JP4719586B2 - Tackiness measuring method and measuring apparatus - Google Patents

Description

  The present invention relates to a method and an apparatus for evaluating the tackiness of a patch such as a patch or plaster applied to the skin.

  Currently, patches such as poultices and plasters that are applied to the skin are widely used. These patches are applied to the skin to absorb the drug percutaneously, and adhesion to the skin (adhesiveness) is an important issue. In particular, tackiness is important among tackiness, meaning tackiness that adheres to an adherend in a short time with a light force. If the tackiness is weak, a phenomenon occurs in which the patch falls off or peels off at the time of use, and therefore the adhesiveness of various patches has been studied.

  For example, Patent Document 1 below discloses a cataplasm having excellent usability, which imparts elasticity to a hydrous plaster (adhesive) to reduce skin irritation and prevent stickiness after peeling. .

  Further, as a method for testing the tackiness of such a patch, the following Patent Document 2 describes an evaluation method based on the ball tack method (JIS Z 0237), and Patent Document 3 describes a probe tack method (ASTM-D). -2979) is described.

On the other hand, Patent Literature 4 below discloses a strain measuring device using a strain gauge, for example, for measuring a large strain such as a rubber material used for a tire.
Japanese Patent No. 3044352 JP-A-8-53346 JP 2001-328935 A JP-A-9-159401

  However, the poultice of Patent Document 1 may cause problems such as the skin application surfaces of the poultice sticking to each other and not peeling off during use, and inconvenience may be felt in terms of handling.

  Further, in the tackiness evaluation methods of Patent Documents 2 and 3, it is good to evaluate the strong adhesive strength of industrial adhesive tapes and the like, but a patch having a weak adhesive strength applied to human skin (such as a patch). In this case, it was not possible to accurately evaluate the adhesiveness to the skin and the adhesiveness (adhesiveness) between patches. In addition, the methods for evaluating tackiness in Patent Documents 2 and 3 are not sufficient in terms of correlation with actual sensory tests. In practice, the adhesiveness with the skin surface and the adhesiveness between the adhesive surfaces are evaluated. Whereas there was no test device that could use skin samples.

  The present invention has been made in view of the above problems, and its purpose is highly correlated with sensory evaluation (which sufficiently reflects the actual adhesive state), a method for testing the tackiness of a patch, and a method therefor It is to provide an apparatus to be used.

  More specifically, the present invention provides the following.

  (1) A tackiness measuring method for measuring the tackiness of a patch, wherein the first support is supported with the tack surface of the patch facing outside, and the tack surface to be tacked is facing outside. The first support and the second support from the point where the second support to be supported is separated from each other after being brought into point contact with each other and then separated from each other and completely separated after starting the retreat. A tackiness measurement method for measuring a change in load applied to a contact point of a support and evaluating the tackiness of the patch by a pattern of the load change.

  According to the tackiness measuring method of the present invention, the tackiness is measured by changing the load applied to the contact point by bringing the tack surface of the patch and the tack target surface to be tacked into point contact instead of each other. Therefore, it is possible to measure the tackiness more accurately even in a sample that is not affected by the peripheral portion of the contact point and has a problem of a subtle difference in tackiness such as a patch. Moreover, since a patch and a tack target can be made small, a small sample and a skin piece can be used suitably. Furthermore, since it can be measured by using different types of patches on the first support and the second support, or using materials other than the patches, not only the tackiness between the patches and the patches but also the patches. The tackiness between the agent and the skin sample can also be evaluated.

  (2) Said 1st support body and / or said 2nd support body have a shape part curved convexly, said 1st support body and said 2nd support body are orthogonally crossed, and said 1st support body The tackiness measuring method according to (1), wherein the point contact is made in the vicinity of the apex of the convex portion of the second support.

  According to this aspect, since the first support and the second support can be easily brought into point contact, the tackiness can be accurately measured. Moreover, since the area of the circle of a contact part is dependent on the curvature radius and pressing force of a 1st support body and / or a 2nd support body, the area of a contact part can be estimated.

  (3) A flexible member is connected to the first support body or the second support body, and the member bends due to the point contact and the subsequent retreat, and the load change depends on the amount of the bend. (1) or the tackiness measuring method according to (2).

  According to this aspect, the change in load applied to the contact point is measured by replacing the amount of deformation (strain) of the flexible member provided on the support, so that one of the supports can be displaced. The tackiness can be evaluated in a form closer to the usage situation of the patch.

  (4) The tackiness measurement method according to any one of (1) to (3), in which a maximum load value from the start of reverse movement to the separation is obtained, and the tackiness is determined based on the maximum load value. (5) The tackiness measuring method according to any one of (1) to (3), wherein the tackiness is determined by an area surrounded by a load curve from the start of retreating to the separation and a baseline after the separation.

  According to this aspect, the tackiness can be easily evaluated by determining the tackiness based on the above maximum load value or area, and a high correlation with the skin sensory test can be obtained. .

  (6) Any of (1) to (5), wherein the patch is one or more selected from a patch, a plaster, a tape, a bandage, a sheet, a wound dressing, and a cosmetic pack. The tackiness measuring method described.

  According to the tackiness measuring method of the present invention, tackiness can be measured more accurately in the patch.

  (7) The tackiness measuring method according to any one of (1) to (6), wherein the patch is a poultice having a hydrous plaster layer.

  According to the tackiness measuring method of the present invention, a subtle difference in tackiness can be evaluated even in a cataplasm having a weak tackiness, such as a cataplasm having a hydrous plaster layer.

  (8) A tackiness measuring device for measuring the tackiness of a patch, comprising: a first support that supports the patch; a second support that supports a tack target to be tacked by the patch; A movement control means for reciprocating the first support or the second support, causing the first support and the second support to be brought into point contact from a mutually separated state, and then retracted and separated; And a load measuring means for measuring a load change applied to a contact point between the first support and the second support.

