CN113281288A - Pretreatment method of tipping paper for cigarettes and method for measuring saccharin sodium in tipping paper for cigarettes - Google Patents
Pretreatment method of tipping paper for cigarettes and method for measuring saccharin sodium in tipping paper for cigarettes Download PDFInfo
- Publication number
- CN113281288A CN113281288A CN202110541375.9A CN202110541375A CN113281288A CN 113281288 A CN113281288 A CN 113281288A CN 202110541375 A CN202110541375 A CN 202110541375A CN 113281288 A CN113281288 A CN 113281288A
- Authority
- CN
- China
- Prior art keywords
- tipping paper
- cigarettes
- saccharin sodium
- water
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 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 57
- 229940085605 saccharin sodium Drugs 0.000 title claims abstract description 57
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 47
- 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 42
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 17
- 239000006228 supernatant Substances 0.000 claims abstract description 15
- 238000001514 detection method Methods 0.000 claims abstract description 14
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 11
- 239000012498 ultrapure water Substances 0.000 claims description 11
- 238000002835 absorbance Methods 0.000 claims description 10
- 239000007795 chemical reaction product Substances 0.000 claims description 8
- 238000002386 leaching Methods 0.000 claims description 6
- 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
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 22
- 239000012086 standard solution Substances 0.000 description 19
- 239000012085 test solution Substances 0.000 description 13
- 239000011550 stock solution Substances 0.000 description 9
- 235000003599 food sweetener Nutrition 0.000 description 8
- 239000003765 sweetening agent Substances 0.000 description 8
- 235000013305 food Nutrition 0.000 description 7
- 238000005259 measurement Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000004364 calculation method Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 230000001419 dependent effect Effects 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000000611 regression analysis Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000005022 packaging material Substances 0.000 description 3
- 239000012488 sample solution Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- UDIPTWFVPPPURJ-UHFFFAOYSA-M Cyclamate Chemical compound [Na+].[O-]S(=O)(=O)NC1CCCCC1 UDIPTWFVPPPURJ-UHFFFAOYSA-M 0.000 description 1
- 241000208125 Nicotiana Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000625 cyclamic acid and its Na and Ca salt Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 239000005003 food packaging material Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- 238000001294 liquid chromatography-tandem mass spectrometry Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229960001462 sodium cyclamate Drugs 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 235000019605 sweet taste sensations Nutrition 0.000 description 1
- 238000004885 tandem mass spectrometry Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 235000021404 traditional food Nutrition 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
Images
Classifications
-
- 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
Abstract
The invention belongs to the field of detection and analysis, and particularly relates to a method for pretreating tipping paper for cigarettes, which comprises the following steps: extracting a tipping paper sample for cigarettes by adopting a water-methanol mixed solution, and separating an extracting solution; wherein the volume ratio of water to methanol in the water-methanol mixed solution is 2: 3-10: 3, and 60-300 mL of the water-methanol mixed solution is adopted per gram of sample; centrifuging the extracting solution at the rotating speed of 500-3000 rpm for 1-10 minutes, and collecting supernatant; reacting the supernatant with a bromocresol green solution; wherein the proportion of the supernatant to the bromocresol green is 100L (0.01-0.3) mol. The invention also relates to a method for measuring the content of saccharin sodium in tipping paper for cigarettes. The method can quickly and accurately measure the content of saccharin sodium in the tipping paper for cigarettes.
Description
Technical Field
The invention belongs to the field of detection and analysis, and particularly relates to a method for pretreating tipping paper for cigarettes, and also relates to a method for measuring the content of saccharin sodium in the tipping paper for cigarettes.
Background
The sweetener belongs to common food additives and mainly has the functions of giving sweet taste and improving food quality. With the development of the food industry, the pursuit for green and safe foods is increasing, and ensuring food safety is becoming a key point. At present, the food industry has strict requirements on green, safety and the like, and the detection and analysis of the sweetener content of food is one of the requirements. All countries adopt strict restriction policies on sweetening agents such as saccharin sodium, sodium cyclamate and the like, set a large number of standards, and become the key points of international trade and domestic production investigation.
Compared with the traditional food packaging material, the paper packaging material has many advantages, so the occupation ratio of the paper packaging material is steadily increased year by year. In order to improve the taste and enrich the characteristic aroma, some food manufacturers add sweeteners to paper packaging materials to ensure that the sweeteners are not easily volatilized or attenuated, for example, the tobacco industry adds sweeteners to commonly used tipping paper for cigarettes. The existing sweetener determination methods comprise ion chromatography, liquid chromatography tandem mass spectrometry, gas chromatography tandem mass spectrometry and the like, but the methods cannot rapidly and accurately determine the content of the sweetener in the tipping paper for cigarettes.
