CN109521130B - Method for detecting antioxidant in elastomer sealing element for medicine packaging - Google Patents
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Abstract
The invention belongs to the technical field of analytical chemistry, and discloses a method for detecting antioxidants in elastomer sealing elements for medicine packaging, which comprises the steps of detecting prepared test solution by using a liquid chromatograph, and recording a chromatogram; and calculating the contents of the antioxidant and the degradation product in the elastomer sealing element and the liquid medicine by peak area according to a standard curve method. The invention establishes a method for screening and analyzing antioxidants in elastomer sealing parts for medicine packaging, and adopts high performance liquid chromatography to separate the 12 antioxidants and degradation products at one time, and the retention time is taken as a qualitative basis. Dissolving various antioxidants and degradation products in dichloromethane solution, mechanically crushing a sealing element, swelling with dichloromethane overnight, performing microwave heating extraction, filtering, and detecting by using high performance liquid chromatography. The method has the advantages of simple and efficient extraction operation, low requirement on equipment by adopting liquid chromatography analysis and detection, high detection speed by one needle for screening and analyzing 12 substances and comprehensive coverage of the antioxidant.
Description
Technical Field
The invention belongs to the technical field of analytical chemistry, and particularly relates to a method for detecting an antioxidant in an elastomer sealing element for medicine packaging.
Background
The pharmaceutical packaging material is used for manufacturing packaging containers, packaging decoration, packaging printing, packaging transportation and the like, and is used for meeting the requirements of product packaging. Elastomer seal: the elastic body is an object which has the strain and stress of each point in the elastic body which are in one-to-one correspondence under the action of external force and can be recovered to the original state after the external force is removed. Elastomer seals are here primarily referred to as rubber-like seals and thermoplastic elastomer seals in pharmaceutical packaging materials. The rubber materials commonly used for medicine packaging can be divided into the following types according to the difference of monomers used in polymerization reaction: polyisoprene rubber, butyl rubber, halogenated butyl rubber, silicone rubber, ethylene propylene rubber; according to the structure and the processing technology of the rubber component, the rubber component can be divided into the following steps: coated seals, non-coated seals; the coating sealing member includes a coating film, a plating film, and the like. Thermoplastic elastomers are classified into copolymerization type (chemical synthesis type) thermoplastic elastomers and blend type (rubber blend type) thermoplastic elastomers according to the preparation method. They can be classified into Styrenic Block Copolymers (SBCs), polyurethanes (TPU), polyesters (TPEE), polyamides (TPEE), polyolefins (TPO), etc. according to their chemical structures. Antioxidant: antioxidants are a class of chemicals which, when present in only small amounts in polymer systems, retard or inhibit the progress of the polymer oxidation process, thereby preventing the aging of the polymer and extending its useful life, also known as "age resistors". As a packaging component, on one hand, the sealing member should meet the requirement of the packaging system on sealing performance, provide protection for medicines and meet the expected use function of the packaging; on the other hand, the extract has good compatibility with the medicine, namely, extracts with safety risks cannot be introduced, or the extract level meets the safety requirement; and the quality, the curative effect and the safety of the medicine cannot be influenced by adsorbing the active ingredients or the functional auxiliary materials in the medicine. Antioxidants, which are conventionally added additives to elastomers, run the risk of migrating into pharmaceutical products during packaging, storage and transportation of the products, so that care needs to be taken regarding the migratable amount of antioxidants in elastomers and the actual migration amount of antioxidants in pharmaceutical products during the quality control of pharmaceutical products, particularly during the study of compatibility of pharmaceutical products with packaging materials. The production and processing flow of the elastomer is long, and a plurality of links from raw materials of the elastomer to storage and transportation to final product molding all involve the addition of the antioxidant, so that the types of target antioxidants in actual detection are various, and the concentration difference of different antioxidants is large. In addition, antioxidants are degraded by themselves, and their degradation products risk to migrate into the drug product and affect the efficacy of the drug, even producing toxicity. Therefore, it is difficult and necessary to analyze and detect the degradation products of the antioxidant together with the antioxidant itself in the process of analyzing and detecting the antioxidant. In the background of the prior art, there is no method to extract and detect various antioxidants and their degradation products commonly found in elastomers. Common antioxidants in elastomeric seals for pharmaceutical packaging include BHT, 3114, 1010, 1330, 1076, 168, and their series antioxidant degradation products BHT-OH, BHT-COOH, BHT-CHO, BHT-Q (degradation products of BHT, 1330, 1076, etc.), 2, 4-di-tert-butylphenol (degradation product of 168), degradation product 1310 (degradation product of 1010, 1076).
