CN112083086A - Micro-determination method for migration and dissolution of pigment red 254 in medical light-resistant material - Google Patents
Micro-determination method for migration and dissolution of pigment red 254 in medical light-resistant material Download PDFInfo
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- G—PHYSICS
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- 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
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- G—PHYSICS
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Abstract
The invention belongs to the technical field of detection, and particularly relates to a micro-determination method for migration and dissolution of pigment red 254 in a medical light-resistant material. The determination method is reversed-phase high performance liquid chromatography. The pigment red 254 has good linear relation in the concentration range of 5.200 ng/mL < -1 > -208.0 ng/mL < -1 >, and the detection limit is 1.560ng·mL‑1The limit of quantitation is 5.200 ng/mL‑1. The method has good precision; the solution is stable within 12h, and the accuracy of the detection result can be ensured. The method has the advantages that the 7 kinds of medicine solution do not interfere the determination of the pigment red 254, and the recovery rate is good.
Description
Technical Field
The invention belongs to the technical field of detection, and particularly relates to a micro-determination method for migration and dissolution of pigment red 254 in a medical light-resistant material.
Background
Many pharmaceutical ingredients clinically used are sensitive to light and easy to decompose in the presence of light, so that pigment red 254 is added to some pharmaceutical polymer materials as a light-shielding agent, such as disposable light-shielding infusion sets, light-shielding plastic bottles and the like, and the migration and dissolution amount of the pigment red 254 of the light-shielding agent of the materials containing the pigment red 254 directly contacting with the drugs needs to be researched so as to determine whether the migration and dissolution amount is within a safe range.
Pigment Red 254 (CAS number: 84632-65-5) has the chemical name bis (p-chlorophenyl) -1, 4-diketopyrrolopyrrole. The molecular structural formula is as follows:
at present, no report of a micro-determination method for migration and dissolution of pigment red 254 in a light-resistant material for medical use is available. Disclosure of Invention
In order to solve the technical problems, the invention provides a micro-measurement method for migration and dissolution of pigment red 254 in a light-resistant material for medicine. The method is reversed phase high performance liquid chromatography.
The invention is realized by the following technical scheme:
a micro-measuring method for migration and dissolution of pigment red 254 in a medical lightproof material is a reversed phase high performance liquid chromatography.
In the method for micro-measuring migration and dissolution of pigment red 254 in the light-resistant material for medicine, the reversed phase high performance liquid chromatography comprises the following chromatographic conditions: the chromatographic column is ZORBAX SB-C18(ii) a The mobile phase is acetonitrile-water; the detection wavelength was 504 nm.
In the method for micro-determination of migration and dissolution of pigment red 254 in the light-resistant material for medicine, the chromatographic column ZORBAX SB-C18Model number of 150 Í 4.6.6 mm, 5μm。
In the above method for micro-determination of migration and dissolution of pigment red 254 in the light-resistant material for medicine, the volume ratio of acetonitrile-water is 55: 45.
the micro-determination method for migration and dissolution of pigment red 254 in the light-resistant material for medicine comprises the following steps:
chromatographic conditions chromatographic column: ZORBAX SB-C18（150Í4.6 mm，5 μm); mobile phase: acetonitrile-water (55: 45); detection wavelength: 504 nm; flow rate: 1.0 mL/min-1(ii) a Column temperature: 35 ℃。
Assay method
Preparation of control solutions: taking an appropriate amount of pigment Red 254 reference substance, precisely weighing, and dissolving with dimethyl sulfoxide to obtain about 50 ng/mL-1The solution of (4) as a control solution;
preparation of a test solution: taking a light-proof infusion set 1, and dripping 500mL of a drug solution for 8 hours at a speed of 20 drops/min or 24 hours circularly according to a clinical use method to serve as a test solution;
precisely measuring each of the reference solution and the sample solution 50μAnd injecting the L into a high performance liquid chromatograph, recording a chromatogram, and calculating the content of the pigment red 254 in the test sample according to an external standard method.
The external standard method calculation is disclosed as follows: cTest article=CReference substance×ATest article/AAnd (5) a reference substance.