  According to the tackiness measuring apparatus of the present invention, the first support and the second support can be brought into point contact, and the tackiness can be measured by a load change applied to the contact point. More accurate tackiness can be measured. Moreover, since a patch and a tack target can be made small, a small sample and a skin piece can be used suitably. Furthermore, since it can be measured by using different types of patches on the first support and the second support, or using materials other than the patches, not only the tackiness between the patches and the patches but also the patches. The tackiness between the agent and the skin sample can also be evaluated.

  (9) Said 1st support body and / or said 2nd support body have a shape part curved in convex shape, make said 1st support body and said 2nd support body orthogonal, and said 1st support body The tackiness measuring device according to (8), wherein the point contact is made in the vicinity of the apex of the convex portion of the second support.

  According to this aspect, the first support and the second support can be easily brought into point contact. When the first support body and the second support body have a convexly curved shape portion, point contact can be made near the apex of the convex portion. Moreover, even if one has a convexly curved shape portion and the other is a flat surface, point contact can be made between the vicinity of the apex of the one convex portion and the other plane. Moreover, since the area of the circle of a contact part is dependent on the curvature radius and pressing force of a 1st support body and / or a 2nd support body, the area of a contact part can be estimated.

  (10) One of the first support and the second support is connected to one end of a flexible member, the other end of the member is fixed, and the member is provided with a strain gauge. The tackiness measuring device according to (8) or (9).

  According to this aspect, the amount of flexure of the flexible member provided on the support is measured by the strain gauge provided on the member, so that subtle load changes that differ depending on the measurement sample can be measured more accurately. it can.

  (11) The tackiness measuring apparatus according to (10), wherein the flexible member is formed of a phosphor bronze plate.

  According to this aspect, the phosphor bronze plate is suitably used as a flexible member because it has excellent spring properties, high strength, and good wear resistance.

  (12) The tackiness measuring apparatus according to (10) or (11), wherein the strain gauge is provided in a pair at least on the front side and the back side of the member.

  According to this aspect, since the amount of bending due to the axial force generated in the member can be canceled by the strain gauges provided on the front side and the back side, the accurate amount of bending can be measured.

  (13) The tackiness measuring device according to any one of (10) to (12), wherein the strain gauge is connected to a Wheatstone bridge circuit and measured by a 2 or 4 active gauge method.

  According to this aspect, a more accurate deflection amount can be measured by measuring by the 2 or 4 active gauge method.

  The tackiness measuring apparatus and measuring method of the present invention can test and evaluate the tackiness of a patch having a high correlation with the sensory evaluation (which sufficiently reflects the actual adhesive state). Furthermore, various objects such as animal skin can be used, and measurement can be performed by changing the object to be measured and the object according to the purpose.

  Hereinafter, although an example of an embodiment of the present invention is explained based on a drawing, the present invention is not limited to the following embodiment. In the following description of the embodiments, the same reference numerals are assigned to common components, and the description thereof is omitted or simplified.

<Tack measurement device>
〔overall structure〕
1 to 4 are diagrams showing an outline of the tackiness measuring apparatus according to the present invention, FIG. 1 is a front view showing the entire tackiness measuring apparatus according to the present invention, and FIG. 2 is a view of a support contact portion in FIG. FIG. 3 is an enlarged plan view, FIG. 3 is an enlarged view of the support contact portion in FIG. 1, FIG. 4 is an enlarged perspective view in the vicinity of the support contact portion, and FIG. 5 is an explanatory view showing a moving state of the support contact portion in the test. .

  As shown in FIG. 1, this tackiness measuring apparatus 100 mainly includes an X-axis stage supporter 10 and a Y-axis stage supporter 20. An arm 12 extending in the horizontal direction (X direction) extends from the upper part of the X-axis stage supporter 10 via an L-shaped jig 11, and from the tip of the arm 12, as shown in FIG. A total of four flexible members 40 each extending from left to right extend in the vertical downward direction (Y direction), and in the horizontal direction (X direction) so as to cross both ends of the member 40. A first support 60 is provided. A strain gauge 50 is disposed on the upper portion of the member 40.

  A wide jig 21 extending in the horizontal direction (X direction) is provided from the vicinity of the substantially central portion of the Y-axis stage supporter 20, and the second support body 61 is perpendicular to the tip of the jig 21. It is provided in the direction (Y direction). Further, a stepping motor 30 is provided on a pedestal portion below the Y-axis stage supporter 20. As a result, the entire Y-axis stage supporter 20 can also move in the Z direction, and the second support 61 in a state in which the second support 61 is disposed perpendicular to the first support 60. The first support body 60 and the second support body 61 can contact each other.

  Hereinafter, the main components of the tackiness measuring apparatus of the present invention will be described in more detail.

[First support, second support]
The 1st support body 60 is a site | part which attaches the patch 70 used as a measurement sample, and the 2nd support body 61 is a site | part which attaches the tack target 71. FIG. The shape of the first support body 60 and the second support body 61 is not particularly limited, but it is preferable that the first support body 60 and the second support body 61 have a formation portion that is curved in a convex shape such as a circle or an ellipse. In particular, a cylindrical shape (diameter 4 to 15 mm) as shown in FIG. 3 can be cited as a preferred example. Moreover, as shown in FIGS. 1-4, it is preferable that the 1st support body 60 and the 2nd support body 61 are installed so that it may become a cross shape, and the point contact may be carried out. In addition, the material of the 1st support body 60 and the 2nd support body 61 is not specifically limited, All are possible except the thing which deform | transforms easily, For example, things made from glass, ceramics, etc. can be used. .

