CN111912964A - Method for judging 3-year validity period of wet tissue product - Google Patents
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Abstract
The invention discloses a method for judging the 3-year validity period of a wet tissue product, which comprises the following steps: performing a 12-week stability test on the wet wipe samples; detecting the mass of the wet tissue sample in different periods within 12 weeks, calculating the mass reduction rate, drawing a regression curve of the mass reduction rate of the wet tissue sample and the time, and judging whether the mass reduction rate is linearly related to the time; and if the mass reduction rate is linearly related to the time, calculating the mass reduction rate of the wet tissue sample after 3 years based on the regression curve, and if the mass reduction rate meets the expected requirement of the 3-year effective period, preliminarily judging that the recommended effective period of the wet tissue product is 3 years. The invention can draw a linear regression equation of the product quality reduction rate and the time for the wet tissue product with the validity period of 3 years needing to be judged through the stability test data of 12 weeks, the quality reduction rate of the product in 3 years is calculated by the equation, and the product recommended validity period is preliminarily judged to be 3 years if the result meets the customer requirements.
Description
Technical Field
The invention belongs to the field of disposable hygienic products, and particularly relates to a method for judging the 3-year validity period of a wet tissue product.
Background
The purpose of the stability test is to investigate the change rule of the product along with time under the influence of temperature, humidity and illumination conditions, provide scientific basis for the production, packaging, storage and transportation of the product, and establish the validity period of the product through experiments. At present, the stability test method of the wet tissue product mainly refers to the specified test in the national standard, and the conclusion of the national standard GB15979-2002 of the wet tissue is as follows: and (3) accelerated test: placing the original packaging sample in an incubator at 54-57 ℃ for 14 days, wherein the product stability test result is supposedly maintained at room temperature for at least 1 year; the results of the test of the stability of the product in an incubator at 37-40 ℃ for 3 months are presumably maintained at room temperature for at least 2 years. The national standard does not specify a method for testing the validity of a wet tissue product for 3 years (at least 3 years at room temperature), but the general practice in the industry is to accelerate the test of a wet tissue sample at about 40 ℃ for 36 weeks, and the result of the product stability test is presumably maintained for at least 3 years at room temperature. However, the test period of the 36-week period is long, so that the product development period is long.
Therefore, a method for determining the 3-year validity period of a wet tissue product, which can shorten the test period, is needed.
Disclosure of Invention
In order to solve the technical problem, the invention provides a method for judging the 3-year validity period of a wet tissue product, which comprises the following steps:
step A: performing a 12-week stability test on the wet wipe samples;
and B: detecting the mass of the wet tissue sample in different periods within 12 weeks, calculating the mass reduction rate, drawing a regression curve of the mass reduction rate of the wet tissue sample and the time, and judging whether the mass reduction rate is linearly related to the time;
and C: and if the mass reduction rate is linearly related to the time, calculating the mass reduction rate of the wet tissue sample after 3 years based on the regression curve, and if the mass reduction rate meets the expected requirement of the 3-year effective period, preliminarily judging that the recommended effective period of the wet tissue product is 3 years.
Optionally, in the step C, the recommended validity period of the wet tissue product is preliminarily determined to be 3 years, the stability test is continued to 36 weeks, and whether the validity period of the wet tissue product is 3 years is determined according to the stability test data of other stability test items within the period of 36 weeks.
Optionally, in the step B, if the correlation coefficient R of the regression curve is greater than or equal to 0.99, it is determined that the mass reduction rate is linearly related to time; otherwise, continuing to perform the stability test for 36 weeks, and judging whether the effective period of the wet tissue product is 3 years or not according to the stability test data of other stability test items within the period of 36 weeks.
Optionally, in the step C, if the mass reduction rate meets the expected requirement, the stability test data of other stability test items in 12 weeks are referred to, and if the stability test data of other stability test items does not have a variation trend of serious deviation, the validity period of the wet tissue product is determined to be 3 years; otherwise, the stability test is terminated and the shelf life of the wet wipe product cannot be judged as 3 years.
Optionally, the mass reduction rate in step B is calculated by the following formula:
the mass reduction rate at a certain point is (initial mass-product mass at a certain point)/initial mass × 100%.
