Rapid determination method for residual amount of paraffin on inner and outer surfaces of soft capsule

Abstract

The invention belongs to the technical field of pharmaceutical manufacturing quality control, and discloses a rapid determination method of residual paraffin on the inner and outer surfaces of a soft capsule, which comprises quantitative detection on the inner and outer surfaces of a capsule, and adopts the core scheme that filter paper is respectively adopted to adsorb residual paraffin on the inner and outer surfaces of a sample; and calculating according to a weight difference value before and after the adsorption of the filter paper. The rapid determination method is simple and rapid to operate, the detection result is rapidly obtained, the use condition and the residual quantity of the light liquid paraffin are conveniently and regularly monitored in the pelleting production process, and the drug production quality is guaranteed.

Description

Technical Field

[0001] The invention relates to the technical field of pharmaceutical manufacturing quality control, in particular to a method for quickly determining the amount of paraffin residue on the inner and outer surfaces of a soft capsule. Background Art

[0002] During the soft capsule production process, light liquid paraffin is typically used for lubrication and mold release during the transfer of the rubber sheet to the mold for compression molding. After compression molding, some paraffin residue may remain on both the inner and outer surfaces of the soft capsule. Currently, the soft capsule manufacturing industry lacks standardized operating procedures for detecting paraffin residues, nor are there limits for residual paraffin oil. However, as an additive to drug formulations, controlling residual levels is beneficial to drug quality and human health. Therefore, to better control the quality of soft capsule production, it is necessary to develop a method for rapidly detecting paraffin residues during production. Summary of the Invention

[0003] In order to solve the above problems in the prior art, the present invention provides a method for quickly determining the amount of paraffin residue on the inner and outer surfaces of soft capsules, so as to better control the production quality of soft capsules.

[0004] To achieve the above object, the present invention adopts the following technical solutions:

[0005] The invention provides a method for quickly determining the amount of paraffin residue on the inner and outer surfaces of a soft capsule. Filter paper is used to adsorb the paraffin residue on the inner and outer surfaces of a sample, and the amount is calculated based on the weight difference before and after the adsorption.

[0006] Preferably, the sample for detecting the amount of paraffin residue on the outer surface of the soft capsule is a finished soft capsule that has not been dried after pelleting.

[0007] Preferably, the sample for detecting the amount of paraffin residue on the inner surface of the soft capsule is a double-layer rubber sheet that has been screen-printed but not cut into pellets by a pill press.

[0008] Preferably, the method for detecting the amount of paraffin residue on the outer surface of the soft capsule comprises the following steps:

[0009] S11 filter paper weighing: accurately weigh the total weight W1 of several round filter papers;

[0010] S12 Sampling: Use a clean and dry sampler to take N pellets and place them in a clean and dry beaker;

[0011] S13 Paraffin transfer: Use clean and dry tweezers to pick up filter papers one by one and stir them in the pellet 10 times until all the round filter papers are used up;

[0012] S14 weighing calculation: Accurately weigh the total weight W2 of all filter papers and calculate the residual paraffin:

[0013] The amount of paraffin residue on the outer surface of each capsule (mg) = (W2-W1) / N.

[0014] More preferably, in step S11, the number of the circular filter papers is 3-6 pieces, and the circular filter papers can be placed in the beaker. Preferably, the area of ​​the circular filter papers is smaller than the area of ​​the cup mouth of the beaker.

[0015] More preferably, in step S12, the number N of the capsule sample is 30-50 capsules, and the sampler is used for one-time sampling.

[0016] Preferably, the method for detecting the amount of paraffin residue on the inner surface of the soft capsule comprises the following steps:

[0017] S21 sampling: At the pill pressing operation site, adjust the distance between the two rollers of the pill pressing machine until the two rubber sheets are pressed together and only screen prints are produced without being cut into pills. Cut a piece of double-layer rubber sheet, about the size of an A4 paper.