[Flexible member]
The member 40 having flexibility is a portion that generates strain (deflection) during the test, and is directly or indirectly attached to the first support body 60. In FIG. 1 and FIG. 4, four members 40 are attached to the left and right, respectively, but the number of members 40 is not particularly limited, and the left and right ones may be a total of two or even one. Good. The member 40 is not particularly limited as long as it is flexible, but a plate-like member that is displaced by bending is preferable. For example, phosphor bronze plate, copper plate, rubber plate, synthetic resin plate, carbon steel plate, stainless steel A plate such as a steel plate, beryllium copper plate, or white plate is preferably used. Among them, the phosphor bronze plate is most suitable because it has excellent properties such as excellent spring property, high strength, and good wear resistance.

  The member 40 preferably has a thickness of 0.005 mm to 5 mm, more preferably 0.05 mm to 1.5 mm, and still more preferably 0.08 mm to 1.2 mm. If the thickness of the member 40 exceeds 5 mm, the amount of deflection may be small and the measurement accuracy may decrease. If the thickness of the member 40 is less than 0.005 mm, the amount of deflection is large, and the rotation of the patch 70 cannot be ignored and becomes unsuitable. There is. For example, in FIG. 4, a total of four phosphor bronze plates are attached to each end of the first support 60, each having two rectangular (5 mm × 50 mm, thickness 0.1 mm) members 40.

[Strain gauge]
The strain gauge 50 measures the amount of bending of the member 40 caused by the test, and is attached to the member 40. The position of the strain gauge 50 is not particularly limited, but is preferably provided on the upper portion of the member 40 on the side opposite to the portion to which the first support 60 is attached as shown in FIGS. . By providing in this part, a load change can be measured accurately from the amount of bending that has occurred, and it can be converted to tackiness. In addition, the strain gauge 50 is not specifically limited, A commercially available thing can be used.

[X-axis stage supporter]
The X-axis stage supporter 10 fixedly supports the member 40 to which the first support body 60 is attached. The X-axis stage supporter 10 is preferably movable so as to move the first support 60 in the X-axis direction. For example, in FIG. 1, the first support 60 can be translated in the horizontal direction (X direction) by the gauge 13. Thereby, the measurement part of the patch 70 can be shifted little by little. Therefore, there is no need to replace the patch 70, and measurement can be performed many times at a time.

[Y-axis stage supporter]
The Y-axis stage supporter 20 has the same purpose as the above-described X-axis stage supporter, and is used for fixing and supporting the second support 61. The Y-axis stage supporter 20 is not particularly limited, but is preferably movable so as to move the second support 61 in the Y-axis direction. For example, in FIG. 1, the second support 61 can be moved in the vertical direction (Y direction) along the gauge 24 by the dial 23. Therefore, there is no need to replace the tack target 71, and measurement can be performed many times at a time.

[Z-axis stage movable device (stepping motor)]
A stepping motor 30 that is a Z-axis stage movable device is a drive device for bringing the first support 60 and the second support 61 into contact with each other. In the present invention, the stepping motor 30 may be provided on either the X-axis stage supporter and / or the Y-axis stage supporter. For example, in FIG. 1, the stepping motor 30 is provided on the Y-axis stage supporter 20. When the second support 61 moves in the Z-axis direction, the first support 60 and the second support 61 to which the patch 70 is attached as shown in FIGS. It can be pressed and pulled apart, and the patch 70 can make point contact and measure tackiness.

<Measurement method>
Next, a tackiness measuring method using the tackiness measuring apparatus 100 will be described.

  First, the patch 70 is cut to an arbitrary size on the first support 60 shown in FIG. 1 and fixed with the surface to be measured (tack surface) on the outside. Further, the tack target 71 is cut to an arbitrary size on the second support 61 and fixed with the surface to be tacked outside. The tack target may be the patch 70 or animal skin or the like that becomes pseudo human skin. Further, in this embodiment, the first support 60 is a part to which the patch 70 to be a measurement sample is attached, and the second support 61 is a part to which the tack target 71 is attached. You may attach to the support body 61 and attach the tack object 71 to the 1st support body 60. FIG.

  Next, as shown in FIG. 1, the first support body 60 and the second support body 61 are attached to the flexible member 40 provided in the X-axis stage support device 10 and the Y-axis stage support device 20. Install. Then, using the stepping motor 30 which is a Z-axis stage movable device, the second support 61 is moved at a constant speed as shown in FIGS. After making point contact in a state where the 70s are orthogonal to each other and pressing for a certain period of time, they are retracted at a constant speed and separated.

  In this test method, the first support 60 and the second support 61 to which the patch 70 is attached can be contacted, pressed, and separated under any conditions. The numerical range is not particularly limited, but when testing a patch that is a water-containing patch, the advance speed at which the second support is brought into contact is preferably 0.05 to 1 mm / s, particularly 0.2 mm / s. preferable. The pressing load is preferably 0.1 to 30 gf, more preferably 1 to 20 gf, and still more preferably 10 gf. The pressing time is preferably 0 to 600 seconds, and more preferably 5 to 10 seconds. Further, the retreating speed is preferably 0.01 to 10.0 mm / s, more preferably 0.02 to 8.0 mm / s. By performing measurement within this numerical range, it is possible to accurately reflect the functionality. A test can be performed.

  At the time of separation, the first support 60 is pulled by the tackiness of the patch 70, and the member is distorted. The strain gauges 50 attached to the front and back surfaces of the member 40 are connected to the well-known 2-active gauge Wheatstone bridge circuit shown in FIG. 6 or the well-known 4-active gauge Wheatstone bridge circuit shown in FIG. In FIGS. 6 and 7, R1 to R4 are resistances), and the amount of deflection of the member 40 is measured by connecting it to a measuring device, and the contact between the first support 60 and the second support 61 is determined from this measurement. It is possible to measure the tackiness of the patch 70 by converting the load change applied to the points.