Optionally, in the step C, the expected requirement of the 3-year validity period further includes: the liquid content of the wet tissue product is more than or equal to 1.7 times after 3 years.
Optionally, the other stability test items include weight, wet wipe appearance, squeeze appearance, odor, pH, inner label color, package integrity, package sealability, and microbial limit.
Optionally, the trend of the stability test data of the other stability test items without serious deviation is that:
weight: within ± 8% of the initial weight of the product;
wet tissue appearance, extrusion fluid appearance, odor, pH, inner label color: no significant change compared to week 1;
packaging integrity: the conditions of damage and non-setting adhesive falling are avoided;
packaging sealing property: the package is pressed by hand without air leakage;
the microbial limit: the total number of aerobic bacteria colonies is less than 100cfu/g, and the total number of yeast and mould colonies is less than 10 cfu/g; gram negative bacteria and staphylococcus aureus were not detected.
Optionally, the method comprises an accelerated test A, an accelerated test B, a room temperature test, a light test, a low temperature test and a temperature cycle test, wherein,
the accelerated test A is to place a wet tissue sample at the temperature of 38-42 ℃ and the relative humidity of 70-80%, sample at different time points and determine a stability detection item;
the accelerated test B is to place the wet tissue sample at the temperature of 54-57 ℃, sample at different time points and determine a stability detection item;
the room temperature test is to place a wet tissue sample at room temperature, sample at different time points and determine a stability detection item;
the illumination test is to place the wet tissue sample in the indoor windowsill under the natural illumination condition, sample at different time points and determine the stability detection item;
the low-temperature test is to place a wet tissue sample at the temperature of 2-8 ℃, sample at different time points and determine a stability detection item;
the temperature cycle test refers to that a wet tissue sample is placed under a variable temperature condition, samples are taken at different time points, and stability detection items are determined, wherein the variable temperature condition refers to that the temperature lasts for 12 hours at 21-25 ℃, 24 hours at-15 ℃, 12 hours at 21-25 ℃ and 24 hours at 43-47 ℃ in sequence, and the conditions are cycled.
Optionally, the method for determining the microbial limit is:
step S1, adding the wet tissue sample into the solution D to prepare a test solution;
step S2, filtering the test solution by using a filter membrane, flushing the filter membrane by using a solution D, and detecting the total number of aerobic bacteria and the total number of mould yeasts in the filtrate;
step S3, preparing a primary enrichment fluid A from the test fluid in the step S1, and detecting staphylococcus aureus, escherichia coli and pseudomonas aeruginosa in the primary enrichment fluid A;
and step S4, preparing the initial enrichment liquid B from the test solution obtained in the step S1, and detecting salmonella in the initial enrichment liquid B.
Compared with the prior art, the invention has the following technical effects:
1. the invention can draw a linear regression equation of the product quality reduction rate and the time for the wet tissue product with the validity period of 3 years needing to be judged through the stability test data of 12 weeks, the quality reduction rate of the product in 3 years is calculated by the equation, the product recommended validity period of the product is preliminarily judged to be 3 years if the result meets the customer requirement, meanwhile, the stability test is continued, and the validity period of the product can be temporarily determined to be 3 years after the complete 36-week test is completed.
2. The invention provides a stability testing method for judging the 3-year validity period of wet tissue products for the first time, which has guiding significance for the development of the wet tissue products.
3. As the improvement of the existing wet tissue product stability test method, the invention develops a suitable simulation investigation method for verifying the 3-year validity period of the product by summarizing the use rule of daily wet tissues and combining the wet tissue stability test method, greatly shortens the stability test time, and can preliminarily judge the stability performance of the wet tissues in 12 weeks.
Drawings
FIG. 1 is a regression curve plotted in example 4 of the present application.
Detailed Description
While specific embodiments of the present invention or prior art will be described briefly in order to more clearly illustrate it, it should be apparent that the following description of the embodiments is illustrative of some embodiments of the present invention and that others can be devised by those skilled in the art without departing from the inventive concept.
