、灵敏度高、线性范围宽、仪器设备简单优点。The invention discloses a method for extracting and detecting nitrate and nitrite in sauerkraut, relating to an extraction and detection method. The invention solves the problems of long time, low efficiency and complex operation in the existing method for extracting nitrate and nitrite in sauerkraut, and the shortcomings of the detection method such as complicated process, long time consumption and narrow linear range. The invention utilizes a microwave method to assist in extracting nitrate and nitrite in sauerkraut. Nitrate was reduced by zinc-cadmium water bath shaking method, and nitrate and nitrite were detected by photochemical method. The extraction method of the invention has the characteristics of simple process, short time consumption, high extraction rate, simple equipment, wide application range, good reproducibility, time saving, reagent saving, little pollution and the like. The detection method of the invention has the advantages of simple process, short time consumption, high sensitivity, wide linear range and simple equipment.
Description
技术领域technical field
本发明涉及一种提取和检测的方法。The invention relates to a method for extraction and detection.
背景技术Background technique
酸菜作为一种北方常见腌菜，以白菜为原料，采用腌制的方法贮藏，以此来补充冬季蔬菜的缺乏。在腌制过程中，借助天然附着在蔬菜表面的某些微生物进行发酵，在还原菌作用下，蔬菜中的硝酸盐会被还原成亚硝酸盐。有研究表明[1]，蔬菜在腌制的过程中，其亚硝酸盐的含量呈现先上升后下降的趋势。当人们食用亚硝酸盐含量超标的酸菜，就会一起亚硝酸盐中毒，轻者头昏、心悸、呕吐、口唇青紫，重者神志不清、抽搐、呼吸急促，抢救不及时可危及生命。此外，亚硝酸盐在人体内外与仲胺类作用形成亚硝胺类[2]，它在人体内达到一定剂量时是致癌、致畸、致突变的物质，可严重危害人体健康。Sauerkraut, as a common pickled vegetable in the north, uses cabbage as raw material and is stored by pickling to supplement the lack of winter vegetables. During the pickling process, the fermentation is carried out with the help of certain microorganisms naturally attached to the surface of the vegetables, and the nitrate in the vegetables will be reduced to nitrite under the action of reducing bacteria. Studies have shown that [1] , during the pickling process of vegetables, the nitrite content presents a trend of rising first and then falling. When people eat sauerkraut with excessive nitrite content, they will suffer from nitrite poisoning. In mild cases, dizziness, heart palpitations, vomiting, and blue lips. In addition, nitrite reacts with secondary amines inside and outside the human body to form nitrosamines [2] . When it reaches a certain dose in the human body, it is carcinogenic, teratogenic, and mutagenic substances, which can seriously endanger human health.
关于硝酸盐，亚硝酸盐的提取，传统提取方法有溶剂提取法[3]，热水提取法，振荡提取法[4]等，但是它们在提取过程中有一些不足之处，例如，提取时间长(15～20min)，提取率低(75％～85％)，操作复杂等。Regarding the extraction of nitrate and nitrite, traditional extraction methods include solvent extraction [3] , hot water extraction, vibration extraction [4] , etc., but they have some shortcomings in the extraction process, for example, extraction time Long (15-20min), low extraction rate (75%-85%), complicated operation, etc.
目前，直接测定硝酸盐的方法较少，主要是将其还原成亚硝酸盐进行测定。还原硝酸盐多数是采用镉柱进行还原，该方法还原效率虽高，但制镉粒，装柱，还原，洗涤，测定及活化步骤繁琐，耗时长。At present, there are few methods to directly measure nitrate, mainly to reduce it to nitrite for determination. Most of the reduction of nitrate is carried out by using cadmium column. Although the reduction efficiency of this method is high, the steps of preparing cadmium particles, column packing, reduction, washing, determination and activation are cumbersome and time-consuming.