  FIG. 9 is a diagram showing a change in the load at the point contact point at the time of measurement. In the measurement method according to the present invention, the force generated at the time of separation after pressing under a certain condition is regarded as tackiness, and the positive Y-axis value (maximum load value from the start of retraction to the separation) in FIG. gf) is preferred. Further, the positive area represented by the hatched portion in FIG. 9 (the area of the positive part under the curve until the measured objects are completely separated) is measured as the work required for peeling (peeling work gf · mm). Can also be tacky. In the following embodiments, the above maximum load value is used as tackiness.

In summary, the typical test procedures are as described in the following procedures A) to H). However, the test procedure is not particularly limited to this procedure.
A) Arranged on the surface of the cylindrical first support with the tack surface of the patch facing outside,
B) Arranged on the surface of the cylindrical second support with the tack surface to be tacked facing outside,
C) A member having flexibility is connected to the first support, and the first support is displaceable by bending of the member.
D) In this state, the first support and the second support are arranged so as to be orthogonal to each other,
E) From the state where the second support is separated, the first support is brought into point contact at a forward speed of 0.2 mm / s,
F) After pressing for 5 seconds with a pressing load of 10 gf,
G) Retreat at a retreating speed of 0.02 to 8 mm / s (8 conditions of 0.02, 0.04, 0.1, 0.2, 0.4, 1, 2, 8 mm / s) Separate the support,
H) Measure each maximum load value for each of the 8 conditions from the start of reverse movement to the separation, and use the average value as tackiness.

  The first support body 60 and the second support body 61 are preferably installed so as to have a cross shape and are in point contact. In the case of point contact, the area (radius) of the circle of the contact portion depends on the radius of curvature of the first support 60 and / or the second support 61 and the pressing force. Therefore, when the patch 70 is brought into contact during the test, the area of the contact portion can be estimated by using point contact. In the case of point contact, more accurate tackiness can be measured without being influenced by the periphery of the measured object (sample). Moreover, since the area of a use site is small, even a small sample or skin piece can be used, it is preferable.

  Also, compared with the conventional measurement method, the conventional measurement method is surface contact, and contacts with the surface and comes off from the end with a line like a peel test (probe tack test). On the other hand, the measurement method according to the present invention is point contact, and after making a circular surface contact once around a point, it is likely that it deviates from the periphery of the contact surface toward the center of the point contact portion. Different. This is presumed to be one of the reasons for reflecting sensory evaluation.

  As the measurement method, it is preferable to use a 2-active gauge method in which the strain gauge 50 is provided at the target positions on both sides of the front and back surfaces of the member 40 as shown in FIG. Ideally, the deflection amount is a numerical value that has the same absolute value before and after the member 40 and has the opposite sign. However, since actual bending due to axial force occurs, different numerical values are shown. Therefore, by arranging the strain gauge 50 in such a manner, the bending strain is doubled, the deflection due to the axial force can be canceled out, and an accurate deflection amount can be measured.

In addition, the symbol in a formula shows the following words.
E _IN : Input voltage E _OUT : Output voltage R: Strain gauge resistance value ΔR: Strain gauge resistance change R ₁ : Strain gauge resistance value ΔR ₁ : Resistance value due to deformation of strain gauge member 40 Change amount L: initial length of member 40 ΔL: change amount due to deformation of member 40 ε: strain ε ₁ : strain of strain gauge of 1 K: strain rate of strain gauge (value specific to strain gauge used) In other words, the constant of the strain and resistance change of the strain gauge,
ε = (ΔL / L) = (ΔR / R) / K
It can be expressed by the relationship.

  Although the 1-active gauge method in which the strain gauge 50 is provided only on one side of the member 40 is possible, the absolute value cannot be evaluated because this method cannot eliminate the amount of bending in the axial direction. is there. Further, when the 4-active gauge method is used, the amount of deflection in the axial direction and the amount of deflection in the left-right direction can be canceled out, the output can be quadrupled, and the accuracy can be increased. The 4-active gauge method is also used when the difference in deformation between the left and right leaf springs cannot be ignored.

  Examples of the measurement object that can be used in this test method include patches such as poultices, plasters, tapes, adhesive bandages, sheets, wound dressings, and cosmetic packs. In particular, tackiness can be measured more accurately in a water-containing patch, and more effective in a patch that is a relatively weak tackiness patch.

  In addition to the above-mentioned patches, animal skins such as rats and mice, silicon films similar to the skin, human cultured skin, and the like can be used as objects that can be used.

  When only the patch is used, the tackiness between the adhesive surfaces of the patch can be measured. For example, it is possible to evaluate the ease of peeling when the patch (plaster surface) sticks. In addition, when a patch and other objects are used, their tackiness can be measured. For example, when a patch and animal skin are used, the patch's adhesiveness to the skin can be evaluated.

<Patch>
When measured by the measurement method of the present invention, it became clear that those satisfying both of the following conditions a) and b) would be ideal patches (such as poultices). A poultice which is an example of an ideal patch will be described. The poultice is formed by laminating a hydrous plaster layer on the surface of a support, and a release film that is peeled off during use may be further laminated. And both conditions a) and b) below are satisfied. The measurement conditions at this time are tackiness obtained by the measurement methods of the above procedures A) to H).

  a) When the plaster layers of the cataplasm are pasted and peeled off, the tackiness is 4 gf or less, preferably 2 to 3.8 gf, more preferably 2.5 to 3.5 gf. . This is because when the amount exceeds 4 gf, the plaster surfaces adhere to each other, and the plaster surfaces cannot be peeled apart.

  b) When the plaster layer of the cataplasm and the skin sample (stratum corneum) are bonded and peeled off, the tackiness is 5 gf or more, preferably 5 to 7 gf, more preferably 5.5 to 6 .5 gf. This is because when the tackiness is less than 5 gf, it cannot be applied to the plaster surface for a long time and is easily peeled off. In addition, as a skin sample (keratin layer) here, for example, isolated skin such as a hairless mouse or pig can be used. Alternatively, artificial skin (BIO SKIN (trade name): manufactured by Beaulux Co., Ltd.) or the like can also be used as an equivalent product thereof.