Wherein, CThe test article is a test articleConcentration of solution, CReference substanceConcentration of control solution, AThe test article is a test articlePeak area of solution, AReference substanceThe peak area of the control solution.
500mL of the drug solution was recorded in the corresponding package insert for each drug according to the clinical method of use. Specifically, in the present application, 500mL of the drug solution is shown in table 1 according to the clinical use method.
The invention has the beneficial effects that:
the invention provides a micro-determination method for migration and dissolution of pigment red 254 in a light-resistant material for medicine. The results of the linear range test show that pigment Red 254 is 5.200 ng.mL-1～208.0ng·mL-1The linear relationship within the concentration range is good. The detection limit and the quantitative limit test result show that the detection limit of the pigment red 254 of the method is 1.560ng·mL-1The limit of quantitation was determined to be 5.200 ng/mL in terms of 10 times the noise-1. The precision test result shows that the method has good precision. The stability test result of the solution shows that the solution is stable within 12h, and the accuracy of the detection result can be ensured. The results of the method specificity tests show that the 7 kinds of medicine solutions do not interfere the measurement of the pigment red 254And (4) determining. The recovery test results showed an average recovery of 100.6% and an RSD of 1.5%, indicating that the recovery of the process was good.
Detailed Description
The present invention will be further described with reference to specific examples so that those skilled in the art may better understand the present invention, but the present invention is not limited thereto.
Unless otherwise specified, concentrations generally refer to the weight to volume ratio of solute to solution, g/ml. If the solute is a liquid, the concentration is by volume, e.g., 0.1% aqueous triethylamine solution means 0.1ml triethylamine dissolved in 100ml water.
Example 1
A methodological experiment is carried out on the method for determining the migration and dissolution of the pigment red 254 in the light-resistant material for medicine, and the specific conditions are as follows:
test protocol and test drugs
The migration and dissolution of pigment red 254 added into a light-resistant filtering infusion set are studied by simulating a clinical instillation mode, increasing the dosage and prolonging the extraction time and selecting 500mL each of 3 extreme solvents and 7 medicine solutions. The pigment red 254 dissolution profile is shown in table 1.
TABLE 1 pigment Red 254 dissolution protocol
| Extraction solvent | Concentration of | Test temperature | Extraction method |
| Ethanol | 65% | 40℃±2℃ | 20 drops/min circulation dripping for 24 hours |
| Hydrochloric acid solution | 0.1mol/L | 40℃±2℃ | 20 drops/min circulation dripping for 24 hours |
| Sodium hydroxide solution | 0.1mol/L | 40℃±2℃ | 20 drops/min circulation dripping for 24 hours |
| Vitamin B6Injection solution | 0.4mg/ml | 25℃±1℃ | 20 drops/min instillation for 8 hours |
| Vitamin C injection | 1mg/ml | 25℃±1℃ | 20 drops/min instillation for 8 hours |
| Levofloxacin hydrochloride sodium chloride injection | 2mg/ml | 25℃±1℃ | 20 drops/min instillation for 8 hours |
| Vitamin K1Injection solution | 0.04mg/ml | 25℃±1℃ | 20 drops/min instillation for 8 hours |
| Sodium nitroprusside for injection | 0.1mg/ml | 25℃±1℃ | 20 drops/min instillation for 8 hours |
| Cisplatin injection | 0.06mg/ml | 25℃±1℃ | 20 drops/min instillation for 8 hours |
| Vincristine sulfate for injection | 0.008mg/ml | 25℃±1℃ | 20 drops/min instillation for 8 hours |
2 reagent and instrument
High performance liquid chromatograph (Shimadzu, LC-20AT, SIL-20A, SPD-20A, CTO-20A, DGU-20A)5R) (ii) a High performance liquid chromatography (agilent, 1260 definition, DAD); electronic analytical balance (Sartorius, BT 125D); digital display constant temperature water bath (HH-4, Shuangjie laboratory instruments, jin Tan) acetonitrile is chromatographically pure, other reagents are analytically pure; the used infusion medicines are all samples sold in the market;
3 micro-determination methodology research of pigment red 254 migration dissolution in light-resistant material for medicine
3.1 chromatographic conditions
A chromatographic column: ZORBAX SB-C18（150Í4.6 mm，5 μm); mobile phase: acetonitrile-water (55: 45); detection wavelength: 504 nm; flow rate: 1.0 mL/min-1(ii) a Column temperature: 35 ℃; sample introduction amount: 50μL。
3.2 Linear Range
10.40mg of pigment Red 254 control sample was diluted with dimethyl sulfoxide to 208.0 ng/mL-1、52.00 ng·mL-1、26.00 ng·mL-1、10.40 ng·mL-1、5.200 ng·mL-150 μ L of the solution was injected, and the chromatogram was recorded. Taking the concentration as a horizontal coordinate and the peak area as a vertical coordinate to make a regression curve, and obtaining a linear regression equation as follows: y = 345.37x +758.08, R2= 0.9998. The results show that pigment Red 254 is 5.200 ng.mL-1～208.0ng·mL-1The linear relationship within the concentration range is good.
