CN113281287B - Pretreatment method for paper surface layer and method for determining saccharin sodium content in paper surface layer - Google Patents
Pretreatment method for paper surface layer and method for determining saccharin sodium content in paper surface layer Download PDFInfo
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- CN113281287B CN113281287B CN202110541369.3A CN202110541369A CN113281287B CN 113281287 B CN113281287 B CN 113281287B CN 202110541369 A CN202110541369 A CN 202110541369A CN 113281287 B CN113281287 B CN 113281287B
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- 239000002344 surface layer Substances 0.000 title claims abstract description 55
- FTLYMKDSHNWQKD-UHFFFAOYSA-N (2,4,5-trichlorophenyl)boronic acid Chemical compound OB(O)C1=CC(Cl)=C(Cl)C=C1Cl FTLYMKDSHNWQKD-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229940085605 saccharin sodium Drugs 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 45
- 238000002203 pretreatment Methods 0.000 title description 3
- FRPHFZCDPYBUAU-UHFFFAOYSA-N Bromocresolgreen Chemical compound CC1=C(Br)C(O)=C(Br)C=C1C1(C=2C(=C(Br)C(O)=C(Br)C=2)C)C2=CC=CC=C2S(=O)(=O)O1 FRPHFZCDPYBUAU-UHFFFAOYSA-N 0.000 claims abstract description 53
- 235000019504 cigarettes Nutrition 0.000 claims abstract description 46
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000006228 supernatant Substances 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 15
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001514 detection method Methods 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 238000007781 pre-processing Methods 0.000 claims abstract description 3
- 238000002835 absorbance Methods 0.000 claims description 10
- 239000007795 chemical reaction product Substances 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 7
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 238000010812 external standard method Methods 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 5
- 239000012498 ultrapure water Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 4
- 238000002798 spectrophotometry method Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 abstract description 15
- 239000000203 mixture Substances 0.000 abstract description 6
- 238000004458 analytical method Methods 0.000 abstract description 4
- 235000019605 sweet taste sensations Nutrition 0.000 abstract description 4
- 238000002791 soaking Methods 0.000 abstract 1
- 239000012086 standard solution Substances 0.000 description 24
- 239000012488 sample solution Substances 0.000 description 18
- 238000012360 testing method Methods 0.000 description 8
- 238000011084 recovery Methods 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 6
- 235000003599 food sweetener Nutrition 0.000 description 6
- 239000011550 stock solution Substances 0.000 description 6
- 239000003765 sweetening agent Substances 0.000 description 6
- 239000010413 mother solution Substances 0.000 description 5
- 238000000611 regression analysis Methods 0.000 description 4
- 238000004364 calculation method Methods 0.000 description 3
- 230000001419 dependent effect Effects 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 230000000391 smoking effect Effects 0.000 description 3
- 239000012085 test solution Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 241000208125 Nicotiana Species 0.000 description 2
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 2
- 238000002372 labelling Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000105 evaporative light scattering detection Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000001294 liquid chromatography-tandem mass spectrometry Methods 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
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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
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention belongs to the field of detection and analysis, and particularly relates to a method for preprocessing the surface layer of paper, which comprises the following steps: soaking the mixture in 2-10 mL water-methanol mixture solution of 500-1300 mm 2 Separating out liquid from the surface layer surface of the paper for 5-60 seconds; wherein the volume ratio of water to methanol in the water-methanol mixed solution is 1:3-10:3; centrifuging the liquid at a rotation speed of 500-3000 rpm for 1-10 minutes, and collecting supernatant; reacting the supernatant with bromocresol green solution; wherein the ratio of the supernatant to bromocresol green is 100L (0.01-0.3) mol. The invention also relates to a method for determining the sodium saccharin content in the surface layer of the paper. The method can rapidly and accurately measure the saccharin sodium content in the surface layer of the paper, so as to rapidly evaluate the influence of the paper (such as tipping paper for cigarettes) on the sweet taste, and is simple and convenient to operate.
Description
Technical Field
The invention belongs to the field of detection and analysis, and particularly relates to a method for pretreatment of a paper surface layer and a method for measuring the content of saccharin sodium in the paper surface layer.
Background
In recent years, with the change of cigarette consumer groups, consumer consumption tends to be more individual, and the demands of individuation and customization become stronger. Among them, the cigarette products in which sweetener is added to tipping paper for cigarettes are popular among consumers.
In order to evaluate the effect of sweetener in cigarette tipping paper on the taste of a cigarette for smoking, it is often necessary to determine the sodium saccharin content in the cigarette tipping paper. At present, the published literature mainly adopts a solvent to extract the sweetener contained in the whole tipping paper for cigarettes, and then the sweetener is detected by a high performance liquid chromatography attached evaporative light scattering detector or a high performance liquid chromatography-tandem mass spectrometry. However, the existing method has long detection time and complex operation steps, and cannot meet the requirement of on-site rapid analysis.
