CN114441691B - Method for detecting plastic additive in ophthalmic preparation container - Google Patents
Method for detecting plastic additive in ophthalmic preparation container Download PDFInfo
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- CN114441691B CN114441691B CN202210377266.2A CN202210377266A CN114441691B CN 114441691 B CN114441691 B CN 114441691B CN 202210377266 A CN202210377266 A CN 202210377266A CN 114441691 B CN114441691 B CN 114441691B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/047—Standards external
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The application provides a method for detecting a plastic additive in an ophthalmic preparation container. According to the detection method, the extraction sample or the migration sample of the ophthalmic preparation container is treated by the extraction solvent, then high performance liquid chromatography is adopted for analysis, and the liquid chromatography condition is optimized, so that the solvent effect is overcome, the separation degree of a target peak is improved, the detection method can be used for detecting and safely evaluating the contents of the plastic additives 08 and 15 in the ophthalmic preparation container, the technical problems of poor accuracy and low sensitivity of the existing detection method are solved, and the high requirement on quality control of the plastic additives in the medicinal packaging material can be met.
Description
Technical Field
The application belongs to the technical field of package material compatibility analysis, and particularly relates to a detection method of a plastic additive in an ophthalmic preparation container.
Background
3- (1, 1-Dimethylethyl) - β - [3- (1, 1-Dimethylethyl) -4-hydroxyphenyl ] -4-hydroxy- β -methylbenzoic acid 1, 2-ethylene ester (plastics additive 08) and 1, 1' -dioctadecyl disulfide (plastics additive 15) are common hazardous materials in pharmaceutical packaging. The european pharmacopoeia indicates that the content of polyethylene-containing materials (including plastic additives 08 and 15) for injection and ophthalmic preparation containers should not exceed 0.3%.
At present, liquid phase UV method or thin layer chromatography is mostly adopted for detecting the plastic additives 08 and 15, but the accuracy of the methods is poor. Meanwhile, the plastic additives 08 and 15 are mutation-causing impurities in the medicine, and the quality control requirement is higher, and the limit evaluation method for the plastic additives in the container is not enough to support the use safety specification of the medicine. Therefore, there is an urgent need to improve the accuracy and detection limit of the method for detecting plastic additives in pharmaceutical preparation containers and to improve the quality safety of the pharmaceutical products.
Disclosure of Invention
In view of this, the application provides a method for detecting a plastic additive in an ophthalmic preparation container, which solves the problem that the existing methods for detecting plastic additives 08 and 15 in a medicinal packaging material have poor performance such as accuracy and detection limit, and can accurately evaluate the content of the plastic additive in the ophthalmic preparation container.
The specific technical scheme of the application is as follows:
the application provides a method for detecting a plastic additive in an ophthalmic preparation container, which comprises the following steps:
boiling the ophthalmic preparation container in a first organic solvent, refluxing, adding a second organic solution, filtering, and diluting with a mixed solvent of the first organic solvent and the second organic solvent to obtain an extracted sample;
placing the ophthalmic preparation container under a preset condition for a certain time, and taking out the content to obtain a migration sample;
collecting the extract or migration sample of the ophthalmic preparation container, evaporating to dryness in water bath, dissolving the residue with extraction solvent, diluting, and analyzing by high performance liquid chromatography, wherein the content of plastic additive 08 is analyzed by mobile phase acetonitrile-water or methanol-water, and the content of plastic additive 15 is analyzed by mobile phase n-hexane or cyclohexane.
Preferably, the liquid chromatography conditions of the plastic additive 08 are: the chromatographic column adopts a C18 chromatographic column, and the volume ratio of mobile phases is acetonitrile: water = (70-80): (20-30), detection wavelength is 260-280 nm.
Preferably, the liquid chromatography conditions of the plastic additive 15 are: the chromatographic column adopts a silicon dioxide chromatographic column, the detector adopts a CAD detector, and the temperature of the CAD atomizer is 60-80 ℃.
Preferably, the high performance liquid chromatography conditions are: the column temperature is 20-30 ℃, the flow rate is 0.5-2 ml/min, and the sample injection volume is 1-5 mul.
Preferably, the extraction reagent is selected from one or more of n-hexane, cyclohexane, tetrahydrofuran and acetonitrile.
Preferably, the extraction reagent of the plastic additive 15 is cyclohexane, the extraction reagent of the plastic additive 08 is tetrahydrofuran and acetonitrile, and the volume ratio is (1-2): 1.
preferably, the first organic solution is toluene and the second organic solution is methanol.
Preferably, the volume ratio of the first organic solvent to the second organic solvent is 1: (1-2), wherein the volume ratio of the first organic solvent to the second organic solvent in the mixed solvent is 1: (1-2).