In summary, the prior art has the problems that1. In the sample preparation process, technical means such as toluene reflux and the like which are relatively time-consuming, waste in materials and relatively large in environmental pollution are generally adopted. 2. The detection target species are limited to one to two specific antioxidant targets, the species and the number of the antioxidants actually added in the elastomer are many, if the traditional method is adopted, the multiple targets need to be injected respectively, and multiple tests are needed to complete qualitative screening and quantitative analysis of potential extractables, so that the system is lacked, and the screening efficiency is low. 3. The detection target for antioxidants is focused on the antioxidant itself, neglectingVarious products resulting from the degradation of the antioxidant during processing and elastomer life are described. 4. The screening of a small part of antioxidants by expensive instruments such as liquid chromatography-mass spectrometry has no efficiency, and also puts high requirements on instruments and equipment.
The difficulty and significance for solving the technical problems are as follows:1, a rapid, simple and environment-friendly extraction method is provided for screening the antioxidant in the elastomer; 2, provides a systematic screening antioxidant and degradation product detection means; 3, the screening efficiency is greatly improved, and only 55 minutes are needed for detecting 12 antioxidants; 4, the liquid chromatography is adopted, the requirement on the instrument is low, and each detection mechanism can meet the detection condition.
Disclosure of Invention
In view of the problems of the prior art, the present invention provides a method for detecting antioxidants in elastomeric seals for pharmaceutical packaging.
The method for detecting the antioxidant in the elastomer sealing element for the medicine packaging is realized by detecting the prepared test solution by using a liquid chromatograph and recording a chromatogram; and calculating the contents of the antioxidant and the degradation product in the elastomer sealing element and the liquid medicine by peak area according to a standard curve method.
Further, the high performance liquid chromatography conditions of the method for detecting antioxidants in elastomeric seals for pharmaceutical packaging are: c18 forward chromatography column; the mobile phase A is acetonitrile obtained by chromatography, the mobile phase B is chromatographically pure methanol, and the mobile phase C is acetic acid aqueous solution with the concentration of 1%; column temperature: 35 ℃; detecting the wavelength of 277 nm; flow rate: 1.0 ml/min; sample introduction amount: 10 μ l.
Further, the detection of the prepared test solution by the liquid chromatograph requires:
step one, crushing an elastomer to be detected into small particles of about 5mm multiplied by 5mm, weighing 0.5g of a crushed rubber plug, putting the crushed rubber plug into a microwave digestion tube, adding 10ml of dichloromethane, swelling for 12 hours, performing microwave digestion at 40 ℃ for 45min, and cooling to room temperature;
filtering by using a glass funnel to remove small elastomer particles, vacuumizing and evaporating filtrate in a rotary manner to remove a dichloromethane solvent; dissolving the volatilized residue by 8ml of methanol through ultrasonic oscillation, transferring the dissolved solution to a 10ml volumetric flask, and fixing the volume of the methanol solution;
and step three, taking the solution with constant volume, filtering the solution by using a 0.45-micron nylon filter membrane, and detecting the filtrate by using a liquid chromatography.
Another object of the present invention is to provide a pharmaceutical packaging box to which the method for detecting antioxidants in elastomeric seals for pharmaceutical packaging is applied.
In summary, the advantages and positive effects of the invention are12 kinds of 12 kinds
Drawings
FIG. 1 is a flow chart of a method for detecting antioxidants in elastomeric seals for pharmaceutical packaging according to an embodiment of the present invention.