Disclosure of Invention
The invention aims at providing a method for pretreating tipping paper for cigarettes, which comprises the steps of extracting the tipping paper for the cigarettes by adopting water-methanol mixed solution in a certain proportion, centrifuging the extract, collecting supernatant, and reacting the supernatant with bromocresol green solution for detection; on the basis, the invention further aims to provide a method for measuring the content of the saccharin sodium in the tipping paper for the cigarettes, which can quickly and accurately measure the content of the saccharin sodium in the tipping paper for the cigarettes by detecting a reaction product obtained by a pretreatment method by using an ultraviolet spectrophotometer.
In order to achieve the above object, a first aspect of the present invention relates to a method for pretreating tipping paper for cigarettes, comprising the following steps:
extracting a tipping paper sample for cigarettes by adopting a water-methanol mixed solution, and separating an extracting solution; wherein, the volume ratio of water to methanol in the water-methanol mixed solution is 2: 3-10: 3 (preferably 1: 1-3: 1, such as 3:1, 8:3, 7:3, 3:2, 1:1, 1:1.3), and 60-300 mL (such as 80mL, 100mL, 110mL, 120mL, 130mL, 150mL, 170mL, 200mL, 230mL, 250mL, 280mL) of water-methanol mixed solution is adopted per gram of sample;
centrifuging the extract at 500-3000 rpm (such as 1000rpm, 2000rpm, 2500rpm) for 1-10 min (such as 2, 3, 4, 5, 6, 8 min), and collecting supernatant;
reacting the supernatant with a bromocresol green solution; wherein the ratio of the supernatant to the bromocresol green is 100L (0.01-0.3) mol, such as 100L:0.1mol, 100L:0.02mol, 100L:0.04 mol.
In some embodiments of the first aspect of the present invention, the leaching is under sonication conditions.
In some embodiments of the first aspect of the present invention, the ultrasonic power is 1300 to 2000W, for example 1500W.
In some embodiments of the first aspect of the present invention, the ultrasound frequency is 40 to 60Hz, for example 50 Hz.
In some embodiments of the first aspect of the present invention, the leaching is for more than 5 minutes.
In some embodiments of the first aspect of the present invention, the leaching is for 5 to 100 minutes, preferably for 5 to 60 minutes, such as 10 minutes, 20 minutes, 30 minutes.
In some embodiments of the first aspect of the present invention, the concentration of the bromocresol green solution is 10 to 200. mu.M, such as 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 aspect of the present invention, the solvent used for the bromocresol green solution is water, preferably ultrapure water.
The invention relates to a method for measuring the content of saccharin sodium in tipping paper for cigarettes, which comprises the following steps:
pretreating a tipping paper sample for cigarettes according to the method of the first aspect of the invention to obtain a reaction product;
detecting the reaction product by using an ultraviolet spectrophotometer to obtain an ultraviolet spectrophotometer; wherein the width of the crack of the ultraviolet spectrophotometer is 1-2 nm (such as 1nm), and the detection range of the absorption wavelength is 300-800 nm (preferably 350-700 nm);
and calculating the content of saccharin sodium in the tipping paper sample for the cigarette according to the absorbance data of the absorption wavelength of 441nm or 616nm in the ultraviolet spectrography.
In some embodiments of the second aspect of the present invention, the sodium saccharin content of the sample of tipping paper for cigarettes is calculated using an external standard method.
In some embodiments of the second aspect of the present invention, the series of standard solutions used in the external standard method is prepared by the following steps: taking saccharin sodium standard solutions with different concentrations to respectively react with a bromocresol green solution; wherein the ratio of the sodium saccharin standard solution to the bromocresol green is equal to the ratio of the supernatant to the bromocresol green in the method according to the first aspect of the invention; the bromocresol green solution is as described in the first aspect of the invention.
In some embodiments of the second aspect of the present invention, in the preparation steps of the series of standard solutions used in the external standard method, the ratio of the saccharin sodium standard solution to the bromocresol green is 100L (0.01-0.3) mol, for example, 100L:0.1mol, 100L:0.02mol, and 100L:0.04 mol.
