CN113447356B - Method and equipment for testing mechanical properties of soft capsule shell - Google Patents
Method and equipment for testing mechanical properties of soft capsule shell Download PDFInfo
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- CN113447356B CN113447356B CN202110784971.XA CN202110784971A CN113447356B CN 113447356 B CN113447356 B CN 113447356B CN 202110784971 A CN202110784971 A CN 202110784971A CN 113447356 B CN113447356 B CN 113447356B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/02—Details
- G01N3/04—Chucks
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
- G01N5/045—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder for determining moisture content
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0001—Type of application of the stress
- G01N2203/0003—Steady
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0014—Type of force applied
- G01N2203/0016—Tensile or compressive
- G01N2203/0017—Tensile
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/006—Crack, flaws, fracture or rupture
- G01N2203/0067—Fracture or rupture
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/026—Specifications of the specimen
- G01N2203/0262—Shape of the specimen
- G01N2203/0266—Cylindrical specimens
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/0605—Mechanical indicating, recording or sensing means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/067—Parameter measured for estimating the property
- G01N2203/0682—Spatial dimension, e.g. length, area, angle
Abstract
The invention discloses a method and equipment for testing the mechanical properties of a soft capsule shell, belonging to the technical field of medical capsules. The test method comprises the following steps: standing the capsule shell with the humidity of 32-48% for 20-60min at 20-22 ℃ in an environment with the relative humidity of 35 +/-5%, cutting, and cutting into long strips to obtain a sample to be detected; the middle of two ends of a stable clamp at two sides of a sample is clamped, the longitudinal axis of the sample is superposed with the central lines of the clamp at the two ends, the capsule skin is kept horizontal, and the initial length L of a marking line is recorded0Drawing at the constant speed of 250-350mm/min, stopping drawing when the sample is cracked, recording the length L of the marked line at the position, and recording the elongation at break (L-L)0)/L0100%. The method can amplify the difference of the fracture elongation rate among the capsule skin samples, obviously distinguish the unqualified capsule skin samples, and is beneficial to the quality control of the capsule skin.
Description
Technical Field
The invention belongs to the technical field of medical capsules, and particularly relates to a method and equipment for testing mechanical properties of a soft capsule shell.
Background
The soft capsule is a dosage form which is formed by encapsulating a solution, a suspension, an emulsion or a semisolid serving as a content by a capsule shell, and is widely applied to health care products and medicines. The soft capsule is prepared by pressing and dripping. The capsule shell has gelling characteristic and plasticity, can realize the inclusion of the soft capsule when the capsule shell is heated to reach the melting temperature, and recovers harder strength after drying. The pressing method has higher requirements on the capsule skin than the dripping method, and the capsule skin of the soft capsule has the most obvious change at the joint seam because of the influences of moisture migration, contents, environmental temperature and humidity, rubber aging and the like in the storage period of the product, and the phenomenon of thinning and even pinhole-shaped leakage can occur. The mechanical strength of the capsule shell provides structural support for the soft capsule after molding to a certain extent, and the better capsule shell can reduce adverse effects of temperature, humidity, contents and the like on the soft capsule.
At present, most of the health products and the medicine soft capsules are gelatin soft capsules. Gelatin is a hydrophilic protein formed by incomplete degradation of collagen in connective tissues such as animal skin and bone, and is derived from a complicated source. In the same gelatin boiling process, gelatin raw materials of different manufacturers are used, the uniformity of the product is fluctuated, and the soft capsule quality expression characteristics are different. Sometimes, different contents are required for forming the capsule shell.
In the production of soft capsules, the prescription, preparation process and performance of the capsule skin of the soft capsules have a decisive role on the quality of finished soft capsule products, and parameters such as dynamic viscosity of glue solution, water content of the glue solution, thickness of the capsule skin, difference of pill loading and the like are commonly used as process indexes when the quality of prepared pills is controlled at present. Different glue formulations, such as the use of different plasticizers, can result in different skin strengths and can cause variations in the operating parameters of the pellet mill during the pelletization process. Soft capsules are unacceptable if the capsule shell leaks, sticks, disintegrates, overrun, etc. during pelleting or shelf life. It is necessary to increase the strength of the capsule shell, and provide a basis for the quality analysis of the soft capsule and the preparation process parameters.