Preferably, the ophthalmic formulation comprises sodium hyaluronate eye drops and the container comprises a pharmaceutical vial of low density polyethylene.
Preferably, the migration conditions for migrating the sample are: the ophthalmic preparation container is placed for 0-24 months under the conditions that the temperature is 20-60 ℃ and the humidity is 50-80%.
In summary, the present application provides a method for detecting a plastic additive in an ophthalmic formulation container. According to the detection method, the extraction sample or the migration sample of the ophthalmic preparation container is treated by the extraction solvent, then high performance liquid chromatography is adopted for analysis, and the liquid chromatography condition is optimized, so that the solvent effect is overcome, the separation degree of a target peak is improved, the detection method can be used for detecting and safely evaluating the contents of the plastic additives 08 and 15 in the ophthalmic preparation container, the technical problems of poor accuracy and low sensitivity of the existing detection method are solved, and the high requirement on quality control of the plastic additives in the medicinal packaging material can be met.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive exercise.
FIG. 1 is a specificity profile of a control solution in example 1 of the present application;
FIG. 2 is a special spectrum of a labeled test solution in example 1 of the present application;
FIG. 3 is a specificity profile of a control solution in example 2 of the present application;
FIG. 4 is a specificity profile of a labeled test solution in example 2 of the present application;
FIG. 5 is a detection spectrum of a labeled test solution in comparative example 2 of the present application;
FIG. 6 is a detection spectrum of the labeled test solution in comparative example 3 of the present application.
Detailed Description
In order to make the objects, features and advantages of the present application more obvious and understandable, the technical solutions in the embodiments of the present application are clearly and completely described, and it is obvious that the embodiments described below are only a part of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The reagents and raw materials used in the examples of the present application are commercially available or self-made.
Example 1
The embodiment of the application relates to a detection method for extracting a plastic additive 15 in a sample of sodium hyaluronate eye drops and a single-dose eye drop bottle for low-density polyethylene medicine, which comprises the following specific steps:
1. solution preparation:
control solution: precisely weighing 25mg of a plastic additive 15 reference substance, placing the reference substance in a 10ml volumetric flask, adding an extraction reagent cyclohexane for dissolving and diluting, and fixing the volume and diluting to obtain a reference substance solution;
test solution: the low-density polyethylene medicinal single-dose eye drop bottle is cut into small pieces with the length and width not exceeding 1 cm. Precisely weighing about 2g of the small pieces, placing the small pieces in a glass flask, adding 80ml of toluene, boiling, stirring at a constant speed and refluxing for 90min, cooling to 60 ℃, adding 120ml of methanol under continuous stirring, filtering by using a glass funnel, leaching the flask, the funnel and filter paper by using a toluene-methanol (40: 60, v/v) mixed solution, combining filtrate and washing liquor, diluting by using the toluene-methanol (40: 60, v/v) mixed solution, fixing the volume to a 250ml measuring flask, and shaking uniformly. Precisely transferring 50ml of the solution, rotating and evaporating the solution at the temperature of 45 ℃ in a water bath to dryness, and dissolving the residue by using 5ml of cyclohexane to obtain the compound.
Adding a standard test solution: dissolving appropriate amount of the above residue with diluted reference solution, and preparing 100% limit concentration standard sample solution.
2. Liquid chromatography conditions:
and (3) chromatographic column: silica chromatographic column, column temperature 20 deg.c, flow rate 0.3 ml/min, sample volume 1 microliter, mobile phase n-hexane, CAD filtering 5.0s and CAD atomizer temperature 70 deg.c.
Example 2
The embodiment of the application relates to a method for detecting plastic additives 08 in extracted samples of sodium hyaluronate eye drops and low-density polyethylene medicinal single-dose eye drop bottles, which comprises the following specific steps:
1. solution preparation:
control solution: precisely weighing 25mg of a plastic additive 08 reference substance, placing the reference substance in a 10ml volumetric flask, adding an extraction reagent tetrahydrofuran-acetonitrile (50: 50, v/v) for dissolving and diluting, and fixing the volume and diluting to obtain a reference substance solution.
Test solution: the low-density polyethylene medicinal single-dose eye drop bottle is cut into small pieces with the length and the width not exceeding 1 cm. Precisely weighing about 2g of the small pieces, placing the small pieces into a glass flask, adding 80ml of toluene, boiling, stirring at a constant speed and refluxing for 90min, cooling to 60 ℃, adding 120ml of methanol under continuous stirring, filtering by using a glass funnel, leaching the flask, the funnel and filter paper by using a toluene-methanol (40: 60, v/v) mixed solution, combining filtrate and washing liquor, diluting by using the toluene-methanol (40: 60, v/v) mixed solution, fixing the volume to a 250ml measuring flask, and shaking uniformly. Precisely transferring 50ml of the above solution, rotary evaporating to dryness in 45 deg.C water bath, and dissolving the residue with 5ml of tetrahydrofuran-acetonitrile (50: 50, v/v).