  In addition, the positive area (area of the positive part under the curve until the objects to be measured are completely separated) represented by the shaded area in FIG. 9 was measured as the work required for peeling (peeling work gf · mm). The tackiness in the case is 4.5 gf · mm or less when the plaster layers of the cataplasm are stuck together and peeled off. Furthermore, it is preferably 2 to 4 gf · mm, more preferably 2 to 3.5 gf · mm. If it exceeds 4.5 gf · mm, the plaster surfaces adhere to each other and cannot be peeled off. Further, when the plaster layer of the cataplasm and the skin sample (keratin layer) are bonded and peeled off, the peeling work is 3 gf · mm or more. Furthermore, it is preferably 3.2 to 6 gf · mm, and more preferably 3.5 to 4.5 gf · mm. When the peeling work is less than 3 gf · mm, it cannot be applied to the plaster surface for a long time, and is easily peeled off.

[Constituent components of hydrous paste]
The constituents of the hydrous plaster used in the poultice are not particularly limited, but those having tackiness capable of fixing the drug to the skin surface at room temperature for a long time are preferable. Water, thickener, wetting agent, filler In addition, a crosslinking agent, a polymerization agent, a solubilizing agent, an absorption accelerator, a medicinal effect aid, a stabilizer, an antioxidant, an emulsifier, a drug and the like are added as necessary.

[Thickener]
As the thickener used in the hydrous plaster, one that can stably hold water of 30% to 80% and has water retention is desirable. Specific examples thereof include acrylic polymers such as polyacrylic acid and sodium polyacrylate; natural polymers such as animal systems such as gelatin and collagen; cellulose systems such as methylcellulose, ethylcellulose, hydroxyethylcellulose, and sodium carboxymethylcellulose; carboxyvinyl polymers; Water-soluble polymers such as vinyl-based materials such as polyvinyl alcohol, polyvinyl pyrrolidone, and polyvinyl methacrylate; synthetic polymers such as polyethylene oxide, methyl vinyl ether, and maleic anhydride copolymers;

  In particular, as such a thickening agent, acrylic materials such as polyacrylic acid, sodium polyacrylate, and neutralized polyacrylic acid are preferably used in terms of strong gel strength and excellent water retention, and other gelatins. Are preferably used.

  The partially neutralized sodium polyacrylate is obtained by partially neutralizing and polymerizing acrylic acid and having a neutralization degree of 40 to 70%. The lower the degree of neutralization, the lower the aqueous solution pH and the stronger the tackiness of the patch. When the degree of neutralization is 40%, the tackiness when made into a patch is very strong, but slightly soluble in water. On the other hand, those having a neutralization degree of 70% are well soluble in water but have a slightly weak tack. Those having a neutralization degree of 50% are particularly preferred in terms of solubility in water, reactivity with aluminum, and tackiness when applied to the skin.

  The blending amount of acrylic substances such as polyacrylic acid, sodium polyacrylate, and polyacrylic partial neutralized product is preferably 2 to 10% by weight, more preferably 4 to 8% by weight of the total amount of the base. If it is less than 2% by weight, the shape retention is poor, and if it exceeds 10% by weight, the viscosity during the patch preparation process becomes too high and uniform kneading becomes difficult, and a desired patch base cannot be obtained. There is.

  Gelatin improves the persistence of stickiness during use of the patch. In addition, since it has a property of gelling when cooled, it effectively acts to prevent the patch from sticking out and from the support during the preparation process. The amount of gelatin is preferably 0.5 to 5% by weight, more preferably 1 to 3% by weight. By using this blending amount, the patch can maintain a tack property that lasts for a long time from the time of application until it is peeled off. If the blending amount is less than 0.5% by weight, the above effect is not exhibited, and if it exceeds 5% by weight, the gelatin gel becomes too strong and the tackiness of the patch surface becomes weak. Further, when applied to the skin, gelatin may be sol- lated at body temperature, and may peel off before exhibiting the inherent tackiness of gelatin.

[Wetting agent]
Examples of the wetting agent used in the hydrous plaster include polyhydric alcohols such as glycerin, propylene glycol, and sorbitol, and water candy, reduced maltose and water candy, and the like.

[filler]
Examples of the filler include kaolin, zinc oxide, talc, titanium, bennite, aluminum silicate, titanium oxide, zinc oxide, aluminum metasilicate, calcium sulfate, calcium phosphate, light anhydrous silicic acid, hydrous silicon dioxide, and the like.

[Solution aids, absorption enhancers]
As a solubilizer or absorption enhancer, N-methyl-2-pyrrolidone, propylene carbonate, crotamiton, l-menthol, mint oil, limonene, diisopropyl adipate, etc., methyl salicylate, glycolic salicylate, thymol, nonylic acid vanillylamide, red pepper extract N-methyl-2-pyrrolidone, l-menthol, thymol and the like are preferably used.

[Others]
If necessary, stabilizers, antioxidants, emulsifiers and the like may be added to the hydrous plaster.

  Moreover, in order to strengthen the hydrous plaster and to have water retention, a crosslinking agent, a polymerization agent, or the like may be added. Such a crosslinking agent and a polymerization agent can be appropriately selected according to the type of the thickener and the like.