关于亚硝酸盐检测方法有很多种，目前检测亚硝酸盐的方法主要有格里斯试剂比色法，催化光度法，示波极谱法等，这些方法灵敏度低，干扰多，易受试剂颜色影响等缺点。试剂盒、快速检测仪等亚硝酸盐的快速检测方法，又具有线性范围窄，检出限低等缺点。There are many methods for detecting nitrite. At present, the methods for detecting nitrite mainly include Griess reagent colorimetry, catalytic photometry, oscillographic polarography, etc. These methods have low sensitivity, many interferences, and are easily affected by the color of the reagent. and other shortcomings. Rapid detection methods for nitrite such as kits and rapid detectors have the disadvantages of narrow linear range and low detection limit.
发明内容Contents of the invention
本发明的目的是为了解决现有提取酸菜中硝酸盐和亚硝酸盐方法存在时间长、效率低操作复杂问题，及检测方法存在工艺复杂、耗时长、线性范围窄等缺点。The purpose of the present invention is to solve the problems of long time, low efficiency and complex operation in the existing method for extracting nitrate and nitrite in sauerkraut, and the shortcomings of the detection method such as complex process, long time consumption and narrow linear range.
本发明中提取酸菜中硝酸盐和亚硝酸盐的方法是按下述步骤进行的：将酸菜绞碎，然后取1g经绞碎处理后的酸菜加入到2.5mL硼砂饱和溶液搅拌均匀，加入10mL蒸馏水，然后在微波加热提取5min，微波加热的温度为80℃，再加入1mL浓度为0.25mol/L的亚铁氰化钾溶液和1mL浓度为1mol/L的乙酸锌溶液，定容，静止过滤，收集滤液得到提取液；即完成酸菜中硝酸盐和亚硝酸盐提取。The method for extracting nitrate and nitrite in sauerkraut in the present invention is carried out according to the following steps: mince sauerkraut, then take 1g of sauerkraut after mincing treatment, add to 2.5mL borax saturated solution and stir evenly, add 10mL distilled water , and then extract by microwave heating for 5 minutes, the temperature of microwave heating is 80°C, then add 1 mL of potassium ferrocyanide solution with a concentration of 0.25 mol/L and 1 mL of zinc acetate solution with a concentration of 1 mol/L, constant volume, static filtration, The filtrate is collected to obtain an extract; that is, the extraction of nitrate and nitrite in sauerkraut is completed.
上述提取方法在微波场作用下，通过吸收微波能力的差异使得被硝酸盐和亚硝酸盐从基体或体系中分离，进入到介电常数较小、微波吸收能力相对差的硼砂饱和溶液中，从而完成了硝酸盐和亚硝酸盐的提取，其具有工艺简单、耗时短、提取率高、设备简单、适用范围广、重现性好、节省时间、节省试剂、污染小等特点。本发明方法的提取时间为5min，硝酸盐和亚硝酸盐提取率均在90％以上。Under the action of the microwave field, the above extraction method separates the nitrate and nitrite from the matrix or system through the difference in microwave absorption ability, and enters the borax saturated solution with a small dielectric constant and relatively poor microwave absorption ability, thereby The extraction of nitrate and nitrite has been completed, which has the characteristics of simple process, short time consumption, high extraction rate, simple equipment, wide application range, good reproducibility, time saving, reagent saving, and small pollution. The extraction time of the method of the invention is 5 minutes, and the extraction rates of nitrate and nitrite are both above 90%.