[0018] S22 Filter paper weighing: Accurately weigh the net weight W1 of at least one round filter paper;

[0019] S23 Paraffin transfer: Open the removed double-layer rubber sheet, place the weighed round filter paper in the middle, close the rubber sheet and press gently to allow the filter paper to fully absorb the paraffin liquid;

[0020] S24 weighing calculation: Peel off the filter paper and take it out, and accurately weigh its total weight W2 to calculate the residual paraffin:

[0021] The paraffin content on the inner surface of each capsule (mg) = (W2-W1) / filter paper contact area × the inner surface area of ​​each capsule.

[0022] Preferably, in step S21, before using the filter paper to adsorb the sample for paraffin residue detection on the inner surface of the soft capsule, the light liquid paraffin on the outer surface of the double-layer rubber is wiped off with oil-absorbing cotton cloth in advance.

[0023] More preferably, in step S22, two circular filter papers are used and placed overlappingly; and the area of ​​the circular filter papers is smaller than the area of ​​the double-layer rubber.

[0024] Preferably, in step S24, the contact area of ​​the filter paper is the area of ​​a single circular piece of filter paper, and the inner surface area of ​​each capsule is calculated based on the geometric shape and size of each capsule in the mesh on the rubber.

[0025] Preferably, in step S24, for irregular-shaped soft capsule products, the surface area of ​​a single capsule can also be calculated by the average capsule weight ÷ total sampled capsule weight × sampled capsule area.

[0026] The present invention adopts the above technical solution, which has the following technical effects compared with the prior art:

[0027] The invention relates to a rapid method for determining the residual amount of paraffin wax in soft capsules, comprising quantitative detection of the inner and outer surfaces of the capsules, wherein the result is mainly obtained by calculating the weight difference after the sample is adsorbed on filter paper. The method is simple and quick to operate, and the detection result is obtained quickly, which facilitates regular monitoring of the use and residual amount of light liquid paraffin wax during the pill pressing production process, thereby facilitating quality assurance of pharmaceutical production. By respectively determining the residual amount on the inner and outer surfaces of the soft capsules, the lubrication oil output of the rubber conveying rollers on the inner and outer surfaces can be adjusted according to the residual result and the actual lubrication effect. The method is particularly suitable for online quality monitoring of soft capsule (such as pharmaceutical and health product) production lines. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 Schematic diagram of the structure of the double-layer rubber sample in the method for detecting the amount of paraffin residue on the outer surface of the soft capsule of the present invention;

[0029] Figure 2 This is a schematic diagram of a cutout of a double-layer rubber sample used in the method for detecting the amount of paraffin residue on the inner surface of a soft capsule according to the present invention. DETAILED DESCRIPTION

[0030] To better control the production quality of soft capsules (such as medicines and health products), the present invention provides a method for rapidly determining the amount of paraffin residue on the inner and outer surfaces of soft capsules. The method comprises two parts: quantitative detection of the inner surface of the capsule and quantitative detection of the outer surface of the capsule. The core solution is to calculate the result by the weight difference after the sample is adsorbed on filter paper.

[0031] The present invention will be described in detail and specifically below through specific examples to provide a better understanding of the present invention, but the following examples do not limit the scope of the present invention.

[0032] Example 1

[0033] A method for detecting the amount of paraffin residue on the outer surface of a soft capsule comprises the following steps:

[0034] S11 Filter paper weighing: Use an electronic balance to accurately weigh the total weight W1 of 4 round filter papers;

[0035] S12 Sampling: Use a clean and dry sampler to take 40 capsules and place them in a 250ml clean and dry beaker;

[0036] S13 Paraffin transfer: Use clean, dry tweezers to pick up a piece of filter paper and stir it in the pellet 10 times, using one piece of filter paper each time, until all four round filter papers are used up;

[0037] S14 Weighing calculation: Then use an electronic balance to accurately weigh the total weight W2 of the four filter papers, and calculate the paraffin residue based on this: the paraffin residue on the outer surface of each capsule (mg) = (W2-W1) / 40.