In some embodiments of the second aspect of the present invention, the external standard method comprises:
detecting a series of standard solutions (the operation condition is consistent with that of reaction product detection) by adopting an ultraviolet spectrophotometer, performing regression analysis by taking the content of saccharin sodium and bromocresol green association (calculated by saccharin sodium content) in the series of standard solutions as independent variables and taking absorbance data of absorption wavelength of 441nm or 616nm as dependent variables to obtain a standard working curve;
correspondingly, substituting the absorbance data of 441nm or 616nm in the ultraviolet spectrography of the reaction product into a standard working curve for calculation to obtain the content (calculated by the content of saccharin sodium) of the saccharin sodium and bromocresol green association in the reaction product, and further calculating the content of saccharin sodium in the tipping paper sample for the cigarette.
In some embodiments of the second aspect of the present invention, the ultraviolet spectrophotometer employs a 1.0cm quartz cuvette.
In some embodiments of the second aspect of the present invention, the uv spectrophotometer is a PerkinElmer Lambda 35 uv spectrophotometer.
In the invention, the cigarette tipping paper is the cigarette paper commonly used in the field and meets the regulation of the industry standard YC 171-.
The invention has the following beneficial effects:
the method can quickly and accurately measure the content of saccharin sodium in the tipping paper for cigarettes.
Drawings
In order that the present disclosure may be more readily and clearly understood, reference is now made to the following detailed description of the embodiments of the present disclosure taken in conjunction with the accompanying drawings, in which
FIG. 1 is a standard operating curve for example 1;
FIG. 2 is an ultraviolet spectroscopy chart of tipping paper samples No. 1 to No. 3 for cigarette in example 1;
FIG. 3 is a standard operating curve for example 3.
Detailed Description
Embodiments of the present invention will now be described more fully hereinafter with reference to the accompanying examples, in which some, but not all embodiments of the invention are shown. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Preparing a series of standard solutions:
taking a saccharin sodium standard substance, and adding ultrapure water to prepare stock solution with the concentration of 8.0 mg/mL; taking 0.0mL, 0.1mL, 0.2mL, 0.3mL, 0.4mL and 0.5mL of stock solutions, adding the stock solutions into different 100mL volumetric flasks, performing constant volume with ultrapure water to obtain a series of solutions with saccharin sodium concentration of 0.000mg/mL, 0.008mg/mL, 0.016mg/mL, 0.024mg/mL, 0.032mg/mL and 0.04mg/mL respectively, accurately transferring 100 mu L of each solution, adding the solution into different 2mL of 50 mu M bromcresol green (BCG) indicators (aqueous bromcresol green solutions), and shaking up to obtain a series of standard solutions.
(2) Preparation of a test solution:
weighing 0.1g (accurate to 0.0001g) of tipping paper sample for cigarettes, placing the tipping paper sample in a 50mL triangular conical flask, adding 10mL of water-methanol mixed solution (the volume ratio of water to methanol is 7:3), extracting for 10min under the ultrasonic condition, wherein the ultrasonic power is 1500W, and the ultrasonic frequency is 50 HZ; and (3) putting 5mL of extract into a centrifuge tube, centrifuging for 2min at the rotating speed of 2000r/min, accurately transferring 100 mu L of supernatant, adding into 2mL of 50 mu M bromocresol green (BCG) indicator (bromocresol green aqueous solution), and shaking up to obtain a test solution.
(3) And (3) detection:
the series of standard solutions and the sample solution are respectively put into a 1.0cm quartz cuvette and measured by an ultraviolet spectrophotometer (Perkinelmer Lambda 35) under the following operating conditions: the width of the slit is 1nm, the wavelength detection range is 350-700 nm, and the blank control is ultrapure water.
Regression analysis was performed with the concentration of saccharin sodium and bromocresol green associate (in terms of saccharin sodium concentration) in the series of standard solutions as independent variables and the absorbance at a wavelength of 616nm as dependent variables, as shown in fig. 1, and the obtained standard working curve was: y 0.40828+ B1 x + B2 x2B1-4.02763 and B2-111.84738 (R2 is 0.99923).
And substituting the absorbance of the test solution at the wavelength of 616nm into a standard working curve for calculation to obtain the concentration (by a saccharin sodium concentration meter) of the saccharin sodium and bromocresol green association compound in the test solution, and further calculating the saccharin sodium content in the tipping paper sample for the cigarette.