Disclosure of Invention
The inventors have surprisingly found that the sweetener which gives the consumer a sweet taste in smoking a cigarette is mainly distributed on the surface layer of the tipping paper for the cigarette (i.e. the outermost layer of the tipping paper for the cigarette after being rolled into a cigarette), and the sweetener in the tipping paper for the cigarette is not easy to permeate out and has an influence on the smoking taste. Therefore, one of the purposes of the present invention is to provide a method for pretreatment of the surface layer of paper, which comprises impregnating the surface layer of paper with a water-methanol mixture solution in a certain ratio, collecting the supernatant after centrifugation of the impregnating solution, and allowing the supernatant to react with bromocresol green solution for measurement; on the basis of the method, the reaction product obtained by the pretreatment method is detected by an ultraviolet spectrophotometer, so that the content of the saccharin sodium in the surface layer of the paper can be rapidly and accurately measured, the influence of the paper (such as tipping paper for cigarettes) on the sweet taste can be rapidly evaluated, and the operation is simple and convenient.
To achieve the above object, a first aspect of the present invention relates to a method for pretreating a surface layer of a paper sheet, comprising the steps of:
adopts 2-10 mL (for example, 4mL, 5mL,7 mL) of water-methanol mixed solution is immersed for 500-1300 mm 2 (e.g. 700mm 2 、800mm 2 、900mm 2 、1000mm 2 、1100mm 2 ) Separating out the liquid from the surface layer surface of the paper for 5-60 seconds (for example, 10, 20, 40, 50, 60 seconds); wherein the volume ratio of water to methanol in the water-methanol mixed solution is 1:3-10:3 (preferably 1:1-3:1, for example 2:3, 3:1, 8:3, 7:3, 3:2, 1:1, 1:1.3);
centrifuging the liquid at 500-3000 rpm (e.g. 1000rpm, 2000rpm, 2500 rpm) for 1-10 minutes (e.g. 2, 3, 4, 5, 6, 8 minutes) and collecting the supernatant;
reacting the supernatant with bromocresol green solution; wherein the ratio of supernatant to bromocresol green is 100L (0.01-0.3) mol, for example 100L:0.2mol, 100L:0.1mol, 100L:0.02mol, 100L:0.04mol.
A second aspect of the present invention relates to a method for pretreatment of the surface layer of paper, which employs a device for extracting sodium saccharin from the surface layer of paper, the device comprising a base, a cup, a locating pin, a cover and a connecting unit; wherein,,
a cavity with an open upper part is arranged in the base;
the upper part of the cup body is open and is positioned in the cavity of the base, and the inner cross section area of the cup body is 500-1300 mm 2 (e.g. 700mm 2 、800mm 2 、900mm 2 、1000mm 2 、1100mm 2 )；
The locating pin is arranged at the upper end of the base, and the upper end of the locating pin is flush with the upper end of the cup body;
the cover body is suitable for covering the open upper part of the cup body and the upper end of the positioning pin, and a sealing gasket is arranged at the inner side of the cover body;
the connecting unit comprises a fixing part arranged on the outer side wall of the base, a clamping ring and a protruding part arranged at the edge of the cover body, one end of the clamping ring is rotationally connected with the fixing part, the other end of the clamping ring is a free end, and the free end of the clamping ring is matched with the protruding part in size and is suitable for buckling and locking;
the method for preprocessing the surface layer of the paper comprises the following steps:
2-10 mL (for example, 3mL, 4mL, 5mL and 7 mL) of water-methanol mixed solution is filled in the cup body, paper is covered on the open upper part of the cup body (the surface layer of the paper faces the cup body) and is positioned by a positioning pin, the cover body is covered, and the cup body is sealed and locked by a connecting unit;
inverting the device for 5-60 seconds (such as 10, 20, 40, 50, 60 seconds) and then restoring to normal position, opening the cover body and removing the paper;
centrifuging the liquid in the cup body at 500-3000 rpm (e.g. 1000rpm, 2000rpm, 2500 rpm) for 1-10 min (e.g. 2, 3, 4, 5, 6, 8 min), collecting supernatant;
reacting the supernatant with bromocresol green solution; wherein the ratio of supernatant to bromocresol green is 100L (0.01-0.3) mol, for example 100L:0.2mol, 100L:0.1mol, 100L:0.02mol, 100L:0.04mol.
In some embodiments of the first or second aspects of the invention, the concentration of bromocresol green solution is from 10 to 200. Mu.M, for example 20. Mu.M, 30. Mu.M, 50. Mu.M, 70. Mu.M, 80. Mu.M, 100. Mu.M, 120. Mu.M, 150. Mu.M, 170. Mu.M.
In some embodiments of the first or second aspects of the invention, the solvent used for the bromocresol green solution is water, preferably ultrapure water.