Example 1:
the present embodiment provides different testing methods, which specifically include the following steps:
accelerating test A: placing the wet tissue sample at the temperature of 38-42 ℃ and the relative humidity of 70-80% for 36 weeks, sampling at 1 week, 2 weeks, 4 weeks, 8 weeks, 12 weeks, 24 weeks and 36 weeks respectively, determining stability detection items, and comparing the results with the results of the same test at 5 ℃ and 0 day. Wherein 1 pack was taken as a weighing sample and weighed at the same time each time.
② accelerated test B: placing the wet tissue sample at the temperature of 54-57 ℃ for 2 weeks, sampling at 1 week and 2 weeks respectively, determining stability detection items, and comparing the results with the results of the same-period test at 5 ℃ and 0 day. Wherein 1 pack was taken as a weighing sample and weighed at the same time each time.
Room temperature test: the wet tissue samples were left at room temperature for 156 weeks (i.e., 3 years), and were sampled at 1 week, 2 weeks, 4 weeks, 8 weeks, 12 weeks, 24 weeks, 36 weeks, 52 weeks, 78 weeks, 104 weeks, 130 weeks, and 156 weeks, respectively, to determine the stability test items, and the results were compared with the results of the same test at 5 ℃ and 0 day. Wherein 1 pack was taken as a weighing sample and weighed at the same time each time.
Wherein, the room temperature means that the average kinetic temperature is 20-25 ℃, the actual temperature fluctuation range is allowed to be 10-30 ℃, and the humidity is not required.
Fourthly, illumination test: placing the wet tissue sample on an indoor windowsill, naturally irradiating the surface of the wet tissue sample for 12 weeks, sampling at 1 week, 2 weeks, 4 weeks, 8 weeks and 12 weeks respectively, determining stability detection items, and comparing the results with the results of the same-period test at 5 ℃ and 0 day. Wherein 1 pack was taken as a weighing sample and weighed at the same time each time.
Low-temperature test: the wet tissue samples are placed at the temperature of 2-8 ℃ for 156 weeks (namely 3 years), and are respectively sampled at 0 week, 1 week, 2 weeks, 4 weeks, 8 weeks, 12 weeks, 24 weeks, 36 weeks, 52 weeks, 78 weeks, 104 weeks, 130 weeks and 156 weeks, and the results are compared with the results of the 5 ℃ and 0 day test in the same period by the stability test item. Wherein 1 pack was taken as a weighing sample and weighed at the same time each time.
Sixthly, temperature cycle test (extreme conditions): placing a wet tissue sample under a variable temperature condition, wherein the variable temperature condition refers to that the wet tissue sample is continuously kept for 12 hours under the conditions of 21-25 ℃ and 55-65% of relative humidity for 24 hours under the condition of-15 ℃, the wet tissue sample is continuously kept for 12 hours under the conditions of 21-25 ℃ and 55-65% of relative humidity for 12 hours under the conditions of 43-47 ℃ and 55-65% of relative humidity for 24 hours and 21-25 ℃ and 55-65% of relative humidity for 12 weeks, circulating the above condition test for 12 weeks, respectively sampling at 1 week, 2 weeks, 4 weeks, 8 weeks and 12 weeks, determining a stability test item, and comparing the result with the test result at 5 ℃ and 0 day in the same period. Wherein 1 pack was taken as a weighing sample and weighed at the same time each time.
Typically, for each of the 6 tests described above, each time after the set-out time has reached the test period, one of the packs is removed and weighed without unpacking and recorded, and the wet wipes are removed and the product is tested for liquid content according to the test method of GB/T27728. The method comprises the following specific steps: 1 piece of wet tissue is respectively taken from the upper, middle and lower 3 positions of a complete wet tissue package by using tweezers to form a test sample (the amount of each piece of wet tissue is less than 3 pieces of sample, and the sample is extracted according to the actual number of pieces in a single package), and the sample is immediately weighed by a balance with the sensing quantity of 0.01 g. And then rinsing the sample by using distilled water or deionized water until no foam exists, placing the sample in an oven at the temperature of (85 +/-2) ° C (when the sample is baked, the sample is not required to be in contact with the four walls of the oven), baking for 4 hours, taking out the sample, weighing again, dividing the difference of the weighed values at the two sides by the mass after baking to obtain the liquid content of the test, calculating by times, and keeping the result to a decimal number according to the following formula by a calculation method.