The content of saccharin sodium in tipping paper samples 1# to 3# for the cigarette is measured according to the method, and the saccharin sodium content is measured in parallel for 5 times, and the result is shown in table 1. The ultraviolet spectrograms of the tipping paper samples for cigarettes are shown in figure 2.
TABLE 1 cigarette tipping paper sample No. 1-3 saccharin sodium content determination results
As can be seen from Table 1, the method of the present invention has a small deviation of the parallel measurement, which indicates that the method of the present invention has good reproducibility.
Example 2
(1) Preparing a series of standard solutions:
taking a saccharin sodium standard substance, and adding ultrapure water to prepare stock solution with the concentration of 8.0 mg/mL; taking 0.0mL, 0.1mL, 0.2mL, 0.3mL, 0.4mL and 0.5mL of stock solutions, adding the stock solutions into different 100mL volumetric flasks, diluting to constant volume with an ultrapure water solvent to obtain a series of solutions with saccharin sodium concentration of 0.000mg/mL, 0.008mg/mL, 0.016mg/mL, 0.024mg/mL, 0.032mg/mL and 0.04mg/mL respectively, precisely transferring 200 mu L of each solution, adding the solution into different 2mL of 20 mu M bromcresol green (BCG) indicators (aqueous bromcresol green solutions), and shaking up to obtain a series of standard solutions.
(2) Preparation of a test solution:
weighing 0.2g (accurate to 0.0001g) of tipping paper sample for cigarettes, placing the tipping paper sample in a 50mL triangular conical flask, adding 20mL of water-methanol mixed solution (the volume ratio of water to methanol is 6:4), extracting for 20min under the condition of ultrasonic addition, wherein the ultrasonic power is 1500W, and the ultrasonic frequency is 50 HZ; and (3) putting 5mL of extract into a centrifuge tube, centrifuging for 2min at the rotating speed of 2000r/min, accurately transferring 200 mu L of supernatant, adding into 2mL of 20 mu M bromocresol green (BCG) indicator (bromocresol green aqueous solution), and shaking up to obtain a test solution.
(3) And (3) detection:
the series of standard solutions and the sample solution are respectively put into a 1.0cm quartz cuvette and measured by an ultraviolet spectrophotometer (Perkinelmer Lambda 35) under the following operating conditions: the width of the slit is 1nm, the wavelength detection range is 350-700 nm, and the blank control is ultrapure water.
And (3) performing regression analysis by taking the concentration (in terms of saccharin sodium concentration) of the saccharin sodium and bromocresol green association compound in the series of standard solutions as an independent variable and the absorbance at the wavelength of 616nm as a dependent variable to obtain a standard working curve.
And substituting the absorbance of the test solution at the wavelength of 616nm into a standard working curve for calculation to obtain the concentration (by a saccharin sodium concentration meter) of the saccharin sodium and bromocresol green association compound in the test solution, and further calculating the saccharin sodium content in the tipping paper sample for the cigarette.
The content of saccharin sodium in tipping paper samples 4# to 6# for the cigarettes is measured according to the method, and the saccharin sodium content is measured in parallel for 5 times, and the result is shown in table 2.
TABLE 2 saccharin sodium content determination results for tipping paper samples 4# to 6# for cigarettes
As can be seen from Table 2, the method of the present invention has a small deviation of the parallel measurement, which indicates that the method of the present invention has good reproducibility.
Example 3
(1) Preparing a series of standard solutions:
taking a saccharin sodium standard substance, and adding ultrapure water to prepare stock solution with the concentration of 8.0 mg/mL; taking 0.0mL, 0.1mL, 0.2mL, 0.3mL, 0.4mL and 0.5mL of stock solutions, adding the stock solutions into different 100mL volumetric flasks, performing constant volume with ultrapure water to obtain a series of solutions with saccharin sodium concentration of 0.000mg/mL, 0.008mg/mL, 0.016mg/mL, 0.024mg/mL, 0.032mg/mL and 0.04mg/mL respectively, precisely transferring 500 mu L of each solution, adding the solution into different 2mL of 100 mu M bromcresol green (BCG) indicator (aqueous bromcresol green solution), and shaking up to obtain a series of standard solutions.