  As the crosslinking agent, polyvalent metal compounds such as aluminum hydroxide, magnesium hydroxide, and aluminum sulfate are preferably used, and aluminum compounds are particularly used. As the aluminum compound, poorly water-soluble aluminum hydroxide is preferably used. In the presence of water, a partially neutralized sodium polyacrylate, and a poorly water-soluble aluminum compound are added to gelatin to act on the acid. Then, aluminum is gradually eluted, and the eluted aluminum reacts with sodium polyacrylate partially neutralized product and gelatin to form a homogeneous hydrous gel. At that time, by adjusting the crosslinking rate and degree of crosslinking, etc., the coating properties when applying the patch to the support during the production process, the water retention, adhesiveness, shape retention property, drug as the patch A base excellent in releasability can be formed.

[Drug]
What is necessary is just to mix | blend with the said hydrous plaster layer, when making a poultice hold | maintain a chemical | medical agent. Examples of such drugs include general anesthetics, sleep, analgesics, anti-inflammatory analgesics, steroid hormones, stimulants / stimulants, psychiatric agents, local anesthetics, skeletal muscle relaxants, autonomic agents, Allergic agent, antihistamine, cardiotonic agent, arrhythmic agent, diuretic, antihypertensive agent, vasoconstrictor, vasodilator, calcium antagonist, antibacterial agent, parasitic skin disease agent, emollient, antibiotic, antidote , Antitussives, antitussives, hypnotics, psychoactive agents, asthma agents, hormone secretion promoters, anti-ulcer agents, anticancer agents, vitamins, and those with whitening effects such as skin beautifying agents.

  The patch is usually provided in such a form that it is applied or spread on an appropriate support in advance, and further a release film or the like that can be peeled off at the time of use is attached to the application surface side. In such a case, as a support, arbitrary things, such as cloth, a nonwoven fabric, a plastic sheet or film, and paper, can be used.

[Support]
The support used for the patch is not particularly limited, but a block copolymer mainly composed of polyethylene terephthalate (PET), ethylene-vinyl acetate copolymer (EVA), polyethylene, polyester, polybutadiene, styrene-butadiene or styrene-isoprene. Polymer resin, butadiene-styrene-methyl methacrylate copolymer resin, nylon, polyurethane, alkoxyalkyl (meth) acrylate copolymer, polyvinyl acetal, polyamide, rayon, woven fabric, knitted fabric, nonwoven fabric, or a laminate thereof is preferable. Polyester nonwoven fabric and polypropylene nonwoven fabric are more preferably used.

  In addition, the thickness of the hydrous plaster layer laminated on the support in the patch is preferably 0.1 mm to 5 mm. If the thickness of the poultice exceeds 5 mm, the end of the poultice will be easily caught and peeled off at the time of application. On the other hand, if the thickness is less than 0.1 mm, the poultice will not be supportable and will tend to cause an application error. There is a tendency.

  In the poultice, a release film may be further laminated on the surface of the hydrous plaster layer. However, such a release film is not particularly limited, and a release-treated resin film, paper, etc. Is appropriately selected.

  EXAMPLES Next, although an Example and a comparative example are given and this invention is demonstrated concretely, this invention is not restrict | limited at all by these Examples.

<Example 1>
After adding a solution in which sodium carboxymethylcellulose is dispersed in glycerin to purified water, gelatin is added and dissolved. Next, a solution obtained by dispersing a partially neutralized sodium polyacrylate, sodium polyacrylate, aluminum hydroxide, and polyoxyethylene sorbitan trioleate in glycerin was added and kneaded sufficiently. Thereafter, a solution obtained by dissolving ketoprofen in N-methyl-2-pyrrolidone and l-menthol in advance is added, and components of pH adjuster, sodium edetate, thymol, and silicic anhydride are added and kneaded sufficiently, and the ketoprofen-containing ointment Got the body. The obtained plaster was spread on a polypropylene non-woven fabric (coating thickness 500 μm), covered with a polypropylene film and cut into 10 cm × 14 cm to prepare a poultice.

<Comparative Example 1-6>
In Comparative Examples 1 to 6, commercial products a, b, c, d, e, and f which are commercially available cataplasms were used.

<Test Example 1: Tackiness measurement test (between plaster layers)>
A rectangular 2.5 cm × 4 cm test piece was cut out from the central part of the cataplasm of Example 1 and Comparative Examples 1 to 6, and fixed to the first support and the second support with the plaster surface to be measured outside. Next, the first support and the second support were attached to the flexible members of the X-axis stage supporter and the Y-axis stage supporter as shown in FIGS. Then, the second support is moved at a constant speed by a Z-axis stage movable device (stepping motor), pressed against the first support at a constant condition, and after standing, it is separated at a constant retraction speed, and is generated in conjunction with it. The amount of bending of was measured. Converted from this measured amount, tackiness and peeling work of each sample were measured. The contact conditions were as follows.
<Contact conditions>
-Advance speed: 0.2 mm / s
・ Pressing distance: 0.684mm
・ Pressing load: 10gf
・ Pressing time: 5 seconds ・ Retraction speed: 0.02 to 8 mm / s (0.02, 0.04, 0.1, 0.2, 0.4, 1, 2, 8 mm / s) The average value of the data (tackiness, peeling work) performed at eight retraction speeds was used for evaluation.

<Test Example 2: Tackiness measurement test (plaster layer and skin stratum corneum)>
The tackiness and peeling work were measured in the same manner as in <Test Example 1> except that the hairless mouse-extracted skin was fixed to the first support so that the skin stratum corneum side was the outside.