Liquid content (mass before baking-mass after baking)/mass after baking
3 samples are made for each sample, and 3 samples are respectively from different complete packages, and the arithmetic mean value of the liquid contents of the 3 samples is taken as the liquid content of the sample.
The test conditions for the above 6 test methods can be seen in table 1.
TABLE 1 test conditions for different test methods
The test cycle of the above 6 test methods can be seen in table 2.
TABLE 2 test periods for different test methods
Table 3 shows the number of tests required for different specifications of the product. The different number of sheets is set because the product with less number of sheets can not meet the requirement of testing number, and the testing amount of the product with less than 10 sheets needs double number. The difference between the four-edge sealing and the three-edge sealing is that the number of the heat sealing edges of the product package is different, and the essential package form is not different.
TABLE 3 number of samples tested
Table 4 shows the expected requirements for a 3 year useful life under different test methods.
TABLE 4 Wet towel products acceptable standards for mass loss and liquid content
| Serial number | Test method | Rate of decrease in product quality | Liquid content |
| 1 | Low temperature test | 1.0％ | - |
| 2 | Room temperature test | 2.0％ | - |
| 3 | Light test | 2.0％ | - |
| 4 | Accelerated test A | 10.0％ | Not less than 1.7 |
| 5 | Temperature cycle test | 8.0％ | - |
| 6 | Accelerated test B | 20.0％ | Not less than 1.7 times |
The standard in table 4 is only suitable for wet wipes packaged by plastic bags (including two types of non-perforated wet wipes and non-dry wipes adhered to perforated wet wipes), and the proportion of low boiling point components (ethanol and the like) in the wet wipe feed liquid is not more than 10%.
Table 5 shows the test reference method and the acceptance criteria of other stability test items.
TABLE 5 test reference method and acceptability criteria for other stability test items
Example 2
This example provides a method for determining the expiration date of a wet wipe product, wherein 6 test methods (i.e., stability tests) are performed simultaneously,
(1) and (B) an accelerated test, namely performing an accelerated test on the wet tissue product at 54-57 ℃ for 2 weeks, and if the result is qualified, judging that the wet tissue product is kept at room temperature for at least 1 year.
(2) And (4) an accelerated test A, namely the wet tissue product is subjected to an accelerated test at 40 +/-2 ℃ for 12 weeks, and if the result is qualified, the wet tissue product is judged to be maintained at room temperature for at least 2 years.
(3)6 stability tests are carried out for 12 weeks, the mass reduction rate at each time point is calculated in each test period shown in table 2, a regression curve is drawn by taking the mass reduction rate data (in units of "%") of the product as a Y axis and the time (in units of "week") as an X axis, and a unitary linear regression equation of the mass reduction rate and the time is obtained; and if the linear regression correlation coefficient R is more than or equal to 0.99, judging that the product quality reduction rate is linearly related to the time. The time of substituting the X value into the linear equation obtained was 3 years (156 weeks), and the mass reduction rate Y value after 3 years under each test condition was calculated. If the quality reduction rate of 3 years meets the expected requirement of the validity period of 3 years, and other stability detection items within 12 weeks are referred, if the quality of the product does not have a variation trend of serious deviation, the quality guarantee period of the product can be tentatively set to 3 years through strict evaluation.
(4) When the accelerated test A is carried out for 36 weeks, if the result is qualified, the wet tissue product is judged to be maintained at room temperature for at least 3 years.