(2) Preparation of a test solution:
weighing 0.3g (accurate to 0.0001g) of tipping paper sample for cigarettes, placing the tipping paper sample in a 50mL triangular conical flask, adding 40mL of water-methanol mixed solution (the volume ratio of water to methanol is 5:5), extracting for 30min under the condition of ultrasonic addition, wherein the ultrasonic power is 1500W, and the ultrasonic frequency is 50 HZ; and (3) putting 5mL of extract into a centrifuge tube, centrifuging for 2min at the rotating speed of 2000r/min, accurately transferring 500 mu L of supernatant, adding into 2mL of 100 mu M bromocresol green (BCG) indicator (bromocresol green aqueous solution), and shaking up to obtain a test solution.
(3) And (3) detection:
the series of standard solutions and the sample solution are respectively put into a 1.0cm quartz cuvette and measured by an ultraviolet spectrophotometer (Perkinelmer Lambda 35) under the following operating conditions: the width of the slit is 1nm, the wavelength detection range is 350-700 nm, and the blank control is ultrapure water.
Regression analysis was performed with the concentration of saccharin sodium and bromocresol green associate (in terms of saccharin sodium concentration) in the series of standard solutions as independent variables and the absorbance at 441nm as dependent variables, as shown in fig. 3, and the obtained standard working curve was: y 0.76228-7.78221 x (R2 is 0.999).
And substituting the absorbance of the test solution at the wavelength of 441nm into a standard working curve for calculation to obtain the concentration (by a saccharin sodium concentration meter) of the saccharin sodium and bromocresol green association compound in the test solution, and further calculating the saccharin sodium content in the tipping paper sample for the cigarette.
The content of saccharin sodium in tipping paper samples 7# to 9# for cigarettes is measured according to the method and is measured in parallel for 5 times, and the result is shown in table 3.
TABLE 3 saccharin sodium content determination results for tipping paper samples 7# -9 # for cigarettes
As can be seen from Table 3, the method of the present invention has a small deviation of the parallel measurement, which indicates that the method of the present invention has good reproducibility.
Examination of test example accuracy
(1) Example 1 accuracy study of the method:
adding three scalar saccharin sodium standard substances into tipping paper samples 1# to 3# for the cigarette in the embodiment 1 respectively to obtain a plurality of standard adding samples; the saccharin sodium content in each standard-added sample was measured according to the method of example 1, and then the standard-added recovery rate was calculated using the average saccharin sodium content measured in parallel for tipping paper samples 1# to 3# in table 1 as the background content, with the results shown in table 4.
TABLE 4 paper sample No. 1-3 normalized recovery results
(2) Example 3 accuracy study of the method:
adding three scalar saccharin sodium standard substances into tipping paper samples 7# to 9# for the cigarette in embodiment 3 respectively to obtain a plurality of standard adding samples; the saccharin sodium content in each standard-added sample was determined according to the method of example 3, and then the standard-added recovery rate was calculated using the average of the saccharin sodium contents determined in parallel for tipping paper samples 7# to 9# for cigarettes in table 3 as the background content, with the results shown in table 5.
TABLE 5 paper sample 7# to 9# normalized recovery results
As can be seen from tables 4-5, the recovery rate of the spiked standard of the method of the invention is 97% -102%, which meets the detection requirement, and the method of the invention has high determination accuracy.
Comparative example
When the test solution was prepared, 10mL of water was added to a conical flask containing a sample of tipping paper for cigarettes, and extraction was carried out for 10min under ultrasonic conditions with an ultrasonic power of 1500W and an ultrasonic frequency of 50HZ, the remainder being the same as in example 1. The saccharin sodium content of cigarette tipping paper samples 1# to 3# was also determined according to this method and the results are shown in table 6 (5 replicates).
Table 6 paper sample 1# to 3# saccharin sodium content determination results
As can be seen from Table 6, the RSD measured in parallel by the comparative example method is more than 5%, and the deviation is large, which indicates that the repeatability measured by the comparative example method is poor; moreover, the measurement result of the comparative example method is greatly different from the measurement result of example 1 with high accuracy, indicating that the measurement accuracy of the comparative example method is low.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A method for pretreating tipping paper for cigarettes comprises the following steps:
extracting a tipping paper sample for cigarettes by adopting a water-methanol mixed solution, and separating an extracting solution; wherein the volume ratio of water to methanol in the water-methanol mixed solution is 2: 3-10: 3, and 60-300 mL of the water-methanol mixed solution is adopted per gram of sample;
centrifuging the extracting solution at the rotating speed of 500-3000 rpm for 1-10 minutes, and collecting supernatant;
reacting the supernatant with a bromocresol green solution; wherein the proportion of the supernatant to the bromocresol green is 100L (0.01-0.3) mol.