In some embodiments of the first or second aspects of the invention, the paper is a tobacco paper, preferably a tobacco tipping paper.
In some embodiments of the second aspect of the invention, the depth of the cup in the device is at least 55mm, such as 55mm, 60mm, 70mm, 80mm, 100mm.
In some embodiments of the second aspect of the present invention, in the device, at least two cavities are provided in the base, and at least two cups are provided.
In some embodiments of the second aspect of the present invention, the two cavities are uniformly disposed along the length of the base.
In some embodiments of the second aspect of the invention, the device is configured such that there is a space between the bottom of the cup and the bottom of the chamber.
In some embodiments of the second aspect of the invention, the upper end of the cup is higher than the upper end of the chamber.
In some embodiments of the second aspect of the present invention, in the device, a pair of connection units are provided corresponding to each cup, and are provided at opposite sides of the cup for locking.
In some embodiments of the second aspect of the present invention, in the device, the positioning pins are arranged in pairs and are located between adjacent cavities.
In some embodiments of the second aspect of the present invention, the number of the positioning pins is two, the positioning pins are located between two adjacent cavities and are respectively located near two opposite sides of the base, and the distances between the positioning pins and the axes of the two adjacent cavities are equal.
In some embodiments of the second aspect of the present invention, in the device, an upper portion (upper end) of the cup body protrudes outward to form an annular hanging table, and an upper portion (upper end) of the inner cavity of the base expands outward to form an annular recess, and the annular hanging table is matched with the size of the annular recess.
In some embodiments of the second aspect of the present invention, in the device, an upper portion (upper end) of the base protrudes to both sides to form a carrying handle.
In some embodiments of the second aspect of the invention, the device wherein the base is sized to match the cover.
In some embodiments of the second aspect of the present invention, in the device, the cup body is cuboid, and a cross section of the cup body is square.
The third aspect of the invention relates to a method for determining the sodium saccharin content in the surface layer of paper, comprising the following steps:
pretreating the surface layer of the paper according to the method of the first or second aspect of the invention to obtain a reaction product;
detecting the reaction product by an ultraviolet spectrophotometer to obtain an ultraviolet spectrophotometry chart; wherein the width of the nip of the ultraviolet spectrophotometer is 1-2 nm (for example, 1 nm), and the detection range of the absorption wavelength is 300-800 nm (preferably 340-700 nm);
and calculating the saccharin sodium content in the surface layer of the paper according to absorbance data of the absorption wavelength of 441nm or 616nm in the ultraviolet spectroscope.
In some embodiments of the third aspect of the present invention, the paper is a cigarette paper, preferably a cigarette tipping paper.
In some embodiments of the third aspect of the invention, the sodium saccharin content in the surface layer of the paper is calculated using an external standard method.
In some embodiments of the third aspect of the present invention, the series of standard solutions used in the external standard method are formulated by the steps of: taking saccharin sodium standard solutions with different concentrations to react with bromocresol green solution respectively; the bromocresol green solution is as described in the first or second aspect of the invention.
In some embodiments of the third aspect of the present invention, the external standard method employs a series of standard solutions in a ratio of saccharin sodium standard solution to bromocresol green of 100L (0.01-0.3) mol, for example 100L:0.1mol, 100L:0.02mol, 100L:0.05mol.
In some embodiments of the third aspect of the present invention, the external standard method comprises:
detecting a series of standard solutions by an ultraviolet spectrophotometer (the operation conditions are consistent with those of detection of reaction products), carrying out regression analysis by taking the content of saccharin sodium and bromocresol green association in the series of standard solutions (based on the content of saccharin sodium) as an independent variable and taking absorbance data of absorption wavelength of 441nm or 616nm as an independent variable to obtain a standard working curve;
correspondingly, absorbance data of 441nm or 616nm in an ultraviolet spectroscope of the reaction product is substituted into a standard working curve for calculation, so that the content of saccharin sodium and bromocresol green association in the reaction product (calculated by the content of saccharin sodium) is obtained, and the content of saccharin sodium in the surface layer of the paper is further calculated.
In some embodiments of the third aspect of the invention, the ultraviolet spectrophotometer employs a 1.0cm quartz cuvette.
In the invention, the tipping paper for cigarettes is paper for cigarettes commonly used in the field, and accords with the specification of industry standard YC 171-2014 tipping paper for cigarettes.
In the present invention, the surface layer of the tipping paper for cigarettes refers to the outermost layer of the tipping paper for cigarettes after being rolled into cigarettes.
The invention achieves one or more of the following beneficial effects:
the method can rapidly and accurately measure the saccharin sodium content in the surface layer of the paper, so as to rapidly evaluate the influence of the paper (such as tipping paper for cigarettes) on the sweet taste, and has simple and convenient operation, and can meet the requirement of rapid on-site analysis.