Since the soft capsule is small and cannot be subjected to mechanical tensile test at the seam, the capsule skin is used as a sample for research. Referring now to the existing papers, only the papers mentioned and specifically referenced GB/T1040.1-2006[1] (e.g. Schhong, Su Yi, Van super spring, Lin Fu Lin, Zhang Na, response surface method optimized plant compound soft capsule shell formulation [ J ]. Guangzhou chemical, 2019,47(22):67-72.), is a national standard for the determination of tensile properties of plastics. The used equipment is an electronic universal tester which is suitable for products with higher tensile strength, such as plastics, metals and the like. The standard has weak pertinence, can only measure the approximate breaking elongation of the dry capsule skin, has low precision, has small difference on the breaking elongation of the gelatin type dry capsule skin prepared by the same method, and can not realize identification and screening.
In view of the above, the invention designs a method and a device for testing the mechanical properties of a soft capsule shell, which can examine the properties of the capsule shell during pill making and provide a reference basis for timely screening out unqualified capsule shells.
Disclosure of Invention
The invention aims to solve the problem that the existing measurement method used in the standard and research can not realize the requirement of screening the capsule skin prepared by the same method, and aims to provide a method and equipment for testing the mechanical property of the capsule skin of the soft capsule so as to examine the performance of the capsule skin and screen the capsule skin during the process of preparing pills. The inventor unexpectedly discovers in experimental exploration that the gelatin dry capsule shells prepared by the same method have small difference in the breaking elongation, and the wet capsule shells with certain humidity can have larger difference in the breaking elongation, so that effective distinction can be realized.
In order to achieve the purpose, the technical scheme of the invention is as follows:
in one aspect, the invention provides a method for testing the mechanical properties of a soft capsule shell, which comprises the following steps:
(1) standing the capsule shell with the humidity of 32-48% for 20-60min at 20-22 ℃ in an environment with the relative humidity of 35 +/-5%, cutting, and cutting into long strips to obtain a sample to be detected;
(2) firmly clamping two sides of a sample in the middle of two ends of a clamp, coinciding the longitudinal axis of the sample with the central lines of the clamps at the two ends, keeping the capsule skin horizontal, and recording the initial length L of a marking line0Drawing at the constant speed of 250-350mm/min, stopping drawing when the sample is cracked, recording the length L of the marked line at the position, and recording the elongation at break (L-L)0)/L0*100％。
The key of the invention is to select the wet capsule skin for measurement, and the humidity of the capsule skin is a key factor influencing the stretching result, preferably, in the step (1), the humidity of the sample to be measured is 35-40%. Different humidity of the capsule skin can be caused by different prescriptions, different processes and different drying degrees, and experiments prove that the capsule skin cannot be effectively screened if the humidity is too high or too low.
In the invention, the humidity of the capsule skin refers to the mass fraction of the water in the capsule skin, and the humidity of the capsule skin can be measured by an oven method for example: taking 1g of a test sample in a fragment shape not exceeding 3mm, spreading the test sample in a flat weighing bottle with constant drying weight, precisely weighing, and opening a bottle cap to dry in an oven at the temperature of 100-; and (3) placing in a dryer for cooling for 30 minutes, precisely weighing, drying at the temperature for 1 hour, placing in a cooler and weighing until the difference between two successive weighing is not more than 5 mg. And calculating the water content according to the weight loss reduction amount. In order to ensure that the humidity of the sample does not change during the measurement period, the sample needs to be completely wrapped by a plastic sample bag, placed in a sealed box and stored in a cool and dry place.
Further examples are tests using rapid moisture determination: a halogen rapid moisture meter was used. Taking 2g of a chip-shaped test article, and flatly paving the chip-shaped test article on a sample plate; setting the heating temperature to 140 ℃ and the heating time to 5min, and automatically displaying the moisture content of the sample on a display screen after heating is finished.
When the existing wet bag skin is cut at equal intervals, unsmooth or small gaps are easy to appear on the edges of the sample, and the stretching result is influenced to a certain extent by the gaps, so the sample is placed for 20-60min at the temperature of 20-22 ℃ and the relative humidity of 35 +/-5% after sampling, and then the cut is carried out. The placing time of the capsule skin with good toughness is short, and the placing time of the capsule skin with poor toughness is long. The placing environment can be any independent setting environment conditions between 20 ℃ and 22 ℃ and between 35 +/-5% of relative humidity, such as 20 ℃, 20.5 ℃, 21 ℃, 21.5 ℃, 22 ℃ and the like, for example, 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39%, 40% of relative humidity and the like, and can also be changed in the range in the experimental process without affecting the technical effect of the application.