Example 3
In this embodiment, stability test data of each detection item at different time points and different test methods will be described with time as a main line. The wet wipe samples used in this example were all the smallest individual packages available on the market. The test was from 2017, 6 month, 20 days (1), week 0-table 6
(2) Week 1-Table 7
(3) Week 2-Table 8
(4) Week 4-Table 9
(5) Week 8-Table 10
(6) Week 12-Table 11
(7) Week 24-Table 12
(8) Week 36-Table 13
(9) Week 52-Table 14
| Detecting items | Low temperature test | Room temperature test |
| Weight (not unsealed), g | 669.71 | 652.75 |
| Appearance of the product | White colour | White colour |
| pH value | 5.12 | 5.55 |
| Smell(s) | Has no peculiar smell | Has no peculiar smell |
| Color of the extruded liquid | Clarification | Clarification |
| Color of inner label | White colour | White colour |
| Integrity of packaging | Intact | Intact |
| Microbial Limit, cfu/g | Qualified | Qualified |
(10) Week 78-Table 15
(11) Week 104-Table 16
| Detecting items | Low temperature test | Room temperature test |
| Weight (not unsealed), g | 669.59 | 632.83 |
| Appearance of the product | White colour | White colour |
| pH value | 5.09 | 5.46 |
| Smell(s) | Has no peculiar smell | Has no peculiar smell |
| Color of the extruded liquid | Clarification | Clarification |
| Color of inner label | White colour | White colour |
| Integrity of packaging | Intact | Intact |
| Microbial Limit, cfu/g | Qualified | Qualified |
(12) Week 130-Table 17
| Detecting items | Low temperature test | Room temperature test |
| Weight (not unsealed), g | 669.62 | 622.87 |
| Appearance of the product | White colour | White colour |
| pH value | 5.11 | 5.56 |
| Smell(s) | Has no peculiar smell | Has no peculiar smell |
| Color of the extruded liquid | Clarification | Clarification |
| Color of inner label | White colour | White colour |
| Integrity of packaging | Intact | Intact |
| Microbial Limit, cfu/g | Qualified | Qualified |
(13) Week 156- -Table 18
Example 4
The purpose of this example is to show the weight loss data over the test period for both the room temperature test and the accelerated test a in example 3. See table 19 for details.
Watch 19
FIG. 1 is a regression curve plotted in example 4 of the present application. Referring to fig. 1, regression curves were plotted based on the data in table 19, with the mass reduction data (in "%") for the product on the Y-axis and time (in "weeks") on the X-axis.
Under room temperature storage conditions (i.e., room temperature testing), the linear equation of mass loss rate versus time plotted against the 12 week data is Y-0.0005902X +0.0004082, R2With 0.9896 ≈ 0.99, the linear relationship is good. The substitution time was 3 years (156 weeks), the mass loss rate was 9.2%, and the weight loss was about 61.823 g. It is very close to the actual mass loss at 156 weeks (61.32g) in Table 19.
Under the conditions of 40 ℃ of temperature and 70-80% of relative humidity (namely, accelerated test A), a linear equation of mass reduction rate and time is drawn by data of 12 weeksy＝0.0013026x+0.0005603，R2The linear relationship is good at 0.9976. The substitution time was 36 weeks, the mass loss rate was 4.7454%, and the weight loss was about 31.7685 g. This is very close to the actual mass loss at 36 weeks (31.45g) in Table 19.
Therefore, it can be determined that a linear regression equation of the product quality reduction rate and the time can be drawn through the stability test data of 12 weeks, the product quality reduction rate in 3 years is calculated by the equation, if the liquid content rate in 3 years is more than 1.7 times, the product meets the customer requirements, meanwhile, the product quality does not have a change trend of serious deviation by referring to other stability detection items of 12 weeks, and the shelf life of the product can be tentatively set to 3 years through strict evaluation.
The above description is only an embodiment of the present invention, and is not intended to limit the scope of the present invention, and all equivalent flow transformations made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. A method for judging the 3-year validity period of a wet tissue product is characterized by comprising the following steps:
step A: performing a 12-week stability test on the wet wipe samples;
and B: detecting the mass of the wet tissue sample in different periods within 12 weeks, calculating the mass reduction rate, drawing a regression curve of the mass reduction rate of the wet tissue sample and the time, and judging whether the mass reduction rate is linearly related to the time;
and C: and if the mass reduction rate is linearly related to the time, calculating the mass reduction rate of the wet tissue sample after 3 years based on the regression curve, and if the mass reduction rate meets the expected requirement of the 3-year effective period, preliminarily judging that the recommended effective period of the wet tissue product is 3 years.