Drawings
In order that the invention may be more readily understood, a more particular description of the invention will be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings, in which
FIG. 1 is a schematic view of one embodiment of the apparatus for extracting sodium saccharin from the surface layer of a sheet of paper according to the present invention;
FIG. 2 is a graph of standard operation in example 1;
FIG. 3 is an ultraviolet spectroscopic spectrum of the sample solutions of tipping paper samples 1 to 3 for cigarettes in example 1;
FIG. 4 is a graph of standard operation in example 3;
the novel portable cup comprises a 1-base, a 2-cup body, a 3-locating pin, a 4-cover body, a 5-1-fixing part, a 5-2-clamping ring, a 5-3 protruding part, a 6-cavity, a 7-sealing gasket, an 8-annular hanging table, a 9-annular recess and a 10-lifting handle.
Detailed Description
Embodiments of the present invention will now be described more fully hereinafter with reference to the accompanying examples, in which it is shown, however, that the examples are shown, and in which the invention is practiced. The following description of at least one exemplary embodiment is merely exemplary in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
FIG. 1 is a schematic view of one embodiment of the apparatus for extracting sodium saccharin from the surface layer of a sheet of paper according to the present invention;
the device for extracting saccharin sodium from the surface layer of the paper comprises a base 1, a cup body 2, a locating pin 3, a cover body 4 and a connecting unit;
a cavity 6 with an open upper part is arranged in the base 1;
the upper part of the cup body 2 is open and is positioned in the cavity 6 of the base 1, and the inner cross section area of the cup body 2 is 900mm 2 ；
The locating pin 3 is arranged at the upper end of the base 1, and the upper end of the locating pin 3 is flush with the upper end of the cup body 2;
the cover body 4 is suitable for covering the open upper part of the cup body 2 and the upper end of the positioning pin 3, and a sealing gasket 7 is arranged on the inner side of the cover body 4;
the connecting unit comprises a fixed part 5-1 arranged on the outer side wall of the base 1, a clamping ring 5-2 and a protruding part 5-3 arranged at the edge of the cover body 4, one end of the clamping ring 5-2 is rotationally connected with the fixed part 5-1, the other end is a free end, and the free end of the clamping ring 5-2 is matched with the protruding part 5-3 in size and is suitable for buckling and locking;
in this embodiment, two cavities 6 are provided in the base 1, and two cup bodies 2 are provided;
in this embodiment, the two cavities 6 are uniformly arranged along the length direction of the base 1;
in this embodiment, the depth of the cup body 2 is 55mm;
in the embodiment, a space is reserved between the bottom of the cup body 2 and the bottom of the cavity 6;
in this embodiment, the upper end of the cup body 2 is higher than the upper end of the cavity 6;
in the present embodiment, a pair of (two) connecting units are provided corresponding to each cup 2, provided on opposite sides of the cup 2 for locking;
in this embodiment, the positioning pins 3 are arranged in pairs, the number of the positioning pins is two, the positioning pins are located between two adjacent cavities 6 and are respectively arranged near two opposite sides of the base 1, and the distances between the positioning pins 3 and the axes of the two adjacent cavities 6 are equal;
in this embodiment, the upper portion (or upper end) of the cup body 2 protrudes outwards to form an annular hanging table 8, and the upper portion (or upper end) of the inner cavity 6 in the base 1 expands outwards to form an annular recess 9, and the annular hanging table 8 is matched with the annular recess 9 in size;
in this embodiment, the upper part (or upper end) of the base 1 protrudes to two sides to form a handle 10, and the base 1 is matched with the cover 4 in size.
In this embodiment, the cup body 2 is rectangular, and the cross section of the cup body 2 is square.
In this embodiment, the height of the positioning pin 3 is 10mm.
Example 1
(1) Preparing a series of standard solutions:
accurately weighing 0.1g (accurate to 0.1 mg) of saccharin sodium, dissolving with a small amount of pure water, transferring into a 100mL brown volumetric flask, and fixing the volume of saccharin sodium stock solution with pure water to 1 mg/mL. Accurately transferring 2mL of saccharin sodium stock solution into a 100mL brown volumetric flask, and fixing the standard solution mother solution with 200 mug/mL of pure water. Transferring 0.1mL, 0.2mL, 0.5mL, 1.0mL, 4.0mL, 5.0mL and 10.0mL of standard solution mother liquor into different 100mL brown volumetric flasks, and fixing the volume by pure water to obtain serial solutions with the concentration of 0.2 mug/mL, 0.4 mug/mL, 1.0 mug/mL, 2.0 mug/mL, 8.0 mug/mL, 10.0 mug/mL and 20.0 mug/mL respectively; 100. Mu.L of each solution was precisely removed and added to 2.0mL of 50. Mu.M bromocresol green (BCG) indicator (bromocresol green aqueous solution), and shaken well to obtain a series of standard solutions.
