CN114858936B - Method for measuring movable saccharin sodium in printing surface of tipping paper for cigarettes - Google Patents
Method for measuring movable saccharin sodium in printing surface of tipping paper for cigarettes Download PDFInfo
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Abstract
The invention discloses a method for measuring movable saccharin sodium in a printing surface of tipping paper for cigarettes, which comprises the steps of placing two tipping paper printing surfaces between two food plastic packaging films for plastic packaging after face-to-face lamination, cooling to room temperature after plastic packaging is finished, and taking a middle part by using a cutting knife to form two parallel samples with back plastic packaging; placing the prepared back plastic sealed paper sample into a headspace bottle containing artificial saliva, sealing, immediately placing the headspace bottle into a water bath for migration experiments after sealing, rapidly taking out the headspace bottle from the water bath after the migration experiments are finished, shaking uniformly to obtain migration liquid, passing the migration liquid through a 0.22 mu m water-based filter membrane, and collecting filtrate for standby detection; and (5) performing machine test on the obtained filtrate, and quantitatively calculating the content of the effective saccharin sodium in the tipping paper by using an external standard method. The invention realizes the single-sided transferable saccharin sodium content detection of the printing surface of the tipping paper, and the sample pretreatment is simple and quick.
Description
Technical field:
the invention relates to a method for measuring movable saccharin sodium in a printing surface of tipping paper for cigarettes.
The background technology is as follows:
compared with the traditional food packaging material, the paper packaging material has the advantages of low cost, good processing performance, good printing performance and the like, so that the occupation ratio of the paper packaging material in the packaging material is steadily increased year by year. Sweeteners are a type of food additive capable of improving mouthfeel, enriching characteristic aroma and imparting sweetness, and some food manufacturers print the sweetener on the surface of paper packaging materials to form products with unique styles, for example, some enterprises add the sweetener to common tipping paper for cigarettes, so that the sweetener is favored by some consumers.
The amount of the sweetener content has a certain correlation with sweetness in the sense, and the existing sweetener content measuring method comprises an ion chromatography, a liquid chromatography tandem mass spectrometry, a gas chromatography tandem mass spectrometry and the like, and the methods are extracted in a soaking mode and then quantified, so that the total sweetener content of the front side and the back side of the tipping paper is obtained. The tipping paper containing the sweetener is usually curled into a roll when stored, so that the printing surface of the tipping paper is closely contacted with the back surface of the adjacent tipping paper, the concentration difference of the sweetener is generated between the printing surface of the tipping paper and the back surface of the adjacent tipping paper, and the sweetener can migrate, namely from the printing surface to the adjacent back surface. In actual production, only the sweetener on the printed side of the tipping paper contacts the consumer's mouth to produce sweetness, while the sweetener that migrates to the back side does not produce a sweetness effect. Therefore, the existing detection technology cannot solve the problem that the sweetness intensity and the detection content of some products are inconsistent in actual work.
The invention comprises the following steps:
the invention provides a method for measuring movable saccharin sodium in a printing surface of tipping paper for cigarettes, which aims to solve the problems in the prior art.
The invention adopts the technical scheme that:
a method for measuring the transferable saccharin sodium in the printing surface of the tipping paper for cigarettes comprises the following steps:
1) Placing two printed surfaces of tipping paper between two plastic packaging films for plastic packaging after face-to-face lamination, cooling to room temperature after plastic packaging is completed, and then taking the middle part by using a cutting knife to form two parallel samples with plastic packaged back surfaces;
2) Placing the prepared back plastic sealed paper sample into a headspace bottle containing artificial saliva, sealing, immediately placing the headspace bottle into a water bath for migration experiments after sealing, rapidly taking out the headspace bottle from the water bath after the migration experiments are finished, shaking uniformly to obtain migration liquid, passing the migration liquid through a 0.22 mu m water-based filter membrane, and collecting filtrate for standby detection;
3) And (3) performing machine test on the filtrate obtained in the step (2), and quantitatively calculating the content of the effective saccharin sodium in the tipping paper by using an external standard method.