Adding a standard test solution: dissolving appropriate amount of the above residue with diluted reference solution, and preparing 100% limit concentration standard sample solution.
2. Liquid chromatography conditions: and (3) chromatographic column: eighteen carbon chromatographic columns, the column temperature is 30 ℃, the flow rate is 2 ml/min, the sample injection volume is 5 mul, the detection wavelength is 280nm, and the mobile phase acetonitrile-water (70: 30) is adopted.
The detection method comprises the following verification results:
1. specificity property
And (3) respectively taking the extraction reagent, the reference substance solution, the test sample solution and the added standard test sample solution in the examples 1-2, and carrying out sample injection detection to investigate whether the target peak is interfered for determination. The specificity verification maps of the plastic additives 08 and 15 are respectively shown in figures 1-4, and the results show that the plastic additive 15 generates a peak at 13-14 min, the plastic additive 08 generates a peak at 23-24 min, the target peaks of the added standard test solution and the reference solution are consistent and are not influenced by the matrix environment, the extraction reagent and the test solution do not interfere with the target peaks, and the specificity of the methods for adding the standard test solution to the plastic additives 08 and 15 meets the requirements.
2. System applicability
The control solutions of examples 1-2 were injected into a high performance liquid chromatograph, and the relative standard deviation of each peak area of 6 consecutive control solutions was calculated. The results show that the RSD of the plastic additive 08 reference substance is 0.31 percent, the RSD of the plastic additive 15 reference substance is 0.27 percent, and the system applicability of the method meets the requirements.
3. Linearity
And respectively taking a plastic additive 08 reference substance solution with the concentration range of 24-720 mug/ml and a plastic additive 15 reference substance solution with the concentration range of 24-480 mug/ml for sample injection test, and taking the solution concentration (mug/ml) as a horizontal coordinate and the peak area as a vertical coordinate to make a standard curve. The result shows that the correlation coefficient r is 0.999 and is more than 0.990 in the concentration range of 23.96-718.80 mug/ml of the plastic additive 08, the requirement is met, and the linear relation is good. The plastic additive 15 is in the concentration range of 23.89-477.80 mug/ml, the correlation coefficient r is 0.996 and is larger than 0.990, and the requirement is met.
4. Quantitative and detection limits
And taking the control solution with the concentration of 1.1980 mug/ml in the example 1 as a quantitative limit solution, and carrying out continuous sample injection test for 6 needles, wherein the signal-to-noise ratio is more than 11, and the RSD is 4.4%. And taking a control solution with the concentration of 0.5990 mug/ml as a detection limit solution for continuous sample injection test for 2 needles, wherein the signal-to-noise ratio is greater than 5.5.
Taking the control solution with the concentration of 1.4334 mu g/ml in example 2 as a quantification limit solution, and carrying out continuous sample injection to test 6 needles, wherein the minimum value of the signal-to-noise ratio is 23.6, and the peak area RSD is not more than 5.4%. Taking a control solution with the concentration of 0.7167 mu g/ml as a detection limit solution, and continuously injecting a sample for testing 2 needles, wherein the minimum value of the signal-to-noise ratio is 26.1.
5. Accuracy of
The sample solutions of the samples to be tested were continuously loaded 3 times at the limit concentration of 100 in examples 1-2, respectively, and the recovery rates of the samples were calculated. The average recovery of the plastics additive 08 was 92.82% with an RSD of 2.56%. The average recovery of the plastics additive 15 was 90.95% and the RSD was 0.40%.
6. Stability of
The sample solution of the sample added with the standard at the limit concentration of 100% in example 1 was placed at room temperature (25 ℃) for 5 hours, 36 hours and 43.5 hours, and the sample injection was performed respectively, and the peak area was compared with the peak area of 0 hour. The results show that the 100% limiting concentration of the plastics additive 08 plus standard test article solution is stable for at least 43.5 hours at room temperature (25 ℃).
The sample solution added with the standard at the limit concentration of 100% in example 2 was taken and placed at room temperature (25 ℃) for 3h, 18h and 24h, and the respective injection samples were compared with the peak area of 0 h. The results show that the 100% limiting concentration of the plastic additive 15 in the test sample solution is stable for at least 24 hours at room temperature (25 ℃).
Comparative example 1
Referring to the method for detecting the plastic additive 15 in the extracted samples of the sodium hyaluronate eye drops and the low-density polyethylene medicinal single dose eye drop bottle in example 1, the difference is only that the mobile phases are respectively adjusted to be isopropanol and isopropanol: n-hexane (10: 90, v/v), and preparing a standard sample solution for sample loading detection. The results show that the target peak response is low, no peak is generated basically, and the method is not applicable.