FIG. 2 is a liquid chromatogram of a mixed control provided by an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
As shown in fig. 1, the method for detecting antioxidants in elastomeric seals for pharmaceutical packaging according to embodiments of the present invention includes the following steps:
s101: crushing the elastomer to be detected into small particles of about 5mm multiplied by 5mm, weighing 0.5g of crushed rubber plugs, putting the crushed rubber plugs into a microwave digestion tube, adding 10ml of dichloromethane, swelling overnight (about 12 hours), performing microwave digestion at 40 ℃ for 45min, and cooling to room temperature;
s102: filtering with a glass funnel to remove small elastomer particles, vacuumizing and evaporating filtrate in a rotary manner, and removing a dichloromethane solvent; dissolving the residue after volatilizing with 8ml methanol (containing 0.1% dichloromethane) under ultrasonic oscillation, transferring the dissolved solution to a 10ml volumetric flask, and fixing the volume with methanol (0.1% dichloromethane) solution;
s103: filtering the solution with 0.45 μm nylon filter membrane, and detecting the filtrate with the above liquid chromatography;
s104: detecting the prepared test solution by using a liquid chromatograph, and recording a chromatogram; and calculating the contents of the antioxidant and the degradation product in the elastomer sealing element and the liquid medicine by peak area according to a standard curve method.
In a preferred embodiment of the invention: high performance liquid chromatography conditions: selecting conventional C18 forward chromatographic column (selecting Waters company Symmetry RP18 type chromatographic column length 250mm × diameter 4.6mm, filler particle size 5 um); the mobile phase A is acetonitrile obtained by chromatography, the mobile phase B is chromatographically pure methanol, and the mobile phase C is acetic acid aqueous solution with the concentration of 1%; column temperature: 35 ℃; detecting the wavelength of 277 nm; flow rate: 1.0 ml/min; sample introduction amount: 10 μ l. The number of theoretical plates is not less than 3000 calculated according to the main component peak. The detection limit of each target should be no more than 200 ug/L.
TABLE 1 mobile phase gradient elution conditions
| Time (min) | A (acetonitrile,%) | B (methanol,%) | C (1% acetic acid-water,%) |
| 0 | 10 | 50 | 40 |
| 3 | 10 | 50 | 40 |
| 6 | 20 | 50 | 30 |
| 9 | 25 | 50 | 25 |
| 12 | 25 | 50 | 25 |
| 15 | 30 | 50 | 20 |
| 21 | 90 | 5 | 5 |
| 24 | 90 | 5 | 5 |
| 30 | 80 | 20 | 0 |
| 33 | 60 | 40 | 0 |
| 36 | 0 | 100 | 0 |
| 42 | 0 | 100 | 0 |
| 45 | 10 | 50 | 40 |
| 55 | 10 | 50 | 40 |
The determination method comprises the following steps: detecting the prepared test solution by using a liquid chromatograph, and recording a chromatogram. As shown in FIG. 2; and calculating the contents of the antioxidant and the degradation product in the elastomer sealing element and the liquid medicine by peak area according to a standard curve method.
Proof part (concrete examples/experiment/simulation /)
1. Methodology validation section:
the method is proved to be true and reliable through a verification process of a common analysis and detection methodology:
1.1. detection limit:
1.2 Analytical Evaluation Threshold (AET)
The results show that the detection limit of the method is obviously lower than the requirement of an analysis and evaluation threshold value, and the method can be completely used for analyzing the contents of the antioxidant and the degradation products thereof in the rubber plug.
