CN103601840B - The preparation of polyacrylamide immobilization ionic liquid capillary monolithic column and solid phase extraction method - Google Patents
The preparation of polyacrylamide immobilization ionic liquid capillary monolithic column and solid phase extraction method Download PDFInfo
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Abstract
The preparation of polyacrylamide immobilization ionic liquid capillary monolithic column and solid phase extraction method, form polymkeric substance by glycidyl methacrylate, acrylamide, N, N-methylene-bis acrylamide and 1-aminopropyl-3-Methylimidazole villaumite.Glycidyl methacrylate and 1-aminopropyl-3-Methylimidazole villaumite are reacted in containing formamide soln, form the monomer of band ion liquid functional group, add monomeric acrylamide, linking agent N subsequently, N '-methylene-bisacrylamide, under the existence of pore-creating agent polyoxyethylene glycol, then add initiator Diisopropyl azodicarboxylate formation polyacrylamide immobilization ionic liquid solution.In kapillary, heated polymerizable makes polyacrylamide immobilization ionic liquid capillary monolithic column.Preparation method is simple, and with low cost, easy control of reaction conditions, has good physical strength, be applied to Solid-Phase Extraction, and loading capacity is large, the rate of recovery is high, favorable reproducibility, is suitable for extraction carboxylic acid compound.
Description
Technical field
The present invention relates to stratographic analysis Sample Pretreatment Technique Used, particularly a kind of preparation of polyacrylamide matrix immobilization ionic liquid capillary monolithic column and the method for Solid-Phase Extraction thereof.
Background technology
Solid-Phase Extraction is as a kind of Sample Pretreatment Technique Used extensively taked, utilize analyte in different media by the feature of capacity variance of adsorbing, effectively target compound is separated with interfering component, enhance the Detection capability to analyte particularly trace analysis thing, also improve the rate of recovery of sample simultaneously.This technology is not only suitable for Trace Organic Compounds in extracting and enriching food and environmental water sample, and the enrichment of determined component in applicable biological sample.The better sorbent material of current development selectivity is the active area of Solid-Phase Extraction research.
In recent years, because integral material is by the method for in-situ polymerization, can be prepared in various upholder, such as be prepared in the injector syringe, Tip head, kapillary, chip channel etc. of stainless steel tube, polypropylene material, easily realize the regulation and control to integral post pore structure, surface properties, specific surface area.For the column extractor of loaded particles sorbent material, adopt integral material as sorbent material, not only eliminate loaded down with trivial details filling process, without the need to loading sieve plate or sintering plunger, and in integral material, distinctive through hole is that the flowing of liquid provides large hole path, instead of diffusion mass transfer slowly, make resistance to mass transfer obviously reduce with convective mass transfer, be conducive to the raising of extraction efficiency, thus obtain increasing concern.
Ionic liquid refers to the organic molten salt be in a liquid state under room temperature (or a little higher than room temperature), by specific volume relatively large, the asymmetric organic cation of structure and the relatively little inorganic anion of volume form, have that volatility is low, thermostability and chemical stability is good, with water and the adjustable viscosity of organic solvent and solvability and the advantage to organism and the good extraction ability of metal ion, be considered to a kind of novel green solvent of alternative conventional solvent, be widely used in sample pretreatment.Immobilization ionic liquid is immobilized to by ionic liquid on organic polymer material or inorganic porous material, thus obtaining the solid matter that supported ion liquid or surface have ionic liquid structure, obtained immobilization ionic liquid has the characteristic of ionic liquid and porous carrier materials concurrently.Compared with free state ionic liquid, immobilization ionic liquid can increase specific surface area, thus improves its utilising efficiency and stability, and the consumption of ionic liquid obviously reduces, and the separation after using, recycling easily realize.In Solid-Phase Extraction, immobilization ionic liquid is mainly as coating (Y. Meng, V. Pino, the J. L. Anderson of solid-phase microextraction, Anal. Chim. Acta 2011,687,141-149), or immobilized at polymer beads (W. Bi, M. Tian, K. H. Row, J. Sep. Sci. 2010,33,1739-1745) with (G. Fang on silica gel particle, J. Chen, J. Wang, J. He, S. Wang, J. Chromatogr. A 2010,1217,1567-1574).
CN102500346A proposes a kind of sol-gel and surface-functionalized technology of golden nanometer particle of adopting and prepares novel ion liquid silica gel capillary monolithic column stationary phase, for capillary liquid chromatography and capillary electrochromatography Separation of Benzene amine or polynuclear aromatics compounds.But it connects silica gel and ionic liquid imidazoles bromine salt with golden nanometer particle, there is cost high and make the problems such as difficulty, be difficult to apply in the trace organic substance abstraction technique of food and environmental water sample.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of polymkeric substance be made up of polyacrylamide immobilization ionic liquid, adopts this polymkeric substance to prepare capillary monolithic column, for the Solid-Phase Extraction to carboxylic acid compound.
The present invention realizes above-mentioned purpose by the following technical solutions:
Polyacrylamide immobilization ion liquid polymer is made up of glycidyl methacrylate, acrylamide, N, N-methylene-bis acrylamide and 1-aminopropyl-3-Methylimidazole villaumite.