Preferably, in the step (1), before standing, the capsule shells with the left and right sides parallel are cut from a pelleting press, the length is more than 30cm, the width is more than 20cm, and the capsule shells are respectively paved on a smooth hard plane and stand.
Preferably, in step (1), the cutting is performed in the longitudinal and transverse directions, respectively.
Longitudinal and transverse refer to: the direction of the capsule skin of the pill pressing machine is longitudinal, and the direction horizontal to the capsule skin is transverse. The soft capsule has oil leakage generally at the joint, and the joint changes in longitudinal and transverse directions due to the factors of the soft capsule such as tension, moisture migration, environmental temperature and humidity, and rubber crosslinking, so that the prepared capsule shell is sampled and tested in the longitudinal and transverse directions of the capsule shell of the pill press.
The slit strips should be easy to stretch by the machine and help to distinguish the breaking tension between strips of different properties. Preferably, in step (1), the cut strips have a width of 15mm and a length of 200mm, and the edges are smooth and have no gaps.
Preferably, in step (2), in order to prevent the sample from slipping off during stretching, a certain length is reserved on both sides of the sample except for the parts fixed on the clamp, so as to observe whether the phenomenon of slipping off or moving in the clamp occurs. Preferably, in the step (2), the constant-speed drawing speed is 300 mm/min. The sample slipped off during the pulling process or broke in the jig and needed to be retested.
In still another aspect, the present invention provides the use of the above test method in the quality control of soft capsules.
Preferably, the content of the soft capsule is a solution content, a suspension content, an emulsion content or a semisolid content, and more preferably a traditional Chinese medicine suspension content or a water absorption content.
The contents of the solution generally refer to water-insoluble liquids such as vitamin E soft capsules, alfacalcidol soft capsules, and the like;
the suspension contents refer to: the content is a certain amount of solid dispersed and suspended in oil-soluble solution, such as common cold soft capsule, vitamin C Yinqiao soft capsule, Xinnaoqing soft capsule, etc.;
the emulsion content means that a water-soluble substance is dispersed in an oil-soluble liquid, such as diphenhydramine hydrochloride soft capsules;
the semisolid content refers to a content with a large solid amount and is semisolid, such as water-absorbing content soft capsules, propolis soft capsules, compound lecithin soft capsules and the like.
Finally, the invention provides equipment used in the testing method, as shown in fig. 1, comprising a bag leather clip 1, a bag leather clip 2, a stretching screw rod, a positioning screw rod and a scale;
wherein, the bag leather clamp 1 is a fixed clamp, and the bag leather clamp 2 is a movable clamp.
stretching the screw: the device is used for horizontally pulling the capsule leather clamp 2 (movable clamp) and the scale so that the capsule leather is gradually and horizontally stretched under the driving of the capsule leather clamp 2 (movable clamp);
positioning a screw rod: the device is used for fixing the position of the stretching screw rod to enable the reading of the stretching screw rod to be stable;
a scale: the device is used for reading the stretching distance at the instant of the bag skin stretch breaking.
Preferably, the capsule clamps 1 and 2 are clamped by air pressure or hydraulic pressure, and further preferably, the air pressure is used for clamping.
The invention has the beneficial effects that:
(1) the thickness unevenness can influence the stretching result of the capsule skin, particularly, if the thickness change in the transverse direction is large, the stretching data can also be greatly changed.
(2) The invention uses the wet capsule skin for testing, overcomes the defect of low difference of the breaking elongation of the dry capsule skin prepared by the same method in the prior art, can enlarge the difference of the breaking elongation among the capsule skin samples, obviously distinguishes unqualified capsule skin samples, and is beneficial to the quality control of the capsule skin.
(3) The electronic tension testing machine in the prior art adopts a screw clamp to fasten a sample, the clamp is composed of two pieces of metal, the capsule skin is easy to slip in a test, particularly, when a dry capsule skin test is carried out, due to the fact that the tension is large, the screw clamp loosens in the stretching process, the sample in the clamp can be thinned, and the accuracy and repeatability of data are seriously influenced.
Drawings
FIG. 1 is a schematic diagram of a test apparatus of the present invention;
wherein, 1-bag leather clip 1, 2-bag leather clip 2, 3-positioning screw rod, 4-stretching screw rod, 5-scale.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way. The following is merely an exemplary illustration of the scope of the invention as claimed, and various changes and modifications of the invention of the present application may be made by those skilled in the art based on the disclosure, which also fall within the scope of the invention as claimed.