Further, the test solution adopted in the step 3) during the power-on test is as follows: the mobile phase was formed by dissolving 0.154g of ammonia acetate in 1L of acetonitrile-water solution, wherein the volume ratio of acetonitrile-water was 1:9.
Further, the on-machine test in the step 3) adopts a liquid chromatograph under the analysis conditions that a chromatographic column is HC-C18, the column temperature is 30 ℃, and the flow rate of a mobile phase is 1.0mL ∙ min -1 The sample injection amount is 2 mu L, and the detection wavelength is 230nm.
Further, before placing the headspace bottle in the tipping paper sample in the step 2), placing the artificial saliva in the headspace bottle in a water bath kettle at 40 ℃ for balancing for 20-30 min.
Further, in the migration experiment in the step 2), the migration condition is that the temperature is 40 ℃ and the time is 5-10 min.
Further, the volume of the artificial saliva adopted by the tipping paper sample per square centimeter is 0.5-2 mL, and the tipping paper sample is completely soaked in the artificial saliva during a migration experiment.
Further, the quantitative process of the external standard method in the step 3) is as follows: preparing saccharin sodium standard solutions with different gradients, and respectively detecting the prepared standard solutions with different gradients by using a liquid chromatograph to obtain corresponding response values of saccharin sodium in each standard solution; and (3) taking the concentration of saccharin sodium in each standard solution as an abscissa and the response value as an ordinate, and manufacturing to obtain a standard curve equation.
Further, the calculating process of the effective saccharin sodium content of the tipping paper in the step 3) comprises the following steps:
the measured response value of the saccharin sodium in the filtrate is brought into the standard curve equation to obtain the content of the saccharin sodium in the filtrate, and the obtained content of the saccharin sodium is brought into the equation x=c×v/S to obtain the content of the movable saccharin sodium in the printing surface of the back plastic packaging paper sample;
wherein x is the content of the transferable saccharin sodium in the printing surface of the tipping paper sample, and the unit is milligrams per square meter;
c is the concentration of saccharin sodium in the migration solution; units are milligrams per milliliter;
v is the volume of the migration liquid; the unit is milliliter;
s is the cutting area of the tipping paper sample, and the unit is square meters.
Further, in the step 2), the prepared back plastic seal packaging paper sample seal surface is curled outwards through tweezers, and then the back plastic seal packaging paper sample seal surface is placed in a cylindrical headspace bottle; the tweezers comprise a tweezers body, a rotating rod and a paper winding clamp, wherein the tweezers body comprises two tweezers handles which are integrally formed, the tail end of one of the tweezers handles extends downwards vertically to form tweezers, a vertically arranged through hole is formed in the other tweezers handle, the rotating rod is inserted into the through hole, the bottom end of the rotating rod is fixedly connected with the paper winding clamp, a paper clamping groove which is vertically arranged is formed in the paper winding clamp, and the lower port of the paper clamping groove extends on the lower end face of the paper winding clamp all the time.
Further, after the printed surfaces of the two tipping papers are bonded face to face, the two tipping papers are placed between two food plastic packaging films for plastic packaging, the number of times of plastic packaging is two, and the temperature of the first plastic packaging and the temperature of the second plastic packaging are both 130-140 ℃.
The invention has the following beneficial effects:
1. the single-sided transferable saccharin sodium content detection of the printing surface of the tipping paper is realized.
2. The sample pretreatment is simple and quick.
3. The test of precision, repeatability, detection limit, quantitative limit and recovery rate of the detection method proves that the method is scientific and effective.
4. When the butt joint paper is curled, the paper clamping groove in the paper winding clamp is spliced on the tipping paper, then two forceps handles are oppositely nipped, the forceps feet are abutted against the paper winding clamp, the paper clamping groove is contracted, and then the rotating rod is rotated by hand, so that the butt joint paper can be curled. The whole crimping process, the hand is not in direct contact with paper, the hand impurity adhesion is effectively avoided on tipping paper, the structural design is ingenious, the manufacture is convenient, and the use effect is good.
Description of the drawings:
fig. 1 is a schematic cutting view of a single-sided seal tipping paper in an embodiment.
Fig. 2 is a liquid chromatogram for detecting sodium saccharin in a tipping paper.
Fig. 3 is a diagram showing the structure of forceps for curling a sheet of tipping paper.
Fig. 4 is an exploded view of the forceps of fig. 3.
The specific embodiment is as follows:
the invention is further described below with reference to the accompanying drawings.
Mobile phase preparation: respectively taking 200mL of acetonitrile and 1800mL of ultrapure water, uniformly mixing in a beaker to prepare acetonitrile-water solution, accurately weighing 0.154 ammonia acetate in a 1L volumetric flask, dissolving with the acetonitrile-water solution, and fixing the volume to a scale to form a mobile phase.
Chromatographic conditions: the liquid chromatograph adopts an Agilent1260 and DAD detector, the chromatographic column adopts an H-C18 column, and the column temperature is 30 ℃; the mobile phase is 0.154g/L of ammonium acetate buffer salt, acetonitrile and water which are mixed according to the volume ratio of 1:9, and the mixed solution is eluted in an isocratic way; the flow rate of the mobile phase is 1 mL/min -1 The method comprises the steps of carrying out a first treatment on the surface of the The single sample injection amount is 2 mu L; detection waveThe length was 230nm.
And (3) manufacturing a standard curve: precisely removing a certain volume of sodium saccharin dihydrate standard solution, diluting with ultrapure water, and preparing into 0.002mg ∙ L respectively -1 、0.004mg∙L -1 、0.006mg∙L -1 、0.008mg∙L -1 、0.010mg∙L -1 、0.012mg∙L -1 Standard solutions of the X series. Detecting the standard solution by using a liquid chromatograph to obtain a corresponding response value of saccharin sodium in the standard solution; and (3) taking the concentration of saccharin sodium in the standard solution as an abscissa and the response value as an ordinate, and manufacturing to obtain a standard curve equation.
The reagents acetonitrile and ammonium acetate used were all analytically pure, from Shanghai's national institute of metrology science, inc., saccharin sodium standard solution (1000 μg ∙ mL).
The calculation method of the content of saccharin sodium comprises the following steps: the measured response value of the saccharin sodium is brought into a standard curve equation to obtain content, and the content of the movable saccharin sodium in the printing surface of the tipping paper for the cigarette can be obtained by bringing the content obtained by the measured response value of the saccharin sodium into the equation x=c×v/S; wherein x is the content of the transferable saccharin sodium in the sample printing surface, and the unit is milligrams per square meter; c is the concentration of saccharin sodium in the migration solution; units are milligrams per milliliter; v is the volume of the migration liquid; the unit is milliliter; s is the cutting area of the sample, and the unit is square meter.
Example 1
1) Sample seal treatment: and taking two pieces of tipping paper, attaching the printing surfaces of the tipping paper face to face, and then placing the tipping paper between two pieces of food plastic packaging films for plastic packaging. And (3) cooling the sealed tipping paper to room temperature by a plastic sealing machine again, and cutting the area of the middle area of the tipping paper with the size of 1cm multiplied by 10cm, as shown in figure 1, so as to prepare two tipping paper samples with back seals.
The printed surfaces of the two tipping papers are bonded face to face and then placed between the two food plastic packaging films for plastic packaging, the times of plastic packaging are two times, and the temperature of the first plastic packaging and the temperature of the second plastic packaging are both 130-140 ℃. And the lamination effect is ensured by adopting twice plastic packaging.