The elementary cell of polyacrylamide immobilization ionic liquid chemical structural formula is:
The synthetic method of polyacrylamide immobilization ion liquid polymer, comprises the following steps:
Glycidyl methacrylate and 1-aminopropyl-3-Methylimidazole villaumite are reacted in containing formamide soln, forms the monomer of band ion liquid functional group; Add monomeric acrylamide, linking agent N, N '-methylene-bisacrylamide subsequently, under the existence of pore-creating agent polyoxyethylene glycol, then add initiator Diisopropyl azodicarboxylate formation polyacrylamide immobilization ionic liquid solution.
The mass ratio of described glycidyl methacrylate and 1-aminopropyl-3-Methylimidazole villaumite is 1:1 ~ 1:3.
Described acrylamide and N, N '-methylene-bisacrylamide is 1:1:1 ~ 1:3:3 with the mass ratio of the monomer that band ion liquid functional is rolled into a ball.
The preparation method of polyacrylamide immobilization ionic liquid capillary monolithic column, comprises the following steps:
A, first by quartz capillary successively through persalt, water, sodium hydroxide, water, washed with methanol, and after drying, after the silicone hydroxyl added on the methanol solution of band γ-2 methyl allyl acyloxypropyl trimethoxysilane and capillary wall reacts, dry up stand-by;
B, the polyacrylamide immobilization gas ions solution prepared is injected into above-mentioned in the kapillary of vinyl modified, polyreaction 20 ~ 24 hours in 65 ~ 80 DEG C of waters bath with thermostatic control, use polymkeric substance in washed with methanol kapillary again, obtain polyacrylamide immobilization ion capillary monolithic column.
Polyacrylamide immobilization ionic liquid capillary monolithic column is used for the method for Solid-Phase Extraction carboxylic acid compound:
Polyacrylamide immobilization ionic liquid capillary monolithic column is first used distilled water flushing, then uses the hydrochloride buffer equilibration capillary integral post of pH 6.3; By carboxylic acid compound with after flow velocity loading 60 ~ 80 min of 10 ~ 13.3 μ L/min, the formic acid of employing 10% and 40% acetonitrile mixing solutions are with flow velocity wash-out 4 ~ 10 min of 4 ~ 10 μ L/min, elutriant will be collected with after 5000 ~ 6000 rpm whizzer high speed centrifugations, carry out stratographic analysis with Ultra Performance Liquid Chromatography instrument.
Advantage of the present invention and positively effect are: be prepared in kapillary by polyacrylamide immobilization ionic liquid solution first, the method preparing polyacrylamide immobilization ionic liquid capillary monolithic column is simple, with low cost, easy control of reaction conditions, obtained novel capillary integral post has stronger physical strength, and be applied to Solid-Phase Extraction, the rate of recovery is high, loading capacity is large, favorable reproducibility, is applicable to extract carboxylic acid compound.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of polyacrylamide immobilization ionic liquid preparation method A;
Fig. 2 a and Fig. 2 b is the schematic diagram of polyacrylamide immobilization ionic liquid preparation method B;
Fig. 3 is the color atlas of polyacrylamide immobilization ionic liquid capillary monolithic column for carboxylic acid compound in Solid-Phase Extraction soda pop of embodiment 1 preparation.(A) direct injection; (B) sample introduction is extracted.In Fig. 3, peak 1 is m-Salicylic acid; Peak 2 is phenylformic acid; Peak 3 is styracin; Peak 4 is 2,4 dichlorophenoxyacetic acid; Peak 5 is m-TrifluoromethylcinnaAcid Acid;
Fig. 4 is the color atlas of polyacrylamide immobilization ionic liquid capillary monolithic column for carboxylic acid compound in Solid-Phase Extraction mineral water of embodiment 2 preparation.(A) direct injection; (B) sample introduction is extracted.In Fig. 4, peak 1 is PCA; Peak 2 is P-hydroxybenzoic acid; Peak 3 is m-Salicylic acid; Peak 4 is forulic acid; Peak 5 is 2-hydroxyl-3-naphthoic acid.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1: as shown in Figure 1, the active amino that epoxy group(ing) glycidyl methacrylate contained and 1-aminopropyl-3-Methylimidazole villaumite contain reacts in methane amide, form the monomer of band ion liquid functional group, add monomeric acrylamide subsequently, linking agent N, N '-methylene-bisacrylamide, at pore-creating agent (PEG 8000, PEG 10000) existence under, add initiator Diisopropyl azodicarboxylate (AIBN), above-mentioned polymers soln is injected in the quartz capillary of vinyl modified, react 20 hours in 80 DEG C of thermostat water baths, finally use washed with methanol stand-by.