本发明中检测酸菜中硝酸盐和亚硝酸盐是按下述步骤完成的：一、鲁米诺分析液的制备：吸取7.5mL浓度为1×10-3mol/L鲁米诺溶液，用浓度为0.25mol/L的NaOH溶液定容得到鲁米诺分析液；二、亚硝酸盐的测定：取5.00mL按上述方法从酸菜中提取的提取液，然后加入10.00mL浓度为0.06mol/L的溴酸钾溶液、3.00mL浓度为5×10-3mol/L的乙二胺四乙酸(EDTA)溶液和2.50mL浓度为0.5mol/L的H2SO4溶液，定容，得到待测样溶液A，将2.00mL步骤一制备的鲁米诺分析液和2.00mL待测样溶液A依次加入到瞬稳静态化学发光仪内测量，记录反应的发光峰信号，读取峰面积Y，然后将峰面积Y带入回归方程即得到亚硝酸盐的浓度X1；三、硝酸盐的测定：取20mL上述方法从酸菜中提取的提取液，加入5mL氨性缓冲溶液、0.2g锌粉和0.4mL氯化镉溶液，锌粉和氯化镉质量比为1∶2，然后在振荡频率180转/min、50℃恒温水浴条件下振荡40min，过滤、定容后得溶液B，然后取10.00mL溶液B，再加入10.00mL浓度为0.06mol/L的溴酸钾溶液、3.00mL浓度为5×10-3mol/L的EDTA溶液和2.50mL浓度为0.5mol/L的H2SO4溶液，定容，待测样溶液C，将2.00mL步骤一制备的鲁米诺分析液和2.00mL待测样溶液A依次加入到瞬稳静态化学发光仪内测量，记录反应的发光峰信号，读取峰面积Y，然后将峰面积Y带入回归方程计算出X2，用(X2-X1)×1.232计算即得到硝酸盐的浓度；即完成了酸菜中硝酸盐和亚硝酸盐检测；其中步骤二和三所述的回归方程：当仪器参数选择为负高压为325V且5.74×107≤Y≤1.13×109时将Y带入Y＝4.66×106+1.08×109X，r＝0.9947，当仪器参数选择为负高压为300V且2.11×108≤Y≤1.14×109时将Y带入Y＝2.02×107+9.38×106X，r＝0.9930。Detect nitrate and nitrite in sauerkraut among the present invention and finish according to the following steps: one, the preparation of luminol analysis liquid: draw 7.5mL concentration and be 1 * 10 -3 mol/L luminol solution, use concentration Be 0.25mol/L NaOH solution constant volume to obtain luminol analysis solution; 2. Determination of nitrite: take 5.00mL of the extract extracted from pickled cabbage according to the above method, and then add 10.00mL concentration of 0.06mol/L Potassium bromate solution, 3.00 mL of ethylenediaminetetraacetic acid (EDTA) solution with a concentration of 5×10 -3 mol/L and 2.50 mL of H 2 SO 4 solution with a concentration of 0.5 mol/L, and constant volume to obtain sample solution A , add 2.00mL of the luminol analysis solution prepared in step 1 and 2.00mL of the sample solution A to be tested into the transient static chemiluminescence meter for measurement, record the luminescence peak signal of the reaction, read the peak area Y, and then calculate the peak area Y is brought into the regression equation to obtain the concentration X of nitrite; 3. The determination of nitrate: take 20mL of the extract extracted from sauerkraut by the above method, add 5mL of ammonia buffer solution, 0.2g of zinc powder and 0.4mL of chloride Cadmium solution, the mass ratio of zinc powder and cadmium chloride is 1:2, then shake for 40 minutes under the conditions of an oscillation frequency of 180 rpm and a constant temperature water bath at 50°C, filter and constant volume to obtain solution B, and then take 10.00mL of solution B, Then add 10.00mL of potassium bromate solution with a concentration of 0.06mol/L, 3.00mL of an EDTA solution with a concentration of 5× 10-3 mol/L, and 2.50mL of a H2SO4 solution with a concentration of 0.5mol/L, constant volume, and to be tested For the sample solution C, add 2.00mL of the luminol analysis solution prepared in step 1 and 2.00mL of the sample solution A to be tested into the transient static chemiluminescence instrument for measurement, record the luminescence peak signal of the reaction, read the peak area Y, and then Bring the peak area Y into the regression equation to calculate X 2 , and use (X 2 -X 1 )×1.232 to calculate the concentration of nitrate; that is, the detection of nitrate and nitrite in sauerkraut is completed; the second and third steps are The above regression equation: when the instrument parameter selection is negative high voltage 325V and 5.74×10 7 ≤Y≤1.13×10 9 , put Y into Y=4.66×10 6 +1.08×10 9 X, r=0.9947, when the instrument When the parameter selection is negative high voltage 300V and 2.11×10 8 ≤Y≤1.14×10 9 , Y is brought into Y=2.02×10 7 +9.38×10 6 X, r=0.9930.