2. The process of claim 1, wherein leaching is under ultrasonic conditions.
3. The method of claim 2, wherein the ultrasonic power is 1300-2000W, such as 1500W.
4. The method according to claim 2, wherein the ultrasound frequency is 40-60 HZ, such as 50 HZ.
5. The process of claim 1, wherein leaching is for more than 5 minutes;
preferably, leaching is carried out for 5-100 minutes.
6. The method according to any one of claims 1 to 5, wherein the concentration of the bromocresol green solution is 10 to 200 μ M.
7. A process according to any one of claims 1 to 6, wherein the solvent used for the bromocresol green solution is water, preferably ultrapure water.
8. A method for measuring the content of saccharin sodium in tipping paper for cigarettes comprises the following steps:
pretreating a sample of tipping paper for cigarettes according to the method of any one of claims 1 to 7 to obtain a reaction product;
detecting the reaction product by using an ultraviolet spectrophotometer to obtain an ultraviolet spectrophotometer; wherein the width of a crack of the ultraviolet spectrophotometer is 1-2 nm, and the detection range of the absorption wavelength is 300-800 nm;
and calculating the content of saccharin sodium in the tipping paper sample for the cigarette according to the absorbance data of the absorption wavelength of 441nm or 616nm in the ultraviolet spectrography.
9. A method according to claim 8 wherein the sodium saccharin content of the sample of tipping paper for cigarettes is calculated using an external standard method.
10. The method of claim 8, wherein the ultraviolet spectrophotometer employs a 1.0cm quartz cuvette.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110541375.9A CN113281288A (en) | 2021-05-18 | 2021-05-18 | Pretreatment method of tipping paper for cigarettes and method for measuring saccharin sodium in tipping paper for cigarettes |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110541375.9A CN113281288A (en) | 2021-05-18 | 2021-05-18 | Pretreatment method of tipping paper for cigarettes and method for measuring saccharin sodium in tipping paper for cigarettes |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113281288A true CN113281288A (en) | 2021-08-20 |
Family
ID=77279764
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110541375.9A Pending CN113281288A (en) | 2021-05-18 | 2021-05-18 | Pretreatment method of tipping paper for cigarettes and method for measuring saccharin sodium in tipping paper for cigarettes |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113281288A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114858936A (en) * | 2022-04-20 | 2022-08-05 | 江苏中烟工业有限责任公司 | Method for measuring transferable saccharin sodium in printing surface of tipping paper for cigarette |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103115994A (en) * | 2013-01-31 | 2013-05-22 | 广东中烟工业有限责任公司 | Method for rapidly measuring Cr(III) and Cr(VI) ion in tipping paper for cigarette |
| CN103175914A (en) * | 2013-02-07 | 2013-06-26 | 广东中烟工业有限责任公司 | Quantitative determination method for toluylene type fluorescent whitening agent APC in cigarette paper |
| CN108614053A (en) * | 2016-12-09 | 2018-10-02 | 内蒙古蒙牛乳业（集团）股份有限公司 | The quick detection of preservative and sweetener in butter or cream |
| 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 |
| 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 |
| US20210000159A1 (en) * | 2018-04-04 | 2021-01-07 | Japan Tobacco Inc. | Oral tobacco product, method for manufacturing packaging material for oral tobacco product, and method for manufacturing oral tobacco product |
-
2021
- 2021-05-18 CN CN202110541375.9A patent/CN113281288A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103115994A (en) * | 2013-01-31 | 2013-05-22 | 广东中烟工业有限责任公司 | Method for rapidly measuring Cr(III) and Cr(VI) ion in tipping paper for cigarette |
| CN103175914A (en) * | 2013-02-07 | 2013-06-26 | 广东中烟工业有限责任公司 | Quantitative determination method for toluylene type fluorescent whitening agent APC in cigarette paper |
| CN108614053A (en) * | 2016-12-09 | 2018-10-02 | 内蒙古蒙牛乳业（集团）股份有限公司 | The quick detection of preservative and sweetener in butter or cream |
| US20210000159A1 (en) * | 2018-04-04 | 2021-01-07 | Japan Tobacco Inc. | Oral tobacco product, method for manufacturing packaging material for oral tobacco product, and method for manufacturing oral tobacco product |