3.3 detection and quantitation limits
Diluting the stock solution of the reference substance step by step, injecting a sample, and recording a chromatogram. The detection limit is 1.560 measured by 3 times of the noiseng·mL-1The limit of quantitation was determined to be 5.200 ng/mL in terms of 10 times the noise-1。
3.4 precision test
Get 52.00 ng·mL-1The sample is continuously injected into the control solution of (1), the peak area of the pigment red 254 is measured, and the precision RSD in the day is calculated to be 1.2%. The results show that the method is good in precision.
3.5 stability of the solution
Get 52.00 ng·mL-1The reference substance solution is injected for 1 time in 0h, 2h, 4h, 6h, 8h and 12h respectively, the peak area of pigment red 254 is determined, and the RSD is 0.6%. The solution is stable within 12 hours, and the accuracy of the detection result can be ensured.
3.6 method specificity
Precisely measuring 208.0 ng/mL-15ml of the control solution is put into a 25ml measuring flask, 7 parts are respectively used, 7 kinds of medicine solutions are diluted respectively, namely, 7 kinds of medicine solutions, namely, vitamin B6 injection (0.4 mg/ml), vitamin C injection (1 mg/ml), levofloxacin hydrochloride sodium chloride injection (2 mg/ml), vitamin K1 injection (0.04 mg/ml), sodium nitroprusside injection (0.1 mg/ml), cisplatin injection (0.06 mg/ml) and vincristine sulfate injection (0.008 mg/ml) are released to a scale mark, shaken uniformly, 50 mu L of the injection is injected respectively, and a chromatogram is recorded. As a result: the 7 drug solutions did not interfere with the determination of pigment Red 254.
3.7 recovery test
The amount of the solution was 208.0 ng/mL-15ml of the control solution is placed in a 25ml measuring flask, diluted to the scale with dimethyl sulfoxide, shaken up, 50 μ L of sample is injected, and the chromatogram is recorded. The recovery of pigment Red 254 added to 7 drug solutions under the term "3.6 method specificity" was calculated. The results are shown in the table below, with an average recovery of 100.6% and an RSD of 1.5%, indicating a good recovery for this process.
Pigment Red 254 recovery yield measurement
3.8 dissolution and measurement
Taking 3 batches of light-resistant infusion sets, preparing an extracting solution according to the method in the table 1, and measuring according to the established method after filtering. The test results show that: 500mL each of 65% ethanol, 0.1mol/L hydrochloric acid solution, 0.1mol/L sodium hydroxide solution and 7 kinds of medicinal solutions was used as an extraction solvent, and no pigment Red 254 was detected in the extract. According to the detection limit calculation of the method, the total dissolution amount of the pigment red 254 in each set of the lightproof infusion apparatus is less than 0.78 mu g.
Claims (5)
1. A micro-measuring method for migration and dissolution of pigment red 254 in a medical light-resistant material is characterized in that the measuring method is a reversed phase high performance liquid chromatography.
2. The microassay method of migration and dissolution of pigment red 254 in a light-resistant material for pharmaceutical use according to claim 1, wherein said reversed-phase high performance liquid chromatography comprises the following chromatographic conditions: the chromatographic column is ZORBAX SB-C18(ii) a The mobile phase is acetonitrile-water; the detection wavelength was 504 nm.