上述检测方法利用锌-镉水浴振荡还原硝酸盐，硝酸盐还原率达到92.65％，检测方法具有工艺简单、耗时短(40min)、灵敏度高、线性范围宽、仪器设备简单优点。The above detection method uses zinc-cadmium water bath to reduce nitrate by oscillation, and the nitrate reduction rate reaches 92.65%. The detection method has the advantages of simple process, short time-consuming (40min), high sensitivity, wide linear range, and simple equipment.
具体实施方式Detailed ways
具体实施方式一：本实施方式中提取酸菜中硝酸盐和亚硝酸盐的方法是按下述步骤进行的：将酸菜绞碎，然后取1g经绞碎处理后的酸菜加入到2.5mL硼砂饱和溶液搅拌均匀，加入10mL蒸馏水，然后在微波加热提取5min，微波加热的温度为80℃，再加入1mL浓度为0.25mol/L的亚铁氰化钾溶液和1mL浓度为1mol/L的乙酸锌溶液，定容，静止过滤，收集滤液得到提取液；即完成酸菜中硝酸盐和亚硝酸盐提取。Specific embodiment one: the method for extracting nitrate and nitrite in sauerkraut in the present embodiment is carried out according to the following steps: sauerkraut is minced, then gets 1g and joins 2.5mL borax saturated solution through the sauerkraut after the minced processing Stir evenly, add 10mL of distilled water, then extract by microwave heating for 5min, the temperature of microwave heating is 80°C, then add 1mL of potassium ferrocyanide solution with a concentration of 0.25mol/L and 1mL of zinc acetate solution with a concentration of 1mol/L, Constant volume, static filtration, collecting the filtrate to obtain the extract; that is to complete the extraction of nitrate and nitrite in sauerkraut.
本实施方式中硝酸盐和亚硝酸盐提取率均在90％以上。测得提取酸菜中亚硝酸盐的含量为3.95mg/kg，与国标法(2.79mg/kg)相比，提高了41.6％。In this embodiment, the extraction rates of nitrate and nitrite are both above 90%. The measured content of nitrite in the extracted sauerkraut is 3.95mg/kg, which is 41.6% higher than the national standard method (2.79mg/kg).
具体实施方式二：本实施方式与具体实施方式一不同的是：所述绞碎酸菜的时间为2min，所用转速为1400r/min。Embodiment 2: This embodiment differs from Embodiment 1 in that: the time for grinding sauerkraut is 2 minutes, and the rotating speed used is 1400 r/min.