| 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 |
| 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 (4)
| Title |
|---|
| H. FARSAM等: "Spectrophotometric determination of meperidine hydrochloride in pharmaceutical preparations by complexation with bromocresol green", 《LOUMAL OF PHARMACEUTICAL & BIOMEDICAL ANALYSIS 》, vol. 2, no. 3, pages 543 - 547 * |
| 宣亚文等: "分光光度法快速测定食品中糖精钠含量", 《PTCA 理化检验－化学分册》, vol. 46, pages 57 - 61 * |
| 张树权等: "超高效液相色谱-串联质谱法同时检测糕点中 6 种甜味剂", 《食品安全质量检测学报》, vol. 12, no. 1, pages 145 - 146 * |
| 陈丽娟等: "超高效液相色谱－高分辨质谱法测定蜂蜜中的苯甲酸、山梨酸、安赛蜜与糖精钠", 《分析测试学报》, vol. 35, no. 9, pages 1143 - 1309 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114858936A (en) * | 2022-04-20 | 2022-08-05 | 江苏中烟工业有限责任公司 | Method for measuring transferable saccharin sodium in printing surface of tipping paper for cigarette |
| CN114858936B (en) * | 2022-04-20 | 2023-10-17 | 江苏中烟工业有限责任公司 | Method for measuring movable saccharin sodium in printing surface of tipping paper for cigarettes |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108956840B (en) | Method for detecting 5 sweetening agents in electronic cigarette liquid through ultra-high performance liquid chromatography-tandem mass spectrometry | |
| WO2019223372A1 (en) | Method for detecting melamine | |
| CN106324144A (en) | Method for detecting chlorate, perchlorate and bromate from milk powder and infant formula milk powder by hydrophilic interaction chromatography-tandem mass spectrometry | |
| Amjadi et al. | Ionic liquid-based, single-drop microextraction for preconcentration of cobalt before its determination by electrothermal atomic absorption spectrometry | |
| CN108387663B (en) | Method for detecting content of phthalic anhydride in toy by using gas chromatography-mass spectrometry | |
| CN101852786B (en) | Method for detecting sulfur dioxide content in shitake mushrooms | |
| CN113281288A (en) | Pretreatment method of tipping paper for cigarettes and method for measuring saccharin sodium in tipping paper for cigarettes | |
| Agatonović-Kuštrin et al. | Spectrophotometric study of diclofenac-Fe (III) complex | |
| Zbinden et al. | Determination of trace element contaminants in food matrices using a robust, routine analytical method for ICP-MS | |
| CN101393180B (en) | Method for measuring beta-naphthol content in additive agent for cigarette | |
| CN106093235B (en) | It is a kind of for measuring the extract liquor and its application method of moisture and nicotine content in cigarette mainstream flue gas | |
| CN109030654A (en) | The method and application of low molecule chlorinatedorganic in a kind of quick detection mthod of white water from paper making | |
| CN111650189A (en) | Method for measuring content of formaldehyde in special slice for cigarette without burning during heating | |
| CN111257452A (en) | Method for detecting synthetic acetic acid added in Zhenjiang aromatic vinegar | |
| CN108107132B (en) | Method for detecting total content of phenol in leather and leather products thereof | |
| CN108508100B (en) | Method for simultaneously measuring contents of Li +, Na +, NH4+, K +, Mg2+ and Ca2+ in reconstituted tobacco | |
| Inés Toral et al. | Simultaneous determination of o-and p-nitrophenol by first derivative spectrophotometry | |
| CN111257449A (en) | Method for determining stable hydrogen isotope ratio of acetic acid methyl sites in vinegar beverage | |
| CN115266983B (en) | Method for measuring antifungal drugs in antibacterial agent of antibacterial product by using gas chromatography mass spectrometry | |
| CN110927088A (en) | Method for rapidly detecting anthocyanin in lycium ruthenicum murr | |
| CN109406429A (en) | A method of the atomic absorption spectroscopy determination content of heavy metal lead without matrix modifier | |
| CN114705648A (en) | Method for detecting antioxidant BHT in edible oil by using ultraviolet spectrophotometer | |
| CN112858533B (en) | Method for measuring plastid pigment content in tobacco shreds | |
| CN113281287A (en) | Paper surface layer pretreatment method and method for measuring content of saccharin sodium in paper surface layer | |
| CN113030333B (en) | Method for measuring plastid pigment content in tobacco shreds |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |