Method for detecting migration condition of sweetening agent on surface of tipping paper and application of method

Abstract

The invention provides a method for detecting the migration condition of a sweetening agent on the surface of tipping paper and application of the method. The detection method comprises the following steps: (1) wrapping and clamping one end of to-be-detected tipping paper with two pieces of blank paper; completely wrapping and clamping the tipping paper to be detected by using plastic packaging film paper, and wrapping and clamping part of the blank paper; (2) performing plastic packaging on the to-be-tested tipping paper which is completely wrapped and clamped by the plastic packaging film paper, and then tearing the to-be-tested tipping paper along the blank paper to obtain the front surface and the back surface of the to-be-tested tipping paper; and (3) detecting the content of the sweetening agent on the front side and the back side of the to-be-detected tipping paper by adopting a liquid chromatography, and judging the migration condition of the sweetening agent on the surface of the to-be-detected tipping paper according to a detection result. The method provided by the invention can accurately and effectively separate the front and back surfaces of the tipping paper so as to accurately detect and analyze the sweetener migration condition, and is convenient to operate, high in accuracy, safe and reliable.

Description

Technical Field

[0001] The invention belongs to the technical field of food additive detection, and particularly relates to a method for detecting sweetener migration on the surface of tipping paper and an application thereof. Background Art

[0002] Compared with traditional food packaging materials, paper packaging materials have the advantages of low cost, good processing performance, and excellent printing performance, which makes its share in packaging materials grow steadily year by year. Sweeteners are a type of food additives that can improve taste, enrich characteristic aromas, and impart sweetness. Some food manufacturers print sweeteners on the surface of paper packaging materials to form unique style products. For example, some companies add sweeteners to commonly used tipping paper, which is favored by some consumers. Because its tipping paper is a reel paper material, after printing, hot stamping, slitting and other manufacturing and processing procedures, the sweetener will migrate to the back side due to the stress inside the reel, that is, migrate from the printed surface to the adjacent back side. In actual production, only the sweetener on the printed surface 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 sweet effect. Therefore, the existing sample preparation and testing technology cannot solve the problem that the surface sweetness sensory intensity of some products does not match the content (front plus back) of the current test sample preparation method in actual work.

[0003] CN217385429U discloses a lip-touch tipping paper sweetness comparison sample, including tipping paper, a printing area and a blank area are provided on the upper end surface of the tipping paper, two blank areas are symmetrically arranged on both sides of the printing area, sweeteners are printed on the printing area to form a comparison layer, a packaging film is provided on the lower end surface of the tipping paper, a plurality of tipping papers are stacked, and the packaging films of two adjacent tipping papers are mutually attached to the comparison layer. The utility model provides a packaging film, and when the tipping papers are stacked in sequence, the packaging film can prevent the sweeteners from migrating to each other, and the setting of the packaging film can also prevent the sweeteners on a single tipping paper from migrating to the back, especially when licking, and will not migrate when encountering saliva, thereby ensuring the sampling effect. The utility model is convenient for detection, convenient for batch production, easy to carry, good in use effect, and improves detection efficiency.

[0004] CN215574471U discloses a device for detecting the coating transfer of plugging paper, comprising an isolation plate, a fixing piece is provided on the isolation plate, the fixing piece fixes the plugging paper base paper to one side of the isolation plate, and a groove for bearing pressure is provided on the other side of the isolation plate, and the plugging paper base paper is in direct contact with the coating printing surface of the plugging paper to be tested. After clamping, when the test time comes, the fixing piece is removed, the plugging paper base paper is taken out, and the sweetener content in the base paper is measured to obtain the migration amount of the sweetener within the test time. The extraction device can conveniently and effectively collect the amount of sweetener transfer between papers in the plugging paper within a certain period of time.

[0005] However, the above methods cannot accurately determine whether the content of the sweetener after migration is completely detected. Therefore, how to provide a method that can effectively detect the migration of sweeteners has become an urgent problem to be solved. Summary of the invention

[0006] In view of the shortcomings of the prior art, the present invention aims to provide a method for detecting the migration of sweeteners on the surface of tipping paper and its application. The method provided by the present invention can accurately and effectively separate the front and back sides of tipping paper, thereby realizing accurate detection and analysis of the migration of sweeteners, and is easy to operate, highly accurate, safe and reliable.

[0007] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0008] In one aspect, the present invention provides a method for detecting the migration of sweeteners on the surface of tipping paper, the detection method comprising the following steps:

[0009] (1) Use two blank papers to wrap one end of the tipping paper to be tested; use plastic film paper to completely wrap the tipping paper to be tested and also wrap part of the blank paper;

[0010] (2) plastic-sealing the tipping paper to be tested after being completely wrapped by the plastic sealing film paper, and then tearing the tipping paper to be tested along the blank paper to obtain the front side of the tipping paper to be tested and the back side of the tipping paper to be tested;

[0011] (3) Using liquid chromatography to detect the sweetener content on the front side and the back side of the tipping paper to be tested, and judging the migration of the sweetener on the surface of the tipping paper to be tested according to the test results.

[0012] The above method uses a plastic sealing method to penetrate the hot melt adhesive on the plastic sealing film paper into the tipping paper to be tested, and then tears it open, which can effectively separate the front and back sides of the tipping paper, thereby realizing accurate detection and analysis of the migration of sweeteners. The operation is convenient, accurate, safe and reliable.

[0013] Due to the special structure of the reel paper, the migration conditions between two adjacent layers are almost the same. Therefore, the migration conditions of two adjacent layers of tipping paper can be determined by testing the front and back sides of a piece of tipping paper to be tested.

[0014] Preferably, the blank paper in step (1) extends beyond the plastic film paper by at least 5 mm, for example 5 mm, 6 mm, 7 mm, 8 mm, 9 mm, 10 mm, 11 mm, 12 mm, 13 mm, 14 mm or 15 mm, but is not limited to the above-listed values. Other values ​​not listed within the above-listed range are also applicable.

[0015] Preferably, the plastic sealing in step (2) is performed using a laminator.

[0016] Preferably, the film thickness of the laminator is 83-87 μm, such as 83 μm, 84 μm, 85 μm, 86 μm or 87 μm, but is not limited to the above-listed values. Other values ​​not listed within the above-listed range are also applicable.

[0017] Preferably, the temperature of the plastic sealing in step (2) is 127-133°C, for example, 127°C, 128°C, 129°C, 130°C, 131°C, 132°C or 133°C, but is not limited to the above-listed values. Other values ​​not listed within the above-listed range are also applicable.

[0018] The above parameter control can effectively separate the front and back sides of the tipping paper, so that the thickness of the front and back tipping papers is equivalent, avoiding the situation of non-layering or partial non-layering when tearing and peeling, and improving the accuracy of the detection result.

[0019] Preferably, the specific steps of using liquid chromatography in step (3) are as follows:

[0020] The front side of the tipping paper to be tested and the back side of the tipping paper to be tested are mixed with the extraction liquid respectively, and then ultrasonic extraction is performed to obtain the injection liquid, and then liquid chromatography detection is performed.

[0021] Preferably, the raw materials for preparing the tipping paper to be tested include coniferous wood pulp and hardwood wood pulp.

[0022] Preferably, the thickness of the tipping paper to be tested is 30-50 μm, such as 30 μm, 35 μm, 40 μm, 45 μm or 50 μm, but is not limited to the above values, and other values ​​not listed in the above range are also applicable.

[0023] The above liquid chromatography detection method can adopt conventional sweetener detection methods in the art, and the present invention does not impose too many limitations on this.

[0024] On the other hand, the present invention also provides the application of the above detection method in cigarette tipping paper detection.

[0025] Compared with the prior art, the present invention has the following beneficial effects:

[0026] The present invention provides a method for detecting the migration of sweeteners on the surface of tipping paper. The method uses a plastic sealing method to infiltrate the hot melt adhesive on the plastic sealing film paper into the tipping paper to be tested, and then tears it open, so that the front and back sides of the tipping paper can be effectively separated, thereby realizing accurate detection and analysis of the migration of sweeteners. The method is convenient to operate, highly accurate, safe and reliable. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 It is a front and back view of the tipping paper obtained by peeling and layering according to the method provided in Example 1;

[0028] Figure 2 It is a front and back view of the tipping paper obtained by peeling and layering according to the method provided in Example 4;

[0029] Figure 3 It is a front and back view of the tipping paper obtained by peeling and layering according to the method provided in Example 5;

[0030] Figure 4 It is the front and back view of the tipping paper obtained by peeling and layering according to the method provided in Example 6. DETAILED DESCRIPTION

[0031] The technical solution of the present invention is further described below by specific implementation methods. It should be understood by those skilled in the art that the embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0032] In the following example, the main components of the tipping paper to be tested are as follows, the thickness is 38μm, and the front side is coated with sweetener dihydrate SAC (C6H4CONNaSO2):

[0033]

[0034]

[0035] Example 1

[0036] This embodiment provides a method for detecting the migration of sweeteners on the surface of tipping paper, and the specific steps are as follows:

[0037] 1) Use a plastic film with hot melt adhesive to clamp the tipping paper to be inspected; the thickness of the plastic film is 7 filaments.