具体实施方式三：本实施方式中检测酸菜中硝酸盐和亚硝酸盐是按下述步骤完成的：一、鲁米诺分析液的制备：吸取7.5mL浓度为1×10-3mol/L鲁米诺溶液，用浓度为0.25mol/L的NaOH溶液定容50mL得到鲁米诺分析液；二、亚硝酸盐的测定：取5.00mL按具体实施方式一所述方法从酸菜中提取的提取液，然后加入10.00mL浓度为0.06mol/L的溴酸钾溶液、3.00mL浓度为5×10-3mol/L的乙二胺四乙酸(EDTA)溶液和2.50mL浓度为0.5mol/L的H2SO4溶液，定容50mL，得到待测样溶液A，将2.00mL步骤一制备的鲁米诺分析液和2.00mL待测样溶液A依次加入到瞬稳静态化学发光仪内测量，记录反应的发光峰信号，读取峰面积Y，然后将峰面积Y带入回归方程即得到亚硝酸盐的浓度X1；三、硝酸盐的测定：取20mL具体实施方式一所述方法从酸菜中提取的提取液，加入5mL氨性缓冲溶液、0.2g锌粉和0.4mL氯化镉溶液，锌粉和氯化镉质量比为1∶2，然后在振荡频率180转/min、50℃恒温水浴条件下振荡40min，过滤、定容50mL后得溶液B，然后取10.00mL溶液B，再加入10.00mL浓度为0.06mol/L的溴酸钾溶液、3.00mL浓度为5×10-3mol/L的EDTA溶液和2.50mL浓度为0.5mol/L的H2SO4溶液，定容50mL，待测样溶液C，将2.00mL步骤一制备的鲁米诺分析液和2.00mL待测样溶液A依次加入到瞬稳静态化学发光仪内测量，记录反应的发光峰信号，读取峰面积Y，然后将峰面积Y带入回归方程计算出X2，用(X2-X1)×1.232计算即得到硝酸盐的浓度；即完成了酸菜中硝酸盐和亚硝酸盐检测；其中步骤二和三所述的回归方程：当仪器参数选择为负高压为325V且5.74×107≤Y≤1.13×109时将Y带入Y＝4.66×106+1.08×109X，r＝0.9947，当仪器参数选择为负高压为300V且2.11×108≤Y≤1.14×109时将Y带入Y＝2.02×107+9.38×106X，r＝0.9930。Specific embodiment three: In this embodiment, the detection of nitrate and nitrite in sauerkraut is completed according to the following steps: 1. Preparation of luminol analysis solution: absorb 7.5mL concentration of 1 × 10 -3 mol/L Luminol Minol solution, be that the NaOH solution constant volume 50mL of 0.25mol/L obtains luminol analytical solution with concentration; , and then add 10.00 mL of 0.06 mol/L potassium bromate solution, 3.00 mL of 5×10 -3 mol/L ethylenediaminetetraacetic acid (EDTA) solution and 2.50 mL of 0.5 mol/L H 2 SO 4 solution, constant volume 50mL, to obtain the sample solution A to be tested, add 2.00mL of the luminol analysis solution prepared in step 1 and 2.00mL of the sample solution A to be tested in sequence in the transient static chemiluminescence instrument for measurement, and record the luminescence of the reaction Peak signal, read the peak area Y, and then bring the peak area Y into the regression equation to obtain the concentration X of nitrite; 3. The measurement of nitrate: take 20mL of the method described in the specific embodiment one to extract from sauerkraut solution, add 5mL of ammonia buffer solution, 0.2g of zinc powder and 0.4mL of cadmium chloride solution, the mass ratio of zinc powder and cadmium chloride is 1:2, and then oscillate under the conditions of an oscillation frequency of 180 rpm and a constant temperature water bath of 50°C After 40 minutes, filter and set the volume to 50mL to obtain solution B, then take 10.00mL of solution B, add 10.00mL of potassium bromate solution with a concentration of 0.06mol/L, 3.00mL of EDTA solution with a concentration of 5× 10-3 mol/L and 2.50 H 2 SO 4 solution with a concentration of 0.5 mol/L, constant volume 50mL, sample solution C to be tested, 2.00mL luminol analysis solution prepared in step 1 and 2.00mL sample solution A to be tested were added to the transient static Measure in the chemiluminescence instrument, record the luminescent peak signal of the reaction, read the peak area Y, then bring the peak area Y into the regression equation to calculate X 2 , and calculate the concentration of nitrate by (X 2 -X 1 )×1.232 ; That is, the detection of nitrate and nitrite in sauerkraut has been completed; the regression equation described in steps two and three: when the instrument parameter selection is that the negative high voltage is 325V and 5.74×10 7 ≤ Y ≤ 1.13×10 9 , the Y band Enter Y=4.66×10 6 +1.08×10 9 X, r=0.9947, when the instrument parameter selection is negative high voltage 300V and 2.11×10 8 ≤Y≤1.14×10 9 , put Y into Y=2.02×10 7 +9.38×10 6 X, r=0.9930.