[0038] Example 2

[0039] A method for detecting the amount of paraffin residue on the inner surface of a soft capsule comprises the following steps:

[0040] S21 sampling: At the pill pressing operation site, adjust the distance between the two rollers of the pill pressing machine until the two rubber sheets are pressed together and only screen prints are produced without being cut into pills. Cut off a piece of rubber sheet. Figure 1 and Figure 2 As shown, it is about the size of A4 paper. Use oil-absorbing cotton cloth to wipe off the light liquid paraffin on the outer surface;

[0041] S22 Filter paper weighing: Accurately weigh the net weight W1 of two overlapping circular filter papers;

[0042] S23 Paraffin transfer: Remove the double-layer rubber and open it, place the weighed round filter paper in the middle, close the rubber and press gently to allow the filter paper to fully absorb the paraffin liquid:;

[0043] S24 Filter paper weighing: Remove the filter paper and immediately weigh W2; paraffin content on the inner surface of each capsule (mg) = (W2 - W1) / filter paper contact area × inner surface area of ​​each capsule;

[0044] The contact area of ​​the filter paper is the area of ​​a single circular piece of filter paper, and the internal surface area of ​​each capsule needs to be calculated based on the geometric shape and size of each capsule in the reticular pattern on the rubber.

[0045] Application Examples

[0046] 1. Materials and Instruments

[0047] Filter paper: 10 cm diameter round filter paper (stored in a sealed bag and dry)

[0048] Electronic balance: Mettler ME203TE, precision 1mg, calibration validity period within the validity period, weight calibration completed on the same day

[0049] Sampler: Clean and dry stainless steel tweezers

[0050] Beaker: Clean and dry 250ml glass beaker with a mouth diameter of 8cm

[0051] Oil-absorbing cotton cloth: microfiber oil-absorbing cotton (lipophilic, chemical-free)

[0052] 2. Operation steps

[0053] 1. A method for detecting the amount of paraffin residue on the outer surface of a soft capsule, comprising the following steps:

[0054] S11 Filter paper weighing: Place 4 filter papers on the electronic balance pan and weigh a total of 3.025 g;

[0055] S12 Sampling: Use clean and dry stainless steel tweezers to randomly take out 40 freshly compressed alfacalcidol soft capsules (specification 0.25 μg) and place them in a clean and dry beaker;

[0056] S13 Paraffin transfer: Use tweezers to pick up the first piece of filter paper and slowly rotate it clockwise along the inner wall of the beaker to stir the capsule 10 times to ensure that the filter paper fully contacts the capsule surface. Remove the filter paper and place it on the electronic balance pan. Repeat the above steps until all four filter papers have been used up.

[0057] S14 weighing calculation: reweigh the total weight of the filter paper 2.951g, each capsule paraffin residue (mg) = (3.025-2.951) ÷ 40 = 0.00185g = 1.85mg.

[0058] 2. A method for detecting the amount of paraffin residue on the inner surface of a soft capsule, comprising the following steps:

[0059] S21 sampling: Alfacalcidol soft capsules (specification 0.25 μg, mold width 25.0 cm) were prepared by adjusting the distance between the two rollers of the pill press until the two rubber sheets were pressed together and only screen-printed without being cut into pills. A 25.0 cm × 20.0 cm double-layer rubber sheet was cut with scissors and immediately wiped along the outer surface of the double-layer rubber sheet in one direction with an oil-absorbing cotton cloth to remove the light liquid paraffin.

[0060] S22 filter paper weighing: overlap two filter papers and place them on the electronic balance pan, weighing the total weight to 1.510 g;

[0061] S23 Paraffin transfer: Open the double-layer rubber sheet, place the double-layer filter paper in the middle layer of the rubber sheet, close the rubber sheet and press evenly with a plastic plate for 5 seconds to allow the filter paper to fully absorb the paraffin liquid;

[0062] S24 weighing calculation: Gently peel off the rubber, take out the filter paper and put it on the electronic balance pan. Weigh the total weight of the filter paper 1.542g. The surface area of ​​the double-layer filter paper = π × 52 × 2 = 50π;

[0063] Alfacalcidol soft capsules (specification 0.25 μg) are ellipsoidal in shape. When the capsule is cut in half, it is a uniform ellipse with a major axis length of 1.25 cm and a minor axis length of 0.75 cm.