[0038] 2) Packaging sample preparation: Cut two pieces of white paper that are thinner than the sample paper and place them at the end of the plastic film and tipping paper. One piece on the front and one on the back are clamped with the tipping paper and placed together in the plastic film. The white paper should protrude 5mm from the plastic film.

[0039] 3) Laminator: Use laminator to seal with thickness of 85μm and constant temperature of 130℃.

[0040] 4) Sample processing: After plastic sealing, let it stand for 10 minutes. When the sample cools down, tear it apart evenly along the two pieces of white paper, and peel off the connecting paper to get the front and back sides.

[0041] 5) Detection of sweetener content in the front and back tipping papers by high performance liquid chromatography: The detection method is as follows:

[0042] Preparation of samples to be tested: accurately cut a sample with a length of 40 mm (the width direction of the sample is fully included), cut it into 10 mm × 10 mm pieces, and transfer them all to a 50 mL stoppered conical flask, accurately add 30 mL of extraction solution (300 mL of methanol (containing ammonium acetate, concentration 2 mmol / L) and 700 mL of first-grade water in a 1 L volumetric flask, mix well), extract by ultrasonic at 30 ° C for 60 min, shake well after the extraction, let it stand for a while, filter through a 0.22 μm organic phase micromembrane to obtain the filtrate, and wait for analysis.

[0043] Chromatographic analysis conditions:

[0044] Mobile phase A: buffer (ammonium acetate solution, 2 mmol / L);

[0045] Mobile phase B: acetonitrile;

[0046] Flow rate: 1.2 mL / min;

[0047] Mobile phase gradient: see the table below;

[0048] Injection volume: 5 μL;

[0049] Column temperature: 30°C;

[0050] Detection wavelength: 230nm;

[0051] Post-running time: 2min.

[0052] Time (min) Mobile phase A (%) Mobile phase B (%) 0 80 20 8 80 20 8.1 40 60 15 40 60 15.1 90 10 18 90 10

[0053] Preparation of a series of standard working solutions

[0054] Accurately weigh 0.1g sweetener dihydrate SAC (purity 98% or more) in a 100mL volumetric flask, dilute with first-grade water and make up to the mark, mix well, and dilute with water to make up to the mark. Prepare a 5-grade standard working solution, use the above-mentioned liquid chromatography process for detection, use retention time for qualitative analysis, and external standard method for quantitative analysis. According to the concentration of the prepared standard solution and its response peak area, establish a standard working curve for sweeteners. The working curve correlation coefficient R 2 ≥0.999.

[0055] 6) The sweetener in the sample to be tested is calculated as dihydrate SAC, and its content is calculated as follows:

[0056]

[0057] Where:

[0058] X——the content of sweetener SAC dihydrate in the sample, in mg / m 2 ;

[0059] C——the concentration of the analyte in the sample filtrate obtained from the standard working curve, in μg / mL;

[0060] V——the volume of the extraction solution, in mL;

[0061] L——sample cutting length, in mm;

[0062] W——sample width, in mm.

[0063] The arithmetic mean of the two parallel determination results is taken as the final determination result, accurate to 0.1 mg / m 2 The relative average deviation between parallel determination results should be less than 10%. The test results (total sample content 140 mg / m 2 , positive content 123.79mg / m 2 , back side content 18.61mg / m 2 ) to determine the migration of sweeteners on the surface of the tipping paper to be tested.

[0064] Example 2

[0065] This embodiment provides a method for detecting the migration of sweeteners on the surface of tipping paper, which is consistent with the embodiment 1 except step 3).

[0066] 3) Laminator: Use laminator to seal with thickness of 83μm and constant temperature of 133℃.

[0067] Example 3

[0068] This embodiment provides a method for detecting the migration of sweeteners on the surface of tipping paper, which is consistent with the embodiment 1 except step 3).