该方法检测酸菜中亚硝酸盐的含量为2.84mg/kg，，11次平行测定结果的相对标准偏差为2.90％，加标回收率为101.00％，硝酸盐含量为7.32mg/kg。The method detects the content of nitrite in sauerkraut to be 2.84mg/kg, the relative standard deviation of 11 parallel determination results is 2.90%, the standard addition recovery rate is 101.00%, and the nitrate content is 7.32mg/kg.
通过下述试验验证本实施方式硝酸盐转化成亚硝酸盐的效果：取20mL硝酸盐标准溶液(溶液每毫升相当于5μg亚硝酸钠)于锥形瓶中，加入5mL氨性缓冲溶液(pH＝9.6～9.7)及固液比为1∶2的锌粉和(1.5％)氯化镉溶液，在温度50℃，振荡频率180转/min的条件下，振荡40min。计算硝酸盐还原率为92.65％，符合硝酸盐还原率应大于90％的要求。The effect that nitrate of this embodiment is converted into nitrite is verified by following test: get 20mL nitrate standard solution (per milliliter of solution is equivalent to 5 μ g sodium nitrite) in conical flask, add 5mL ammoniacal buffer solution (pH= 9.6-9.7) and zinc powder and (1.5%) cadmium chloride solution with a solid-liquid ratio of 1:2, oscillate for 40 minutes at a temperature of 50°C and an oscillation frequency of 180 rpm. The calculated nitrate reduction rate is 92.65%, meeting the requirement that the nitrate reduction rate should be greater than 90%.
本实施方式中回归方程可按下述方法获得：硫酸浓度为0.05mol/L，溴酸钾浓度为0.06mol/L，鲁米诺浓度为1.50×10-4mol/L、NaOH浓度为0.25mol/L条件下，该体系的相对发光强度最大。NO2 -浓度在0.001～0.1mg/L范围内，得到相应的亚硝酸盐标准曲线为Y＝4.66×106+1.08×109X(r＝0.9947)，NO2 -浓度在0.1～10mg/L范围内，得到相应的亚硝酸盐标准曲线为Y＝2.02×107+9.38×106X(r＝0.9930)。亚硝酸盐在0.001～10mg/L范围内与发光强度(面积)呈良好的线性关系。In this embodiment, the regression equation can be obtained as follows: the concentration of sulfuric acid is 0.05mol/L, the concentration of potassium bromate is 0.06mol/L, the concentration of luminol is 1.50× 10-4 mol/L, and the concentration of NaOH is 0.25mol/L Under these conditions, the relative luminous intensity of the system is the largest. The corresponding nitrite standard curve is Y=4.66×10 6 +1.08×10 9 X (r=0.9947 ) , and the NO 2 -concentration is in the range of 0.1～10mg/L. In the L range, the corresponding nitrite standard curve is Y=2.02×10 7 +9.38×10 6 X (r=0.9930). There is a good linear relationship between nitrite and luminous intensity (area) in the range of 0.001-10mg/L.
具体实施方式四：本实施方式与具体实施方式三不同的是：步骤三所述的氨性缓冲溶液的pH值＝9.6～9.7。其它步骤和参数与具体实施方式三相同。Embodiment 4: This embodiment differs from Embodiment 3 in that: the pH value of the ammoniacal buffer solution in Step 3 is 9.6-9.7. Other steps and parameters are the same as those in the third embodiment.
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| CN104330367B (en) * | 2013-11-19 | 2017-01-18 | 上海绿帝环保科技有限公司 | Rapid detection agent for nitrate |
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