<Test Example 3: Functionality test (between plaster layers)>
The plaster surfaces of the poultices (10 cm × 14 cm) of Example 1 and Comparative Examples 1 to 6 were bonded together and folded in half. Based on this, sensory evaluation was conducted on the ease of peeling when it was pulled apart. The test was conducted by 60 volunteers, ranked in order from the 1st to 7th in order from the one that can be easily removed, and evaluated by the average value. (Easy to peel 1 to hard to peel 7)

<Test Example 4: Sensory test (plaster layer and human skin)>
The cataplasm (10 cm × 14 cm) of Example 1 and Comparative Examples 1 to 6 was prepared, and the existing release film was peeled off and the same film (made of polypropylene) was used for the adhesion test in order to make the conditions uniform. And 20 volunteers tested in the following procedure, and sensory evaluation was carried out about the sticking property and handling property of a poultice.
[Test procedure]
1. The release film was peeled off, and first, a test patch was applied to the left shoulder.
2. After 10 seconds, it was peeled off the left shoulder, and this time it was affixed to the right shoulder.
[Evaluation criteria]
A: Most preferable sticking property (easy to handle, adheres to the skin and does not peel off)
○: Slightly preferred stickiness △: Slightly unsuitable stickiness ×: Most unsuitable stickiness (It is difficult to handle or does not stick well to the skin)

<Test Example 5: Ball tack method (adhesive strength test)>
A test piece was cut out from the central part of the cataplasm of Example 1 and Comparative Examples 1 to 6, and subjected to the adhesive strength test (ball tack test method) described in the pharmaceutical production guidelines (2001). Sticking the ball surface to the ball rolling device (tilt angle 30 degrees), leaving the plaster surface exposed 5 cm, covering the upper surface (running path) 10 cm and the lower 15 cm with the paper and fixing . The steel balls (balls) shown in Table 1 were rolled at an initial speed of 0 so that the length of the runway was constant at 10 cm, and the maximum ball number that stopped on the plaster surface was measured.

<Test Example 6: Probe tack method>
A test piece was cut out from the central part of the cataplasm of Example 1 and Comparative Examples 1 to 6, and subjected to the probe tack test method defined in ASTM D 2979 and tested. A 100 g load bakelite plate obtained by bonding a bakelite plate (1 cm ² ) to a 100 g weight was attached to a predetermined position in the apparatus. Next, after removing the peeling film of the test piece, it was fixed on the sample table with the plaster surface facing up, the sample plaster surface and the 100 g load bakelite plate surface were brought into close contact, and then peeled vertically. The resistance (g / cm ² ) when peeling from the sample plaster surface was measured.

<Test Example 7: Tackiness measurement test (plaster layers)>
Measurement was performed in the same manner as in Test Example 1 except that the contact conditions were as follows.
<Contact conditions>
-Advance speed: 0.2 mm / s
・ Pressing distance: 0.793mm
・ Pressing time: 5 seconds ・ Retraction speed: 0.5 to 10.0 mm / s (0.5, 0.8, 1.0, 1.6, 2.0, 3.0, 4.0, 5. 11 points of 0, 6.0, 8.0, 10.0 mm / s)
The tackiness was measured three times at each reverse speed, and the ranking of the examples and comparative examples at each reverse speed was determined from the average value. Next, an average of ranks was obtained at 11 points of each example and comparative example with a reverse speed of 0.5 to 10.0 mm / s, and the average rank was evaluated.

<Test Example 8: Tackiness measurement test (plaster layer and skin stratum corneum)>
Measurement was performed in the same manner as in Test Example 2 except that the contact conditions were as follows.
<Contact conditions>
-Advance speed: 0.2 mm / s
・ Pressing distance: 0.793mm
・ Pressing time: 5 seconds ・ Retraction speed: 0.5 to 8.0 mm / s (0.5, 0.8, 1.0, 1.6, 2.0, 3.0, 4.0, 5. (10 points of 0, 6.0, 8.0 mm / s)
The tackiness was measured three times at each reverse speed, and the ranking of the examples and comparative examples at each reverse speed was determined from the average value. Next, the average of rank was calculated | required in 10 points | pieces of retraction speed 0.5-8.0 mm / s of each Example and a comparative example, and it evaluated by this average rank.

<Evaluation>
The results of Test Example 1 are shown in FIG. 10, FIG. 11 and Table 2, the results of Test Example 2 are shown in FIG. 13, FIG. 14 and Table 3, the results of Test Examples 3 to 6 are shown in Table 4, and the results of Test Examples 7 and 8. Is shown in Table 5.

  In Test Example 5 and Test Example 6, which are conventional test methods, tackiness that is substantially the same numerical value and difficult to evaluate is evaluated by using the tackiness measurement method and measurement apparatus of the present invention. I was able to.

  FIG. 12 shows the relationship between the tackiness at the retraction speed of 0.04 mm / s in Test Example 1 and the average rank in Test Example 3. From FIG. 12, it was confirmed that the correlation between the tackiness obtained by the tackiness measuring method and the measuring apparatus of the present invention and the sensory test was also obtained. In addition, the evaluation ranking of tackiness (average value of data performed at eight retracting speeds) and peeling work (average value of data performed at eight retracting speeds) in Test Example 1, and the sensory test of Test Example 3 The evaluation order was also consistent, and it was confirmed that the average value of each sample was correlated with the sensory test. Further, from Table 3, it was found that tackiness and peeling work showed the same tendency and could be evaluated in a test using animal skin.

  FIG. 15 shows the relationship between the ease of peeling between the pastes in the tackiness (Test Example 1) and the sticking to the skin (Test Example 2). The easier to peel off the plaster is more convenient for handling, and the more difficult to peel from the skin is more convenient for use, so the direction of the upper right arrow in the figure is the ideal poultice. From FIG. 15, Example 1 was a cataplasm satisfying both conditions.

  FIG. 16 shows the relationship between ease of peeling of the plaster bodies in peel work (Test Example 1) and sticking to the skin (Test Example 2). Similar to tackiness, Example 1 was a cataplasm satisfying both conditions.