2) Sample migration treatment: taking a certain amount of artificial saliva into a beaker, placing the beaker into a water bath kettle at 40 ℃ and balancing for 30min. The prepared tipping paper sample seal surface is curled outwards, and is respectively placed in a 20mL headspace bottle, 10mL of balanced artificial saliva is added, the bottle is capped, and the bottle is immediately placed in a water bath kettle at 40 ℃ for 10min, and then is rapidly taken out and shaken uniformly. The migration solution is rapidly filtered by a microporous filter membrane with the diameter of 0.22 mu m, and the filtrate is collected for standby detection.
3) Detection and analysis: the filtrate is detected and analyzed by high performance liquid chromatography to obtain the response value of the liquid chromatography of the target object in the filtrate, and fig. 2 is a liquid chromatography chart for detecting saccharin sodium in a certain tipping paper. And carrying the detected response value into a standard curve equation, obtaining the content of saccharin sodium in the filtrate, and converting the content of the movable saccharin sodium in the printing surface of the tipping paper for the cigarette by using the formula.
Comparative example 1
(1) Sample seal treatment: and (3) taking two pieces of tipping paper, attaching the back sides of the printing surfaces of the tipping paper, and placing the tipping paper between two pieces of food plastic packaging films for plastic packaging. And (3) cooling the sealed tipping paper to room temperature by a plastic sealing machine again, and cutting the area of the middle area of the tipping paper with the size of 1cm multiplied by 10cm, as shown in figure 1, so as to prepare two tipping paper samples with printed surface seal.
(2) Sample migration treatment: taking a certain amount of artificial saliva into a beaker, placing the beaker into a water bath kettle at 40 ℃ and balancing for 30min. The prepared tipping paper sample seal surface is curled outwards, and is respectively placed in a 20mL headspace bottle, 10mL of balanced artificial saliva is added, the bottle is capped, and the bottle is immediately placed in a water bath kettle at 40 ℃ for 10min, and then is rapidly taken out and shaken uniformly. The migration solution is rapidly filtered by a microporous filter membrane with the diameter of 0.22 mu m, and the filtrate is collected for standby detection.
(3) Detection and analysis: and detecting and analyzing the filtrate by using high performance liquid chromatography to obtain a response value of the liquid chromatography of the target object in the filtrate, carrying the detected response value into a standard curve equation to obtain the content of saccharin sodium in the filtrate, and converting the content of the movable saccharin sodium in the back of the tipping paper for the cigarette by using the equation.
Comparative example 2
(1) Sample treatment: and (3) taking a tipping paper sample, and cutting the area of the middle area of the tipping paper, which is 1cm multiplied by 10cm, to obtain an unsealed tipping paper sample.
(2) Sample migration treatment: taking a certain amount of artificial saliva into a beaker, placing the beaker into a water bath kettle at 40 ℃ and balancing for 30min. The prepared unsealed tipping paper sample is curled, placed in a 20mL headspace bottle, added with 10mL of balanced artificial saliva, capped, immediately placed in a water bath kettle at 40 ℃ and rapidly taken out and shaken uniformly after 10min. The migration solution is rapidly filtered by a microporous filter membrane with the diameter of 0.22 mu m, and the filtrate is collected for standby detection.
(3) Detection and analysis: and detecting and analyzing the filtrate by using high performance liquid chromatography to obtain a response value of the liquid chromatography of the target object in the filtrate, carrying the detected response value into a standard curve equation to obtain the content of saccharin sodium in the filtrate, and converting the content of movable saccharin sodium in the tipping paper for the cigarette by using the equation.
Linear evaluation of standard solution: the linear correlation data of the saccharin sodium standard solution experiment are shown in table 1, and the correlation coefficient reaches 0.9999, which shows that the method has good linear correlation in the prepared concentration range and meets the detection requirement.
Table 1 linear relationship data for sodium saccharin
The content of the movable sodium saccharin in the printing face of the tipping paper, the content of the movable sodium saccharin in the back face of the tipping paper, and the content of the total movable sodium saccharin in the tipping paper were measured in example 1, comparative example 1, and comparative example 2, respectively, and the measurement results are shown in table 2. As can be seen from the data in the table, the sum of the detection results of example 1 and comparative example 1 deviates from comparative example 2 by only 0.8%, which means that the seal treatment of the present invention can achieve the purpose of single-sided detection of sodium saccharin in tipping paper.