2. The method as set forth in claim 1, wherein in the step C, the recommended expiration date of the wet towel product is preliminarily determined to be 3 years, the stability test is continued for 36 weeks, and whether the expiration date of the wet towel product is 3 years is determined based on the stability test data of the other stability test items over a period of 36 weeks.
3. The determination method according to claim 1, wherein in the step B, if the correlation coefficient R of the regression curve is not less than 0.99, it is determined that the mass reduction rate is linearly related to time; otherwise, continuing to perform the stability test for 36 weeks, and judging whether the effective period of the wet tissue product is 3 years or not according to the stability test data of other stability test items within the period of 36 weeks.
4. The method as set forth in claim 1, wherein in the step C, if the mass reduction rate meets the expected requirement, the stability test data of other stability test items in 12 weeks are referenced, and if the stability test data of other stability test items has no variation trend of serious deviation, the validity period of the wet tissue product is determined to be 3 years; otherwise, the stability test is terminated and the shelf life of the wet wipe product cannot be judged as 3 years.
5. The determination method according to claim 1, wherein the mass reduction rate in step B is calculated by the formula:
the mass reduction rate at a certain point is (initial mass-product mass at a certain point)/initial mass × 100%.
6. The method of claim 1, wherein the step C, the expected requirement for a 3-year validity period further comprises: the liquid content of the wet tissue product is more than or equal to 1.7 times after 3 years.
7. The method of claim 4, wherein the other stability test items include weight, wet wipe appearance, squeeze appearance, odor, pH, in-label color, package integrity, package sealability, and microbial limit.
8. The method according to claim 7, wherein the trend of the stability test data of the other stability test items without serious deviation is:
weight: within ± 8% of the initial weight of the product;
wet tissue appearance, extrusion fluid appearance, odor, pH, inner label color: no significant change compared to week 1;
packaging integrity: the conditions of damage and non-setting adhesive falling are avoided;
packaging sealing property: the package is pressed by hand without air leakage;
the microbial limit: the total number of aerobic bacteria colonies is less than 100cfu/g, and the total number of yeast and mould colonies is less than 10 cfu/g; gram negative bacteria and staphylococcus aureus were not detected.
9. The determination method according to claim 1, wherein the method comprises an accelerated test A, an accelerated test B, a room temperature test, a light test, a low temperature test, and a temperature cycle test, wherein,
the accelerated test A is to place a wet tissue sample at the temperature of 38-42 ℃ and the relative humidity of 70-80%, sample at different time points and determine a stability detection item;
the accelerated test B is to place the wet tissue sample at the temperature of 54-57 ℃, sample at different time points and determine a stability detection item;
the room temperature test is to place a wet tissue sample at room temperature, sample at different time points and determine a stability detection item;
the illumination test is to place the wet tissue sample in the indoor windowsill under the natural illumination condition, sample at different time points and determine the stability detection item;
the low-temperature test is to place a wet tissue sample at the temperature of 2-8 ℃, sample at different time points and determine a stability detection item;
the temperature cycle test refers to that a wet tissue sample is placed under a variable temperature condition, samples are taken at different time points, and stability detection items are determined, wherein the variable temperature condition refers to that the temperature lasts for 12 hours at 21-25 ℃, 24 hours at-15 ℃, 12 hours at 21-25 ℃ and 24 hours at 43-47 ℃ in sequence, and the conditions are cycled.
10. The method for determining according to claim 7, wherein the method for measuring the microbial limit comprises:
step S1, adding the wet tissue sample into the solution D to prepare a test solution;
step S2, filtering the test solution by using a filter membrane, flushing the filter membrane by using a solution D, and detecting the total number of aerobic bacteria and the total number of mould yeasts in the filtrate;
step S3, preparing a primary enrichment fluid A from the test fluid in the step S1, and detecting staphylococcus aureus, escherichia coli and pseudomonas aeruginosa in the primary enrichment fluid A;
and step S4, preparing the initial enrichment liquid B from the test solution obtained in the step S1, and detecting salmonella in the initial enrichment liquid B.
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