  Further, from the results of FIGS. 15 and 16 and Test Example 4, Example 1 in the upper right in the figure is evaluated as ◎ in Test Example 4, and Comparative Examples 2 and 4 in the lower left in the figure are evaluated as ×. Met. Therefore, it was confirmed that a correlation between the tackiness measuring method and the evaluation method using the measuring device of the present invention and the sensory test was obtained.

As is clear from Tables 2 and 3 and FIGS.
a) When the plaster layers of the cataplasm are stuck together and peeled off, the tackiness is 4 gf or less.
b) When the plaster layer of the cataplasm and the skin sample (stratum corneum) are bonded and peeled off, the tackiness is 5 gf or more.
According to the cataplasm of the present invention that satisfies the above two conditions at the same time, the palatability of the preparation is good, such as good adhesiveness to the skin, and the paste surfaces do not stick together and return. It has been confirmed that it is a good and ideal skin patch.

  In addition, FIG. 17 shows the relationship between the tackiness of each example and the order of ease of peeling between the pastes of the comparative examples (Test Example 7) and the order of sticking to the skin (Test Example 8). The direction of the upper right arrow in the figure is an ideal poultice, but as in FIG. 15 where the measurement results are expressed numerically, even if expressed in order, Example 1 is easy to peel off the paste, and is applied to the skin. It was a cataplasm with good handleability that satisfies both conditions.

It is a front view showing the whole tackiness measuring device of the present invention. It is an enlarged plan view of the support body contact part in FIG. It is an enlarged view of the support body contact part in FIG. It is an expansion perspective view of the support body contact part in FIG. It is explanatory drawing which shows the movement state of the support body contact part at the time of a test. It is a Wheatstone bridge circuit diagram of the 2 active gauge method for detecting the amount of strain from a strain gauge. It is a Wheatstone bridge circuit diagram of the 4 active gauge method for detecting the amount of strain from the strain gauge. It is an enlarged side view of the support body contact part in FIG. It is a figure which shows the change of the load at the time of a measurement. It is a figure which shows the relationship between the reverse | retreat speed | velocity | rate and tackiness in poultices. It is a figure which shows the relationship between the reverse | retreat speed | velocity | rate between peeling agents and peeling work. It is a figure which shows the relationship between tackiness and sensory evaluation. It is a figure which shows the relationship between the reverse | retreat speed | velocity | rate and tackiness in a poultice and hairless mouse skin. It is a figure which shows the relationship between the reverse | retreat speed | velocity | rate and peeling work in a poultice and hairless mouse skin. It is a figure which shows the relationship between the sticking to the skin in tackiness, and the ease of peeling of plaster. It is a figure which shows the relationship between the sticking to the skin in peeling work, and the ease of peeling of plaster. It is a figure which shows the relationship between the sticking to the skin in tackiness, and the ease of peeling of plaster.

Explanation of symbols

10 X-axis stage support device 20 Y-axis stage support device 30 Z-axis stage movable device (stepping motor)
40 member 50 strain gauge 60 first support 61 second support 70 patch 71 tack target 100 tackiness measuring device

Claims (13)

A tackiness measuring method for measuring the tackiness of a patch,
A first support that is disposed in one XY plane and supports the cylindrical surface or the elliptical column portion with the tack surface of the patch facing outside;
A second support that is disposed in the other XY plane and supports the tack target surface to be tacked outside in a cylindrical portion or an elliptical column portion ;
The first support and the second support are movable along respective axial directions,
The first support and the second support are point-contacted from the state separated from each other in the Z direction , and then retracted and separated,
The load change applied to the contact point of the first support and the second support from the start of the retraction to the complete separation is measured, and the tackiness of the patch is evaluated by the load change pattern. To measure tackiness. The tackiness measuring method according to claim 1, wherein the first support and the second support are orthogonally crossed to make the point contact .   A flexible member is connected to the first support body or the second support body, and the member bends by the point contact and the subsequent retreat, and the load change is measured by the amount of the bend. The tackiness measuring method according to claim 1 or 2.   The tackiness measuring method according to any one of claims 1 to 3, wherein a maximum load value from the reverse start to the separation is obtained, and the tackiness is determined based on the maximum load value.   The tackiness measuring method according to any one of claims 1 to 3, wherein the tackiness is determined by an area surrounded by a load curve from the start of retreating to the separation and a base line after the separation. The patch is a cataplasm, plaster, tape, bandage, sheet, wound dressing,
The tackiness measuring method according to any one of claims 1 to 5, which is one or more selected from cosmetic pack agents.   The tackiness measuring method according to any one of claims 1 to 6, wherein the patch is a poultice having a hydrous plaster layer. A tackiness measuring device for measuring the tackiness of a patch,
A first support that is arranged in one XY plane and supports the patch with a cylindrical part or an elliptical column part ;
A second support that is disposed in another XY plane and supports a tack target to be tacked by a cylindrical portion or an elliptical column portion ;
Means for moving the first support and the second support along respective axial directions;
The first support or the second support is reciprocated in the Z direction, and the first support and the second support are moved back from each other and then moved backward to separate them. Control means;
A tackiness measuring device comprising: a load measuring unit that measures a load change applied to a contact point between the first support and the second support. The tackiness measuring apparatus according to claim 8, wherein the first support and the second support are orthogonally crossed to make the point contact .   One of the first support or the second support is connected to one end of a flexible member, the other end of the member is fixed, and the member is provided with a strain gauge. Item 10. The tackiness measuring device according to Item 8 or 9.   The tackiness measuring apparatus according to claim 10, wherein the flexible member is formed of a phosphor bronze plate.   The tackiness measuring apparatus according to claim 10 or 11, wherein a pair of the strain gauges are provided on at least a front side and a back side of the member.   The tackiness measuring apparatus according to any one of claims 10 to 12, wherein the strain gauge is connected to a Wheatstone bridge circuit and measured by a 2 or 4 active gauge method.

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