Table 2 test data for sodium saccharin in the examples
The method according to the invention is carried out againThe renaturation experiment and the labeling recovery experiment show that the detection limit is 1.21 mg.m -2 The daily repeatability is 1.58%, the daily repeatability is 2.68%, the recovery rate of different content levels is 91.14-95.63%, and the method can meet the detection requirement.
Example 3
In order to avoid manual direct curling of the tipping paper, the prepared back plastic sealing tipping paper sample sealing surface is curled outwards through tweezers and then placed in a cylindrical headspace bottle. The tweezers comprise a tweezers body 1, a rotating rod 2 and a paper winding clamp 3, wherein the tweezers body 1 is made of iron or copper, the tweezers body 1 comprises two tweezers handles 11 which are integrally formed, the tail end of one tweezers handle 11 downwards vertically extends to form a tweezers foot 12, a vertically arranged through hole 13 is formed in the other tweezers handle 11, the rotating rod 2 is a plastic rod, the rotating rod 2 is inserted into the through hole 13, the bottom end of the rotating rod 2 and the paper winding clamp 3 are fixedly connected through glue, a paper clamping groove 31 which is vertically arranged is formed in the paper winding clamp 3, and the lower port of the paper clamping groove 31 always extends on the lower end face of the paper winding clamp 3.
When the butt joint tipping paper is curled, the paper clamping groove 31 in the tipping paper clamp 3 is spliced on the tipping paper, then two forceps handles 11 are oppositely nipped, the forceps feet 12 are abutted on the tipping paper clamp 3, the paper clamping groove 31 is contracted, and then the rotating rod 2 is rotated by hand, so that the butt joint tipping paper can be curled. The whole curling process is that hands are not in direct contact with paper, so that hand impurities are effectively prevented from adhering to tipping paper.
The paper winding clamp 3 is of a cylindrical structure, and for facilitating the shrinkage of the paper clamping groove 31, the paper winding clamp 3 is made of rubber. The top surface of dwang 2 is higher than the top surface of tweezers body 1, conveniently rotates dwang 2, is equipped with the net line on the upper end outer wall surface of dwang 2, can increase the frictional force with the hand, conveniently rotates dwang 2.
The foregoing is merely a preferred embodiment of the invention, and it should be noted that modifications could be made by those skilled in the art without departing from the principles of the invention, which modifications would also be considered to be within the scope of the invention.
Claims (9)
1. A method for measuring the transferable saccharin sodium in the printing surface of the tipping paper for cigarettes is characterized in that: the method comprises the following steps:
1) Placing two printed surfaces of tipping paper between two plastic packaging films for plastic packaging after face-to-face lamination, cooling to room temperature after plastic packaging is completed, and then taking the middle part by using a cutting knife to form two parallel samples with plastic packaged back surfaces;
2) Placing the prepared back plastic sealed paper sample into a headspace bottle containing artificial saliva, sealing, immediately placing the headspace bottle into a water bath for migration experiments after sealing, rapidly taking out the headspace bottle from the water bath after the migration experiments are finished, shaking uniformly to obtain migration liquid, passing the migration liquid through a 0.22 mu m water-based filter membrane, and collecting filtrate for standby detection;
3) Performing machine test on the filtrate obtained in the step 2), and quantitatively calculating the content of effective saccharin sodium in tipping paper by using an external standard method;
in the step 2), the prepared back plastic seal packaging paper sample seal surface is curled outwards through tweezers, and then the back plastic seal packaging paper sample seal surface is placed in a cylindrical headspace bottle; the tweezers comprise a tweezers body (1), a rotating rod (2) and a paper winding clamp (3), the tweezers body (1) comprises two tweezers handles (11) which are integrally formed, the tail end of one tweezers handle (11) vertically extends downwards to form a tweezers foot (12), a vertically arranged through hole (13) is formed in the other tweezers handle (11), the rotating rod (2) is inserted into the through hole (13), the bottom end of the rotating rod (2) is fixedly connected with the paper winding clamp (3), a paper clamping groove (31) which is vertically arranged is formed in the paper winding clamp (3), and the lower port of the paper clamping groove (31) always extends on the lower end face of the paper winding clamp (3).