The present invention will be further described below by way of specific examples. The various chemicals used in the examples of the present invention were obtained by conventional commercial routes unless otherwise specified.
The type of the glue melting tank is as follows: HJG-700A;
the type of the pelleting press: YWJ 250-I.
Detection of capsule skin samples of different raw materials
1. The capsule shell samples of the invention were all prepared according to the following method:
preparing glue solution: adding gelatin (with freezing force of 150Bloomg, purchased from manufacturer A), plasticizer (glycerol) and water according to the mass ratio of 100:35:100 of gelatin, glycerol and water, stirring in a gelatin melting tank, heating to 70 ℃ to completely melt the gelatin, defoaming in vacuum, stirring uniformly, and filtering. And (4) after the glue solution is put into a glue storage barrel, keeping the temperature at 60 ℃ for 3-4 hours for later use.
Preparing a capsule shell: the pelleting machine is started to prepare capsule shells on the left side and the right side when pelleting room temperature is 20-22 ℃, relative humidity is 35 +/-5%, spraying body temperature is 40 ℃, glue box temperature is 65 ℃, and drum wheel refrigeration is 20 ℃, capsule shell thickness is measured by a micrometer thickness gauge, and the capsule shell thickness is between 0.60-0.88 mm.
2. The soft capsule of the invention is prepared by the following method:
preparing capsule shell according to the above method, and respectively preparing suspension soft capsule and vitamin E soft capsule with contents of 20% lecithin (the balance of vegetable oil and water soluble solid) by pressing method, each producing hundred thousand capsules. The preparation method and parameters of the product with the same content are completely consistent.
The preparation process of the suspension soft capsule containing 20% lecithin comprises the following steps:
the lecithin, the water-soluble solid and the vegetable oil are ground to be fine by a colloid mill and pass through a 120-mesh sieve to form a content; pelleting: pressing at room temperature of 20-22 deg.C, relative humidity of 35 + -5%, spraying body of 40-45 deg.C, rubber box of 65-75 deg.C, drum wheel refrigeration of 20-25 deg.C, and liquid medicine box insulation of 35-38 deg.C; and (3) drying: drying in a drying cage at room temperature of 20-25 deg.C and relative humidity of 35 + -5% for 24 hr until the water content of the soft capsule is not more than 12%;
the vitamin E soft capsule preparation process comprises the following steps:
vitamin E and vegetable oil are mixed evenly according to the prescription amount to form a content; pelleting: pressing at room temperature of 20-22 deg.C, relative humidity of 35 + -5%, spraying at 30-40 deg.C, rubber box at 60-70 deg.C, and drum wheel refrigerating at 20-25 deg.C; and (3) drying: drying in a drying cage for about 22 hours at the room temperature of 20-25 ℃ and under the relative humidity of 35 +/-5 percent until the moisture of the soft capsule is not more than 12 percent;
3. the gelatin was replaced with gelatin having a freezing force of 150Bloom g purchased from manufacturer B, and the steps 1 and 2 were repeated.
The oil leakage rate of the obtained soft capsule has the following statistical results:
table 1.
Example 1 Strength Performance test of Wet Capsule skin
The test equipment is shown in the attached figure 1 and comprises a bag leather clamp 1, a bag leather clamp 2, a stretching screw rod, a positioning screw rod and a scale; wherein, the bag leather clamp 1 is a fixed clamp, and the bag leather clamp 2 is a movable clamp.
(1) Cutting parallel capsule skin at left and right sides from a pill press, wherein the length is 36cm, the width is 25cm, respectively spreading on a smooth hard plane, standing for 30 minutes, drying the wet capsule skin at 20-22 ℃ under the environment of 35 +/-5% of relative humidity until the humidity is 35-45%, pressing the capsule skin outlet direction of the pill press (the capsule skin outlet direction is longitudinal, and the direction horizontal to the capsule skin outlet direction is transverse), respectively cutting with a special cutter at equal intervals in longitudinal and transverse directions to obtain strips with the width of 15mm and the length of 200 mm. The sample edges must be smooth and unnotched;
a section of left and right capsule skin is a group, longitudinal 6 samples and transverse 6 samples are obtained in parallel left and right, and a section of left and right capsule skin is cut according to the method to prepare two groups of capsule skin samples;
the two groups of capsule shell samples respectively comprise 12 longitudinal samples and 12 transverse samples, and 24 samples for later use.
(2) Taking a sample, wiping off surface lubricating oil, adjusting the movable clamp to a proper position to enable the distance between the two bag leather clamps to be in accordance with the length of a bag leather to be detected, placing the bag leather on the fixed clamp and the movable clamp, and communicating compressed air to enable the air cylinder to drive the clamp plate to move downwards to press the bag leather. The pressure of the bag clamp can be adjusted and read through a pressure adjusting valve at the front end of the air cylinder. In order to prevent the sample from slipping during stretching, a certain length is reserved at the two ends of the capsule skin except for the parts fixed on the clamp, so that whether the phenomenon of slipping or moving in the clamp occurs or not can be observed conveniently; keep the capsule skin level without local degeneration or distortion. The initial length before drawing is 30mm, and the initial length L of the marked line is recorded0The drawing was started at a constant speed of 300mm/min, and when the sample broke, the drawing was stopped, and the distance L from the mark line at that position was recorded, and the elongation at break was (L-L)0)/L0*100％；
And (3) the samples are slipped or broken in the clamp in the drawing process and need to be tested again, and after 24 samples are measured, the arithmetic mean value of the breaking elongation is obtained, namely the final result. The capsule shells prepared from the two gelatins were tested separately.
And (3) thickness testing:
the method comprises the following steps: a horizontal sample to be measured is taken, a micrometer thickness gauge is used, the sample is horizontally placed on a clamping opening of the thickness gauge, the thickness gauge needs to be calibrated to return to zero before use, and two effective numbers are taken from read data. (all the examples and comparative examples were thickness-measured by this method)
The measured thicknesses of the 12 transverse test samples of example 1 (for example capsule shells made from gelatin from manufacturer B) are shown in the table below:
table 2.
Tensile at break results:
calculation examples: the initial length of the strip to be measured before drawing is 30mm, and the initial length L of the marking line is recorded030mm, when the specimen broke, the drawing was stopped, and the position was recorded at a length L of 90mm from the gauge line according to the elongation at break (L-L)0)/L0Calculated as 100%, the elongation at break was 200%.
The maximum and minimum values of the measured 24 elongations at break were 390.1%, 277.5%, respectively, and it was found that the elongation at break distribution was uniform.
The results are as follows:
table 3.
It can be seen that the capsule shells prepared by the same method have obvious performance difference due to different gelatin manufacturers, and the wet capsule shells are detected to have the fracture elongation rates of 213.1% and 333.8%, which are large in difference and easy to distinguish, and are consistent with the oil leakage rate detection result in actual production.
Comparative example 1 detection of Strength Properties of Dry Capsule skin
The difference from the example 1 is that the wet capsule skin is dried for 24 hours at the temperature of 20-22 ℃ and the relative humidity of 35 +/-5 percent until the humidity of the capsule skin is below 8 percent, and the rest is in parallel with the same method. The capsule shells prepared from the two gelatins were tested separately.
And (3) thickness testing:
the thicknesses of the 12 transverse test samples (for example capsule shells made from gelatin from manufacturer a) of comparative example 1 were measured as shown in the table below:
table 4.
It can be seen that the difference in thickness of the dry capsule skin is large.
Tensile at break results:
the maximum and minimum values of the measured elongation at break of 24 pieces were 226.8% and 150.7%, respectively, and it was found that the elongation at break distribution was uniform.
Table 5.
It can be seen that, when the capsule shells of the gelatin of two manufacturers prepared by the same method are detected by adopting dry capsule shells, although the two capsule shells have certain difference in thickness, the breaking elongation rates are 166.2% and 181.0%, respectively, and the difference is not large, so that the capsule shells are difficult to distinguish by judging only from the breaking elongation rate.
Comparative example 2 Strength Property test of overwet Capsule skin
The difference from example 1 is that the wet capsule skin is prepared from gelatin from manufacturer A with a moisture content of 50-52%, and the rest is carried out in parallel.
Thickness test results:
table 6.
Tensile at break results:
the first set of 6 longitudinal samples tested was tested as follows:
314.3％、385.7％、191.0％、210.0％、281.4％、328.6％。
it can be seen that the thickness distribution of the over-wet capsule skin is relatively uniform, but the difference of the breaking tensile rate is relatively large, and the maximum value and the minimum value are 385.7% and 191.0% respectively, and the difference is relatively large.
Second, detection of capsule skin samples of different prescriptions and boiled gelatin
Preparing glue solution C: adding gelatin, plasticizer (glycerol) and water at a ratio of 100:35:100 into gelatin melting tank, stirring, heating to 70 deg.C to completely melt gelatin, vacuum defoaming, stirring, and filtering. And (4) after the glue solution is put into a glue storage barrel, keeping the temperature at 60 ℃ for 3-4 hours for later use.
Preparing glue solution D: taking gelatin, a plasticizer (glycerol) and water, mixing the gelatin, the glycerol and the water according to a ratio of 100: 40: feeding at a ratio of 100. Adding glycerol and water into gelatin melting tank, stirring, heating to 60 deg.C, adding gelatin, stirring, standing, maintaining temperature to completely dissolve gelatin, vacuum defoaming, stirring, and filtering. And (4) after the glue solution is put into a glue storage barrel, keeping the temperature at 55 ℃ for 3-4 hours for later use.
The raw materials are all from the same manufacturer.
The test procedure was as described in example 1 and comparative example 1, with the results as follows:
table 7.
The suspension soft capsule containing 20% lecithin is prepared by pressing the two capsule shells respectively, wherein the oil leakage rate of 10 ten thousand pills prepared from the capsule shell C is 0.003%, and the oil leakage rate of 10 ten thousand pills prepared from the capsule shell D is 0. It can be seen that the method can obviously detect the performance difference of the capsule skin caused by different processes and prescriptions.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A quality control method of a soft capsule shell is characterized by comprising the following steps:
(1) standing the capsule shell with the humidity of 32-48% for 20-60min at 20-22 ℃ in an environment with the relative humidity of 35 +/-5%, cutting, and cutting into long strips to obtain a sample to be detected;
(2) firmly clamping two sides of a sample in the middle of two ends of a clamp, coinciding the longitudinal axis of the sample with the central lines of the clamps at the two ends, keeping the capsule skin horizontal, and recording the initial length L of a marking line0Drawing at the constant speed of 250-350mm/min, stopping drawing when the sample is cracked, recording the length L of the marked line at the position, and recording the elongation at break = (L-L)0)/ L0*100%。
2. The method according to claim 1, wherein in step (1), the sample to be tested has a humidity of 35-40%.
3. The method according to claim 1, wherein in the step (1), before standing, the capsule shells with parallel left and right sides are cut from the pelleting machine, the capsule shells are longer than 30cm and wider than 20cm, and are respectively laid on a smooth hard plane for standing.
4. The method of claim 1, wherein in step (1), the cutting is performed by longitudinal and transverse cutting, respectively, and the cut strips have dimensions of 15mm wide and 200mm long.
5. The method of claim 1, wherein in the step (2), the sample is retained at both sides except the portion fixed to the holder for a predetermined length.
6. The method according to claim 1, wherein in the step (2), the constant-speed drawing speed is 300 mm/min.
7. Use of the quality control method according to any one of claims 1 to 6 for quality control of soft capsules.
8. Use according to claim 7, wherein the contents of the soft capsule are solution contents, suspension contents, emulsion contents or semisolid contents.
9. The use of claim 8, wherein the contents of the soft capsule are traditional Chinese medicine suspension contents or water-absorbing contents.
10. The apparatus for use in the quality control method according to any one of claims 1 to 6, comprising a bladder clamp I, a bladder clamp II, a stretching screw, a positioning screw and a scale; wherein, the first bag leather clamp is a fixed clamp, and the second bag leather clamp is a movable clamp; the first bag leather clamp and the second bag leather clamp are used for clamping and fixing two ends of the bag leather; the stretching screw is used for horizontally pulling the second bag leather clamp and the scale so that the bag leather is gradually and horizontally stretched under the driving of the second bag leather clamp; the positioning screw is used for fixing the position of the stretching screw so that the reading is stable; the scale is used for reading the stretching distance at the instant of the bag skin stretch breaking; the first bag leather clamp and the second bag leather clamp are clamped by air pressure or hydraulic pressure.
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| CN202110784971.XA CN113447356B (en) | 2021-07-12 | 2021-07-12 | Method and equipment for testing mechanical properties of soft capsule shell |
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| CN202110784971.XA CN113447356B (en) | 2021-07-12 | 2021-07-12 | Method and equipment for testing mechanical properties of soft capsule shell |
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