1.3 linearity and range:
the twelve antioxidants and the degradation products thereof have good linear relationship between peak area and concentration within the concentration range of 0.2-20 ppm
1.4 precision
| 1 | 2 | 3 | 4 | 5 | 6 | RSD | |
| BHT-OH | 24824 | 24814 | 24902 | 24752 | 24797 | 24886 | 0.23％ |
| BHT-COOH | 113948 | 113801 | 113869 | 113918 | 112970 | 113967 | 0.34％ |
| BHT-CHO | 178444 | 178386 | 178231 | 178443 | 179657 | 173901 | 1.12％ |
| BHT-Q | 28810 | 28818 | 28705 | 28792 | 28950 | 28787 | 0.28％ |
| BHT | 29731 | 29605 | 29815 | 29819 | 30007 | 29812 | 0.44％ |
| 2, 4-di-tert-butylphenol | 31443 | 31598 | 31405 | 31440 | 31793 | 31444 | 0.47％ |
| 1310 | 14920 | 15897 | 16124 | 16156 | 15902 | 16285 | 3.11％ |
| 3114 | 16179 | 16104 | 16160 | 16203 | 16158 | 16217 | 0.25％ |
| 1010 | 20422 | 20506 | 20394 | 20521 | 20535 | 20577 | 0.34％ |
| 1330 | 25418 | 25279 | 25438 | 25967 | 26026 | 25920 | 1.29％ |
| 1076 | 10023 | 10298 | 10050 | 10252 | 10225 | 10174 | 1.10％ |
| 168 | 13126 | 13242 | 13367 | 13426 | 13309 | 13466 | 0.94％ |
And taking a reference substance solution with the concentration of about 5ppm, continuously injecting a sample for 6 needles, recording a chromatogram, and calculating the RSD of the antioxidant peak area, wherein the RSD is shown in the table, and the method has good precision.
1.5 stability
Sampling control solution of about 5ppm for 0, 9, 35, and 53 hr respectively, analyzing, calculating peak area RSD, and determining that twelve antioxidants, their degradation products, and control solution capable of extracting sulfur are stable within 53 hr
1.6 accuracy:
the accuracy of the method is confirmed by adding a standard substance to detect the recovery rate, the recovery rate is between 86.2% and 102.4% except 168%, and the recovery rate is good.
2. The detection technology is applied as follows:
the results of the tests performed on the collected plugs from 9 butyl plug manufacturers were as follows:
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 and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (2)
1. A method for detecting antioxidants and degradants in elastomer sealing elements for medicine packaging is characterized in that a prepared test solution is detected by a liquid chromatograph, and a chromatogram is recorded; calculating the content of antioxidants and degradants in the elastomer sealing element by peak area according to a standard curve method;
the high performance liquid chromatography conditions of the method for detecting antioxidants and degradants in the elastomer sealing part for the medicine packaging are as follows: c18 reverse phase chromatography column; the mobile phase A is chromatographic pure acetonitrile, the mobile phase B is chromatographic pure methanol, and the mobile phase C is 1% acetic acid aqueous solution; column temperature: 35 ℃; detecting the wavelength of 277 nm; flow rate: 1.0 ml/min; sample introduction amount: 10 mu l of the mixture;
gradient elution conditions of the mobile phase
The antioxidant is as follows: BHT, 3114, 1010, 1330, 1076, and 168; the degradation products of the antioxidant are as follows: BHT-OH, BHT-COOH, 1310, BHT-CHO, BHT-Q and 2, 4-di-tert-butylphenol;
the detection of the prepared test solution by the liquid chromatograph requires:
firstly, crushing an elastomer sealing element to be detected into small particles of about 5mm multiplied by 5mm, weighing 0.5g of the elastomer sealing element, putting the elastomer sealing element into a microwave digestion tube, adding 10ml of dichloromethane, swelling for 12 hours, carrying out microwave digestion at 40 ℃ for 45min, and cooling to room temperature;
filtering by using a glass funnel, removing small particles of the elastomer sealing element, vacuumizing and evaporating filtrate in a rotary manner, and removing a dichloromethane solvent; dissolving the volatilized residue by 8ml of methanol through ultrasonic oscillation, transferring the dissolved solution to a 10ml volumetric flask, and fixing the volume of the methanol solution;
and step three, taking the solution with constant volume, filtering the solution by using a 0.45-micron nylon filter membrane, and detecting the filtrate by using a liquid chromatography.
2. Use of the method of claim 1 for detecting antioxidants and degradants in elastomeric seals for pharmaceutical packaging.
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