(2) Preparing a test solution:
adopting the device shown in fig. 1, filling 5.0mL of water-methanol mixed solution (the volume ratio of water to methanol is 7:3) in a cup body, covering paper on the open upper part of the cup body (the surface layer of the paper faces the cup body), positioning the paper by a positioning pin, covering the cover body, sealing by a connecting unit and buckling a locking device; then the device is inverted for 20 seconds, the forward placement is resumed, the cover body is opened, the paper is removed, 4.0mL of liquid in the cup body is taken and placed in a centrifuge tube, the centrifuge tube is centrifuged for 2 minutes at the rotation speed of 2000r/min, 100 mu L of supernatant liquid is accurately removed and added into 2.0mL of 50 mu M bromocresol green (BCG) indicator (bromocresol green aqueous solution), and the solution is uniformly shaken, thus obtaining the solution of the test sample.
(3) And (3) detection:
respectively filling a series of standard solutions and sample solutions into 1.0cm quartz cuvettes, and measuring by an ultraviolet spectrophotometer (PerkinElmer Lambda) under the following operation conditions: the slit width is 1nm, the wavelength detection range is 340-700 nm, and the blank control is ultrapure water.
Regression analysis was performed with the content of association of saccharin sodium and bromocresol green (based on the content of saccharin sodium) in the series of standard solutions as independent variable, and absorbance at 616nm as dependent variable, as shown in fig. 2, and the standard working curve obtained was: y=0.0711x+0.4237.
Substituting absorbance of the sample solution at 616nm wavelength into a standard working curve for calculation to obtain the content of saccharin sodium and bromocresol green association in the sample solution (calculated by saccharin sodium content), and further calculating the saccharin sodium content of the surface layer of the tipping paper for the cigarette.
The saccharin sodium content of the surface layer of three kinds of tipping papers for cigarettes was measured in the above-described manner, and the results are shown in table 1. The ultraviolet spectroscopic spectra of the sample solutions corresponding to the three cigarette tipping papers are shown in figure 3.
Table 1 determination of sodium saccharin content in the surface layers of tipping papers 1-3 for cigarettes
Example 2
(1) Preparing a series of standard solutions:
accurately weighing 0.1g (accurate to 0.1 mg) of saccharin sodium, dissolving with a small amount of pure water, transferring into a 100mL brown volumetric flask, and fixing the volume of saccharin sodium stock solution with pure water to 1 mg/mL. Accurately transferring 2mL of saccharin sodium stock solution into a 100mL brown volumetric flask, and fixing the standard solution mother solution with 200 mug/mL of pure water. The mother solution of the standard solution of 0.1mL, 0.2mL, 0.5mL, 1.0mL, 4.0mL, 5.0mL and 10.0mL is respectively transferred to different 100mL brown volumetric flasks, pure water is used for constant volume, so as to obtain a series of solutions with the concentration of 0.2 mug/mL, 0.4 mug/mL, 1.0 mug/mL, 2.0 mug/mL, 8.0 mug/mL, 10.0 mug/mL and 20.0 mug/mL, 200 mug of each solution is accurately transferred and respectively added into a 50 mug bromocresol green (BCG) indicator (bromocresol green water solution) of 2.0mL, and the mixture is uniformly shaken, so as to obtain a series of standard solutions.
(2) Preparing a test solution:
adopting the device shown in fig. 1, filling 5mL of water-methanol mixed solution (the volume ratio of water to methanol is 6:4) in a cup body, covering paper on the open upper part of the cup body (the surface layer of the paper faces the cup body), positioning the paper by a positioning pin, covering the cover body, sealing by a connecting unit, and buckling a locking device; then the device is inverted for 20 seconds, the cover body is opened, the paper is removed, 4mL of liquid in the cup body is taken and placed in a centrifuge tube, the centrifuge tube is centrifuged for 2 minutes at the rotation speed of 2000r/min, 200 mu L of supernatant fluid is accurately removed and added into 2mL of 20 mu M bromocresol green (BCG) indicator (bromocresol green aqueous solution), and the mixture is uniformly shaken, so as to obtain a sample solution.
(3) And (3) detection:
respectively filling a series of standard solutions and sample solutions into 1.0cm quartz cuvettes, and measuring by an ultraviolet spectrophotometer (PerkinElmer Lambda) under the following operation conditions: the slit width is 1nm, the wavelength detection range is 340-700 nm, and the blank control is ultrapure water.
And carrying out regression analysis by taking the content of saccharin sodium and bromocresol green association compound (based on the content of saccharin sodium) in a series of standard solutions as independent variables and taking absorbance at 616nm wavelength as dependent variable to obtain a standard working curve.
Substituting absorbance of the sample solution at 616nm wavelength into a standard working curve for calculation to obtain the content of saccharin sodium and bromocresol green association in the sample solution (calculated by saccharin sodium content), and further calculating the saccharin sodium content of the surface layer of the tipping paper for the cigarette.