Comparative example 2
Referring to the method for detecting the plastic additive 08 in the extracted samples of the sodium hyaluronate eye drops and the low-density polyethylene medicinal single-dose eye drop bottle in example 2, the difference is only that acetonitrile-water (90: 10) is respectively adjusted as a mobile phase, and toluene is replaced by dichloromethane for pretreatment to obtain an extracted sample which is configured to be added with a sample solution to be tested. The experimental map is shown in figure 5, and the result shows that the retention time of the target peak is about 5min, the peak of the target peak is too early and is close to the peak of the solvent, and the detection of the object to be detected is influenced.
Comparative example 3
Referring to the method for detecting the plastic additive 08 in the extracted samples of the sodium hyaluronate eye drops and the low-density polyethylene medicinal single dose eye drop bottle in the example 2, the difference is only that acetonitrile-water (90: 10) is respectively adjusted as a mobile phase, and a sample solution to be tested is prepared for sample loading detection. The experimental map is shown in figure 6, and the result shows that an impurity peak exists near the target peak, the separation degree is less than 1.5, the recovery rate is less than 50%, and the method is not applicable.
The above embodiments are only used for illustrating the technical solutions of the present application, and not for limiting the same; although the present application has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions in the embodiments of the present application.
Claims (3)
1. A method for detecting a plastic additive in an ophthalmic formulation container, comprising the steps of:
boiling a low-density polyethylene medicinal bottle in toluene, refluxing, adding methanol, filtering, and diluting with a mixed solvent of toluene and methanol to obtain an extracted sample;
taking an extracted sample of a low-density polyethylene medicinal bottle, evaporating to dryness in a water bath, dissolving and diluting residues by using an extraction reagent, and analyzing by adopting high performance liquid chromatography, wherein the extraction reagent of the plastic additive 15 is cyclohexane, the extraction reagent of the plastic additive 08 is tetrahydrofuran and acetonitrile, and the volume ratio is (1-2): 1;
the liquid chromatography conditions for the plastic additive 08 were: the chromatographic column adopts a C18 chromatographic column, and the volume ratio of mobile phases is acetonitrile: water (70-80) = (20-30), detection wavelength is 260-280 nm, column temperature is 20-30 ℃, flow rate is 0.5-2 ml/min, and sample injection volume is 1-5 mul;
the liquid chromatographic conditions of the plastic additive 15 were: the mobile phase is cyclohexane, the chromatographic column is a silica chromatographic column, the detector is a CAD detector, the temperature of a CAD atomizer is 60-80 ℃, the column temperature is 20-30 ℃, the flow rate is 0.5-2 ml/min, and the sample injection volume is 1-5 mu l.
2. The method of claim 1, wherein the volume ratio of toluene to methanol is 1: (1-2), wherein the volume ratio of toluene to methanol in the mixed solvent is 1: (1-2).
3. The method of claim 1, wherein the ophthalmic formulation comprises sodium hyaluronate eye drops.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999051230A1 (en) * | 1998-04-02 | 1999-10-14 | Novartis Ag | Method for stabilizing pharmaceutical compositions by special use of an antioxidant |
| CN113030319A (en) * | 2021-03-09 | 2021-06-25 | 中国计量科学研究院 | Method for extracting additive in plastic |
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- 2022-04-12 CN CN202210377266.2A patent/CN114441691B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999051230A1 (en) * | 1998-04-02 | 1999-10-14 | Novartis Ag | Method for stabilizing pharmaceutical compositions by special use of an antioxidant |
| CN1295474A (en) * | 1998-04-02 | 2001-05-16 | 诺瓦提斯公司 | Method for stabilizing pharmaceutical composition by special use of antioxidant |
| CN113030319A (en) * | 2021-03-09 | 2021-06-25 | 中国计量科学研究院 | Method for extracting additive in plastic |
Non-Patent Citations (3)
| Title |
|---|
| Non-targeted analysis and risk assessment of non-volatile compounds in polyamide food contact materials;Yajing Hu等;《Food Chemistry》;20201116;第345卷;第1-9页 * |
| Rapid Identification of Antioxidants in Pharmaceutical Packagings with Planar Chromatography Coupled with Photodensitometric Detection;H. El Mansouri等;《Journal of Liquid Chromatography & Related Technologies》;19981231;第21卷(第12期);第1845-1855页 * |
| 药用丁基胶塞与注射用氨曲南相容性研究;韩程佳等;《现代生物医学进展》;20200531;第20卷(第9期);第1624-1630页 * |
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