2. The method for measuring the amount of the movable sodium saccharin in the printing surface of the tipping paper for cigarettes according to claim 1, wherein the method comprises the following steps: the test solution adopted in the step 3) of the power-on test is as follows: the mobile phase was formed by dissolving 0.154g of ammonia acetate in 1L of acetonitrile-water solution, wherein the volume ratio of acetonitrile-water was 1:9.
3. Tipping paper for cigarettes according to claim 1A method for measuring the transferable saccharin sodium in a printing surface is characterized in that: the step 3) of loading and unloading test adopts a liquid chromatograph under the analysis condition that a chromatographic column is HC-C18, the column temperature is 30 ℃, and the flow rate of a mobile phase is 1.0mL ∙ min -1 The sample injection amount is 2 mu L, and the detection wavelength is 230nm.
4. The method for measuring the amount of the movable sodium saccharin in the printing surface of the tipping paper for cigarettes according to claim 1, wherein the method comprises the following steps: and 2) before placing the headspace bottle in the tipping paper sample, placing the artificial saliva in the headspace bottle in a water bath kettle at 40 ℃ for balancing for 20-30 min.
5. The method for measuring the amount of the movable sodium saccharin in the printing surface of the tipping paper for cigarettes according to claim 1, wherein the method comprises the following steps: in the step 2), the migration condition is that the temperature is 40 ℃ and the time is 5-10 min.
6. The method for measuring the amount of the movable sodium saccharin in the printing surface of the tipping paper for cigarettes according to claim 1, wherein the method comprises the following steps: the volume of the artificial saliva adopted by the tipping paper sample per square centimeter is 0.5-2 mL, and the tipping paper sample is completely soaked in the artificial saliva during a migration experiment.
7. The method for measuring the amount of the movable sodium saccharin in the printing surface of the tipping paper for cigarettes according to claim 1, wherein the method comprises the following steps: the quantitative process of the external standard method in the step 3) is as follows: preparing saccharin sodium standard solutions with different gradients, and respectively detecting the prepared standard solutions with different gradients by using a liquid chromatograph to obtain corresponding response values of saccharin sodium in each standard solution; and (3) taking the concentration of saccharin sodium in each standard solution as an abscissa and the response value as an ordinate, and manufacturing to obtain a standard curve equation.
8. The method for measuring the amount of the movable sodium saccharin in the printing surface of the tipping paper for cigarettes according to claim 7, wherein the method comprises the following steps: the calculation process of the effective saccharin sodium content of the tipping paper in the step 3) comprises the following steps:
the measured response value of the saccharin sodium in the filtrate is brought into the standard curve equation to obtain the content of the saccharin sodium in the filtrate, and the obtained content of the saccharin sodium is brought into the equation x=c×v/S to obtain the content of the movable saccharin sodium in the printing surface of the back plastic packaging paper sample;
wherein x is the content of the transferable saccharin sodium in the printing surface of the tipping paper sample, and the unit is milligrams per square meter;
c is the concentration of saccharin sodium in the migration solution; units are milligrams per milliliter;
v is the volume of the migration liquid; the unit is milliliter;
s is the cutting area of the tipping paper sample, and the unit is square meters.
9. The method for measuring the amount of the movable sodium saccharin in the printing surface of the tipping paper for cigarettes according to claim 1, wherein the method comprises the following steps: the printed surfaces of the two tipping papers are bonded face to face and then placed between the two food plastic packaging films for plastic packaging, the times of plastic packaging are two times, and the temperature of the first plastic packaging and the temperature of the second plastic packaging are both 130-140 ℃.
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