The saccharin sodium content of the surface layers of the tipping papers 4 to 6 for cigarettes was measured in the manner described above, and the results are shown in Table 2.
Table 2 determination of sodium saccharin content in the surface layers of tipping papers 4-6 for cigarettes
Example 3
(1) Preparing a series of standard solutions:
accurately weighing 0.1g (accurate to 0.1 mg) of saccharin sodium, dissolving with a small amount of pure water, transferring into a 100mL brown volumetric flask, and fixing the volume of saccharin sodium stock solution with pure water to 1 mg/mL. Accurately transferring 2mL of saccharin sodium stock solution into a 100mL brown volumetric flask, and fixing the standard solution mother solution with 200 mug/mL of pure water. The mother solution of the standard solution of 0.1mL, 0.2mL, 0.5mL, 1.0mL, 4.0mL, 5.0mL and 10.0mL is respectively transferred to different 100mL brown volumetric flasks, pure water is used for constant volume, so as to obtain a series of solutions with the concentration of 0.2 mug/mL, 0.4 mug/mL, 1.0 mug/mL, 2.0 mug/mL, 8.0 mug/mL, 10.0 mug/mL and 20.0 mug/mL, 500 mug of each solution is accurately transferred and respectively added into a 50 mug bromocresol green (BCG) indicator (bromocresol green water solution) of 2.0mL, and the mixture is uniformly shaken, so as to obtain a series of standard solutions.
(2) Preparing a test solution:
adopting the device shown in fig. 1, filling 5mL of water-methanol mixed solution (the volume ratio of water to methanol is 5:5) in a cup body, covering paper on the open upper part of the cup body (the surface layer of the paper faces the cup body), positioning the paper by a positioning pin, covering the cover body, sealing by a connecting unit, and buckling a locking device; then the device is inverted for 20 seconds, the forward placement is resumed, the cover body is opened, the paper is removed, 4mL of liquid in the cup body is taken and placed in a centrifuge tube, the centrifuge tube is centrifuged for 2 minutes at the rotation speed of 2000r/min, 500 mu L of supernatant liquid is accurately removed and added into 2.0mL of 100 mu M bromocresol green (BCG) indicator (bromocresol green aqueous solution), and the solution is uniformly shaken, thus obtaining the solution of the test sample.
(3) And (3) detection:
respectively filling a series of standard solutions and sample solutions into 1.0cm quartz cuvettes, and measuring by an ultraviolet spectrophotometer (PerkinElmer Lambda) under the following operation conditions: the slit width is 1nm, the wavelength detection range is 340-700 nm, and the blank control is ultrapure water.
Regression analysis was performed with the content of sodium saccharin and bromocresol green association (based on sodium saccharin content) in the series of standard solutions as independent variable and the absorbance at 441nm wavelength as dependent variable, to obtain a standard working curve y= -0.0266x+0.7563, as shown in fig. 4.
Substituting absorbance of the sample solution at 441nm wavelength into a standard working curve to calculate, so as to obtain the content of saccharin sodium and bromocresol green association in the sample solution (calculated by the content of saccharin sodium), and further calculating the content of saccharin sodium on the surface layer of the tipping paper for the cigarette.
The saccharin sodium content of the surface layers of the tipping papers for cigarettes 7 to 9 was measured in the manner described above, and the results are shown in Table 3.
Table 3 results of measuring saccharin sodium content on the surface layers of tipping papers 7 to 9 for cigarettes
Test example 1 accuracy verification
The surface layer and the interior of the tipping paper 10-12 for cigarettes are known to contain saccharin sodium, and the designed value of the saccharin sodium content in the surface layer (ink layer) of the tipping paper 10-12 for cigarettes is 25.0mg/m respectively 2 、22.0mg/m 2 、30.0mg/m 2 。
The surface saccharin sodium content of the cigarette tipping papers 10-12 was measured by the method of example 1, and the results are shown in Table 4.
TABLE 4 actual measurement of saccharin sodium content on the surface of tipping papers for cigarettes 10-12 and comparison of the design value
As can be seen from Table 4, the surface saccharin sodium content of the tipping paper for cigarettes, which is determined by the method of the invention, is relatively close to the designed value of the surface saccharin sodium content, which indicates that the method of the invention can accurately determine the saccharin sodium content of the surface of the tipping paper for cigarettes.