[0064] Internal surface area of ​​each capsule = π × 1.25 × 0.75 × 2 = 1.875π;

[0065] The paraffin content on the inner surface of each capsule = (1.542-1.510)÷50π×1.875π=0.0012=1.20 mg.

[0066] While the specific embodiments of the present invention have been described in detail above, these are merely exemplary and the present invention is not limited thereto. For those skilled in the art, any equivalent modifications and substitutions to the present invention are also within the scope of the present invention. Therefore, any equivalent changes and modifications made without departing from the spirit and scope of the present invention are intended to be encompassed within the scope of the present invention.

Claims

1. A method for rapidly determining the amount of paraffin residue on the inner and outer surfaces of soft capsules, characterized in that: Filter paper is used to adsorb the paraffin remaining on the inner and outer surfaces of the sample, and then the weight difference before and after adsorption by the filter paper is calculated.

2. The rapid determination method according to claim 1, characterized in that The sample for detecting the amount of paraffin residue on the outer surface of the soft capsule is a finished soft capsule that has not been dried after pelleting.

3. The rapid determination method according to claim 1, characterized in that The sample for detecting the amount of paraffin residue on the inner surface of the soft capsule is a double-layer rubber sheet that has been screen-printed but not cut into pellets by a pill press.

4. The rapid determination method according to claim 1, characterized in that The method for detecting the amount of paraffin residue on the outer surface of the soft capsule comprises the following steps: S11 filter paper weighing: accurately weigh the total weight W1 of several round filter papers; S12 Sampling: Use a clean and dry sampler to take N pellets and place them in a clean and dry beaker; S13 Paraffin transfer: Use clean and dry tweezers to pick up filter papers one by one and stir them in the pellet 10 times until all the round filter papers are used up; S14 weighing calculation: Accurately weigh the total weight W2 of all filter papers and calculate the residual paraffin: The amount of paraffin residue on the outer surface of each capsule (mg) = (W2-W1) / N.

5. The rapid determination method according to claim 4, characterized in that In step S11, the number of the circular filter papers is 3-6 pieces, and the circular filter papers can be placed in the beaker.

6. The rapid determination method according to claim 4, characterized in that In step S12, the number N of the capsule sample is 30-50 capsules, and the sampler is used for one-time sampling.

7. The rapid determination method according to claim 1, characterized in that The method for detecting the amount of paraffin residue on the inner surface of the soft capsule comprises the following steps: S21 sampling: At the pill pressing operation site, adjust the distance between the two rollers of the pill pressing machine until the two rubber sheets are pressed together and only screen prints are produced without being cut into pills. Cut a piece of double-layer rubber sheet, about the size of an A4 paper. S22 Filter paper weighing: Accurately weigh the net weight W1 of at least one round filter paper; S23 Paraffin transfer: Open the removed double-layer rubber sheet, place the weighed round filter paper in the middle, close the rubber sheet and press gently to allow the filter paper to fully absorb the paraffin liquid; S24 weighing calculation: Peel off the filter paper and take it out, and accurately weigh its total weight W2 to calculate the residual paraffin: The paraffin content on the inner surface of each capsule (mg) = (W2-W1) / filter paper contact area × the inner surface area of ​​each capsule.

8. The rapid determination method according to claim 7, characterized in that In step S21, before using the filter paper to adsorb the sample for paraffin residue detection on the inner surface of the soft capsule, the light liquid paraffin on the outer surface of the double-layer rubber is wiped off with oil-absorbing cotton cloth in advance.

9. The rapid determination method according to claim 7, characterized in that In step S22, two circular filter papers are used and placed overlappingly; and the area of ​​the circular filter papers is smaller than the area of ​​the double-layer rubber.

10. The rapid determination method according to claim 7, characterized in that In step S24 , the contact area of ​​the filter paper is the area of ​​a single circular piece of filter paper, and the inner surface area of ​​each capsule needs to be calculated based on the geometric shape and size of each capsule in the mesh on the rubber.

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