3. The method for microassay of migration and dissolution of pigment Red 254 in a light-shielding material for pharmaceutical use according to claim 2, wherein said column is ZORBAX SB-C18Model number of 150 Í 4.6.6 mm, 5μm。
4. The microassay method for migration and dissolution of pigment red 254 in a light-resistant material for medicine according to claim 2, wherein the volume ratio of acetonitrile-water is 55: 45.
5. the microassay method of migration and dissolution of pigment red 254 in a light-shielding material for pharmaceutical use according to claim 2, wherein said microassay method comprises the steps of:
chromatographic conditions chromatographic column: ZORBAX SB-C18（150Í4.6 mm，5 μm); mobile phase: acetonitrile-water (55: 45); detection wavelength: 504 nm; flow rate: 1.0 mL/min-1(ii) a Column temperature: 35 ℃;
assay method
Preparation of control solutions: taking an appropriate amount of pigment Red 254 reference substance, precisely weighing, and dissolving with dimethyl sulfoxide to obtain about 50 ng/mL-1The solution of (4) as a control solution;
preparation of a test solution: taking a light-proof infusion set 1, and dripping 500mL of a drug solution for 8 hours at a speed of 20 drops/min or 24 hours circularly according to a clinical use method to serve as a test solution;
precisely measuring each of the reference solution and the sample solution 50μAnd injecting the L into a high performance liquid chromatograph, recording a chromatogram, and calculating the content of the pigment red 254 in the test sample according to an external standard method.
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Citations (4)
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| US20010004511A1 (en) * | 1999-12-15 | 2001-06-21 | Kazuo Takebe | Pigment-dispersion photo-sensitive coating solution |
| CN103339536A (en) * | 2011-01-28 | 2013-10-02 | 东洋油墨Sc控股株式会社 | Diketopyrrolopyrrole-type pigment composition for color filters, colored composition for color filters, and color filter |
| CN105486794A (en) * | 2015-12-25 | 2016-04-13 | 广州广电计量检测股份有限公司 | Method for detecting banned dye in printing ink |
| CN108663445A (en) * | 2018-03-22 | 2018-10-16 | 张宪臣 | The remaining analysis method of multiple pollutant in a kind of measurement food contact material acidity simulation soak |
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2020
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010004511A1 (en) * | 1999-12-15 | 2001-06-21 | Kazuo Takebe | Pigment-dispersion photo-sensitive coating solution |
| CN103339536A (en) * | 2011-01-28 | 2013-10-02 | 东洋油墨Sc控股株式会社 | Diketopyrrolopyrrole-type pigment composition for color filters, colored composition for color filters, and color filter |
| CN105486794A (en) * | 2015-12-25 | 2016-04-13 | 广州广电计量检测股份有限公司 | Method for detecting banned dye in printing ink |
| CN108663445A (en) * | 2018-03-22 | 2018-10-16 | 张宪臣 | The remaining analysis method of multiple pollutant in a kind of measurement food contact material acidity simulation soak |
Non-Patent Citations (5)
| Title |
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| INES SCHREIVER 等: "Identification and hazard prediction of tattoo pigments by means of pyrolysis—gas chromatography/mass spectrometry", 《ARCH TOXICOL》 * |
| JOANNA RUSSELL 等: "The identification of synthetic organic pigments in modern paints and modern paintings using pyrolysis-gas chromatography–mass spectrometry", 《ANAL BIOANAL CHEM》 * |
| 于风平 等: "避光输液器中颜料棕25和UV-327的迁移溶出研究", 《药物分析杂志》 * |
| 于风平 等: "避光输液器中颜料橙64和DEHP的迁移溶出研究", 《药物分析杂志》 * |
| 吕艳英 等: "C.I.颜料红254分散体制备及其在彩色滤光片中的应用", 《华东理工大学学报(自然科学版)》 * |
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Inventor after: He Dunwei Inventor after: Dai Mei Mei Inventor after: Yu Fengping Inventor after: Yan Min Inventor before: Dai Mei Mei Inventor before: Yu Fengping Inventor before: Yan Min Inventor before: He Dunwei |