[0069] 3) Laminator: Use laminator to seal with a thickness of 87μm and a constant temperature of 127℃.

[0070] Embodiment 4-6

[0071] Examples 4-6 respectively provide a method for detecting the migration of sweeteners on the surface of tipping paper, which are consistent with Example 1 except that the over-plastic thickness in step 3) is 75 μm, 80 μm and 95 μm respectively.

[0072] Embodiment 7-9

[0073] Examples 7-9 respectively provide a method for detecting the migration of sweeteners on the surface of tipping paper, except that the plastic sealing temperatures in step 3) are 120° C., 125° C. and 135° C. respectively, and the rest are consistent with Example 1.

[0074] Effect test:

[0075] The thickness of the front and back sides obtained in step 4) of the method of Examples 1-9 and the peeling condition when torn were respectively detected. The peeling conditions of Examples 1 and 4-6 were as follows: Figure 1-4 The results are as follows:

[0076] Group Front peel thickness (μm) Back peeling thickness (μm) Peel off the layering effect Example 1 91.8 83.5 Uniform layering Example 2 92.6 83 Uniform layering Example 3 91 84.5 Uniform layering Example 4 69.3 100.3 Unstratified Example 5 90.5 73.2 Local stratification Example 6 68.3 98.8 Unstratified Example 7 91.5 74.3 Local stratification Example 8 69.4 98.6 Local stratification Example 9 67.6 97.5 Local stratification

[0077] In addition, the precision (6 replicates for each test) and recovery (three concentrations of low, medium and high were spiked, 60 mg / m 2 , 120mg / m 2 , 180mg / m 2 ) is calculated, and the results are as follows:

[0078]

[0079]

[0080] From the above data, it can be found that the method provided by the present invention can effectively detect and analyze the migration of sweeteners on the surface of the tipping paper with high accuracy; at the same time, by controlling relevant parameters, the accuracy and precision of the detection can be further improved, and the front and back sides of the tipping paper can be effectively separated so that the thickness of the two are similar, thereby improving the detection accuracy.

[0081] The applicant declares that the present invention uses the above-mentioned embodiments to illustrate the detection method and application of the sweetener migration on the tipping paper surface of the present invention, but the present invention is not limited to the above-mentioned embodiments, that is, it does not mean that the present invention must rely on the above-mentioned embodiments to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of various raw materials of the product of the present invention, addition of auxiliary ingredients, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

[0082] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, a variety of simple modifications can be made to the technical solution of the present invention, and these simple modifications all belong to the protection scope of the present invention.

[0083] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

Claims

1. A method for detecting the migration of sweeteners on the surface of tipping paper, characterized in that: The detection method comprises the following steps: (1) Use two blank papers to wrap one end of the tipping paper to be tested; use plastic film paper to completely wrap the tipping paper to be tested and also wrap part of the blank paper; (2) plastic-sealing the tipping paper to be tested after being completely wrapped by the plastic sealing film paper, and then tearing the tipping paper to be tested along the blank paper to obtain the front side of the tipping paper to be tested and the back side of the tipping paper to be tested; (3) Using liquid chromatography to detect the sweetener content on the front side and the back side of the tipping paper to be tested, and judging the migration of the sweetener on the surface of the tipping paper to be tested according to the test results.

2. The detection method according to claim 1, characterized in that: In step (1), the blank paper extends beyond the plastic film paper by at least 5 mm.

3. The detection method according to claim 1 or 2, characterized in that: The plastic sealing in step (2) is performed using a laminating machine.

4. The detection method according to claim 3, characterized in that: The film thickness of the laminator is 83-87 μm.

5. The detection method according to any one of claims 1 to 4, characterized in that: The temperature of the plastic sealing in step (2) is 127-133°C.

6. The detection method according to any one of claims 1 to 5, characterized in that: The specific steps of using liquid chromatography in step (3) are as follows: The front side of the tipping paper to be tested and the back side of the tipping paper to be tested are mixed with the extraction liquid respectively, and then ultrasonic extraction is performed to obtain the injection liquid, and then liquid chromatography detection is performed.

7. The detection method according to any one of claims 1 to 6, characterized in that: The raw materials for preparing the tipping paper to be tested include softwood pulp and hardwood pulp.

8. The detection method according to any one of claims 1 to 7, characterized in that: The thickness of the tipping paper to be tested is 30-50 μm.

9. Application of the detection method according to any one of claims 1 to 8 in cigarette tipping paper detection.

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