Test example 2 method for labeled recovery and repeatability
1) Example 1 method:
in the (2) of the embodiment 1, 5.0mL of water-methanol mixed solution (the volume ratio of water to methanol is 7:3) is filled in each of the plurality of cup bodies, then saccharin sodium standard substances are respectively added into the plurality of cup bodies according to the addition amount of 0.4 mug/mL, 2.0 mug/mL and 10.0 mug/mL, and are uniformly mixed, and then the surface layer of the tipping paper 3 for cigarettes in the embodiment 1 faces the cup bodies and covers the open upper part of the cup bodies, positions paper by a positioning pin, covers the cover bodies, seals by a connecting unit and locks a locking device; then inverting the device for 20 seconds, then restoring to be placed in the forward direction, opening the cover body, removing paper, taking 4mL of liquid in the cup body, putting the liquid into a centrifuge tube, centrifuging for 2 minutes at a rotating speed of 2000r/min, accurately moving 100 mu L of supernatant, adding the supernatant into 2.0mL of 50 mu M bromocresol green (BCG) indicator (bromocresol green aqueous solution), and shaking uniformly to obtain a plurality of labeled test sample solutions; the content of the association of saccharin sodium and bromocresol green in the labeled test sample solution (calculated as saccharin sodium content) was then determined as in item (3) of example 1, and the labeled recovery was further calculated, and each concentration was measured 3 times in parallel, and the results are shown in table 5. The background value represents the content of sodium saccharin and bromocresol green association (calculated as sodium saccharin content) in the sample solution obtained during the measurement of sodium saccharin on the surface layer of the tipping paper 3 for cigarettes by the method of example 1.
Table 5 method of labeling recovery and repeatability
As shown in Table 5, the standard recovery rate of the method is between 85.7 and 91.3 percent, and the Relative Standard Deviation (RSD) of parallel samples is less than 5.6 percent, which indicates that the determination method has high accuracy, good repeatability and stable and reliable result.
2) Example 3 method:
in example 3, in item (2), 5mL of water-methanol mixed solution (the volume ratio of water to methanol is 5:5) is filled in each of a plurality of cup bodies, then saccharin sodium standard substances are respectively added into the plurality of cup bodies according to the addition standard quantity of 0.4 mug/mL, 2.0 mug/mL and 10.0 mug/mL, and then the surface layer of the tipping paper 9 for cigarettes in example 3 is covered on the open upper part of the cup body towards the cup body, the paper is positioned by a positioning pin, the cover body is covered, and the locking device is sealed and buckled by a connecting unit; then inverting the device for 20 seconds, then restoring to be placed in the forward direction, opening the cover body, removing paper, taking 4mL of liquid in the cup body, putting the liquid into a centrifuge tube, centrifuging for 2 minutes at a rotating speed of 2000r/min, accurately moving 500 mu L of supernatant, adding the 500 mu L of supernatant into 2.0mL of 100 mu M bromocresol green (BCG) indicator (bromocresol green aqueous solution), and shaking uniformly to obtain a plurality of labeled test sample solutions; the content of sodium saccharin and bromocresol green association (calculated as sodium saccharin content) in the labeled test sample solution was then determined as in example 3 item (3), and the labeled recovery was further calculated, and each concentration was measured 3 times in parallel, and the results are shown in table 6. The background value represents the content of sodium saccharin and bromocresol green association (calculated as sodium saccharin content) in the sample solution obtained during the determination of sodium saccharin on the surface layer of the tipping paper 9 for cigarettes by the method of example 3.
Table 6 method of labeling recovery and repeatability
As shown in Table 6, the standard recovery rate of the method is 88.1-94.8%, the Relative Standard Deviation (RSD) of parallel samples is less than 5.1%, and the method is high in accuracy, good in repeatability and stable and reliable in result.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (13)
1. A method for pretreatment of a surface layer of paper, which adopts a device for extracting saccharin sodium from the surface layer of paper, wherein the device comprises a base, a cup body, a locating pin, a cover body and a connecting unit; wherein,,
a cavity with an open upper part is arranged in the base;
the upper part of the cup bodyThe cup body is opened and positioned in the cavity of the base, and the inner cross section area of the cup body is 500-1300 mm 2 ；
The locating pin is arranged at the upper end of the base, and the upper end of the locating pin is flush with the upper end of the cup body;
the cover body is suitable for covering the open upper part of the cup body and the upper end of the positioning pin, and a sealing gasket is arranged at the inner side of the cover body;
the connecting unit comprises a fixing part arranged on the outer side wall of the base, a clamping ring and a protruding part arranged at the edge of the cover body, one end of the clamping ring is rotationally connected with the fixing part, the other end of the clamping ring is a free end, and the free end of the clamping ring is matched with the protruding part in size and is suitable for buckling and locking;
the method for preprocessing the surface layer of the paper comprises the following steps:
2-10 mL of water-methanol mixed solution is filled in the cup body, paper is covered on the open upper part of the cup body and positioned by a positioning pin, the cover body is covered, and the cup body is sealed and locked by the connecting unit; wherein the volume ratio of water to methanol in the water-methanol mixed solution is 1:3-10:3;
inverting the device for 5-60 seconds, then restoring to be placed in the forward direction, opening the cover body, and removing paper;
taking liquid in the cup body, centrifuging at a rotating speed of 500-3000 rpm for 1-10 minutes, and collecting supernatant;
reacting the supernatant with bromocresol green solution; wherein the ratio of the supernatant to bromocresol green is 100L (0.01-0.3) mol.
2. The method according to claim 1, wherein the concentration of bromocresol green solution is 10 to 200 μm.
3. The method of claim 1, wherein the solvent used for the bromocresol green solution is water.
4. The method according to claim 1, wherein the solvent used for the bromocresol green solution is ultrapure water.
5. The method of claim 1, wherein the paper is a cigarette paper.
6. The method of claim 1, wherein the paper is tipping paper for cigarettes.
7. The method of claim 1, wherein at least two cavities are provided in the base and at least two cups are provided in the device.
8. The method of claim 1, wherein a pair of connection units is provided for each cup in the device.
9. The method of claim 1, wherein the alignment pins are provided in pairs and between adjacent cavities in the device.
10. The method of claim 1, wherein in the device, the upper portion of the cup body protrudes outward to form an annular hanging table, the upper portion of the inner cavity in the base expands outward to form an annular recess, and the annular hanging table is matched with the size of the annular recess.
11. A method for determining the sodium saccharin content of a paper surface layer comprising:
pretreatment of the surface layer of paper according to the method of any one of claims 1 to 10 to obtain a reaction product;
detecting the reaction product by an ultraviolet spectrophotometer to obtain an ultraviolet spectrophotometry chart; wherein the width of the crack of the ultraviolet spectrophotometer is 1-2 nm, and the detection range of the absorption wavelength is 300-800 nm;
and calculating the saccharin sodium content in the surface layer of the paper according to absorbance data of the absorption wavelength of 441nm or 616nm in the ultraviolet spectroscope.
12. The method of claim 11, wherein the sodium saccharin content in the paper surface layer is calculated using an external standard method.
13. The method of claim 11 or 12, wherein the ultraviolet spectrophotometer employs a 1.0cm quartz cuvette.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102084248A (en) * | 2008-07-07 | 2011-06-01 | 杭州迪图科技有限公司 | Detection device for fluid sample |
| CN103323548A (en) * | 2013-06-08 | 2013-09-25 | 国家烟草质量监督检验中心 | Measurement method for residual amount of pentachlorophenol in cigarette paper |
| CN110763797A (en) * | 2019-11-12 | 2020-02-07 | 河南中烟工业有限责任公司 | Method for measuring sweetening agent for cigarettes by high performance liquid chromatography |
| CN210119487U (en) * | 2019-04-02 | 2020-02-28 | 赵建雄 | Detection household utensils that food safety inspection used |
| CN210631015U (en) * | 2019-06-25 | 2020-05-29 | 广东东方麦田工业设计股份有限公司 | Disposable tea making cup |
| CN111871474A (en) * | 2020-07-23 | 2020-11-03 | 杭州博拓生物科技股份有限公司 | Detachable detection device |
| CN111912817A (en) * | 2020-09-03 | 2020-11-10 | 福建中烟工业有限责任公司 | Pretreatment method and device, and method and system for measuring content of saccharin sodium in paper |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11234682B2 (en) * | 2018-09-28 | 2022-02-01 | Zhejiang Orient Gene Biotech Co., Ltd. | Apparatus for detecting analyte in a liquid sample |
-
2021
- 2021-05-18 CN CN202110541369.3A patent/CN113281287B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102084248A (en) * | 2008-07-07 | 2011-06-01 | 杭州迪图科技有限公司 | Detection device for fluid sample |
| CN103323548A (en) * | 2013-06-08 | 2013-09-25 | 国家烟草质量监督检验中心 | Measurement method for residual amount of pentachlorophenol in cigarette paper |
| CN210119487U (en) * | 2019-04-02 | 2020-02-28 | 赵建雄 | Detection household utensils that food safety inspection used |
| CN210631015U (en) * | 2019-06-25 | 2020-05-29 | 广东东方麦田工业设计股份有限公司 | Disposable tea making cup |
| CN110763797A (en) * | 2019-11-12 | 2020-02-07 | 河南中烟工业有限责任公司 | Method for measuring sweetening agent for cigarettes by high performance liquid chromatography |
| CN111871474A (en) * | 2020-07-23 | 2020-11-03 | 杭州博拓生物科技股份有限公司 | Detachable detection device |
| CN111912817A (en) * | 2020-09-03 | 2020-11-10 | 福建中烟工业有限责任公司 | Pretreatment method and device, and method and system for measuring content of saccharin sodium in paper |
Non-Patent Citations (1)
| Title |
|---|
| 紫外分光光度法测定饮料中糖精钠的含量;宗水珍等;常熟理工学院学报;第29卷(第4期);68-71 * |
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