The pre-treatment of vinyl modified kapillary: after quartz capillary being used successively 0.5 mol/L HCl, distilled water, 0.5 mol/L NaOH, distilled water, washed with methanol 30 min, dry up with nitrogen, again with syringe by 50%(v/v) the methanol solution of γ-2 methyl allyl acyloxypropyl trimethoxysilane pour in kapillary, after two ends being sealed with silica gel, at room temperature react 12 hours, with methyl alcohol, γ-2 methyl allyl acyloxypropyl trimethoxysilane remained in kapillary is rinsed well again, and capillary column is placed in gas-chromatography stove, at the N of 70 ° of C
2flow down dry 1 hour.
By function monomer glycidyl methacrylate 20.6 mg, ionic liquid 1-aminopropyl-3-Methylimidazole villaumite 30.8 mg, solvent is held concurrently pore-creating agent methane amide 679.4 mg, pH 8-9 is adjusted to NaOH, at room temperature mix, 40 ° of C react 1 hour, form the monomer of band ion liquid functional group, subsequently, at 2-8 ° of C refrigerator and cooled but 10 min, add monomeric acrylamide 10.0 mg, linking agent N, N '-methylene-bisacrylamide 20.0 mg, pore-creating agent PEG 8,000 45 mg and PEG 10,000 25 mg, initiator Diisopropyl azodicarboxylate 0.5 mg, at room temperature ultrasonicly to mix, pour in the quartz capillary of vinyl modified, seal with silica gel, react 20 hours in the thermostat water bath of 80 ° of C, after polyreaction completes, unreacted monomer is removed with washed with methanol quartz capillary, linking agent and pore-creating agent, obtain polyacrylamide immobilization ionic liquid capillary monolithic column.
Embodiment 2: as shown in Figure 2 a and 2 b, by monomer methacrylic acid glycidyl ester and acrylamide, linking agent N, N '-methylene-bisacrylamide, at pore-creating agent (PEG 8000, PEG 10000, methane amide) existence under, add initiator Diisopropyl azodicarboxylate, above-mentioned polymers soln is injected in the quartz capillary of vinyl modified, react in the thermostat water bath of 65 ° of C and generate acrylamide-N in 24 hours, N '-methylene-bisacrylamide-glycidyl methacrylate polymkeric substance, use the unreacted function monomer of washed with methanol and linking agent subsequently, integral post is balanced again with buffered soln, finally, the integral post of above synthesis is slowly rinsed with the ionic liquid 1-aminopropyl-3-Methylimidazole villaumite that buffered soln dissolves, by immobilized on integral material for ionic liquid 1-aminopropyl-3-Methylimidazole villaumite.
Described acrylamide, N, N '-mass ratio between methylene-bisacrylamide and glycidyl methacrylate is 1:1:1 ~ 1:3:3; The mass ratio of described acrylamide-N, N '-methylene-bisacrylamide-glycidyl methacrylate polymkeric substance and 1-aminopropyl 3-Methylimidazole villaumite is 1:1 ~ 1:3.
The pre-treatment of vinyl modified kapillary is with embodiment 1.
By function monomer glycidyl methacrylate 20.6 mg and acrylamide 10.0 mg, linking agent N, N '-methylene-bisacrylamide 20.0 mg, solvent is held concurrently pore-creating agent methane amide 679.4 mg, pore-creating agent PEG 8,000 45 mg and PEG 10,000 25 mg, initiator Diisopropyl azodicarboxylate 0.5 mg, at room temperature ultrasonicly to mix, pour in the quartz capillary of vinyl modified, seal with silica gel, react 24 hours in the thermostat water bath of 65 ° of C, after polyreaction completes, unreacted monomer is removed with washed with methanol quartz capillary, linking agent and pore-creating agent.Use 10 mM Tris-HCl(pH 8.0 again) solution flushing pillar 30 min, subsequently, the ionic liquid 1-aminopropyl-3-Methylimidazole villaumite of 30.8 mg/mL (is dissolved in 10 mM Tris-HCl, pH 8.0) rinse with flow velocity slowly the integral post as above prepared, obtain polyacrylamide immobilization ionic liquid capillary monolithic column, stand-by.
Embodiment 3: the polyacrylamide immobilization ionic liquid capillary monolithic column prepared by checking example 1 is to the Solid-Phase Extraction performance of carboxylic acid compound, with prepared polyacrylamide immobilization ionic liquid capillary monolithic column for spe medium, Ultra Performance Liquid Chromatography is adopted to analyze soda pop.
Soda pop sample preparation: measure soda pop 1 mL, 10 mL are caused with the hydrochloric acid buffer solution dilution of pH 6.3, after the nylon leaching film of 0.45 μm, add the styracin of the m-Salicylic acid of 0.02 μ g/mL, phenylformic acid, 2,4 dichlorophenoxyacetic acid and 0.04 μ g/mL, the extraction of m-TrifluoromethylcinnaAcid Acid standardized solution sample introduction.
Extraction conditions: adopt the capillary monolithic column that example 1 is made, first rinse with water, by the hydrochloric acid buffer solution equilibration capillary integral post of pH 6.3, with flow velocity loading 80 min of 10 μ L/min, finally adopt formic acid and the 40% acetonitrile mixing solutions of 10%, with flow velocity wash-out 4 min of 10 μ L/min, collect elutriant, after 6000 rpm high speed centrifugations, analyze with Ultra Performance Liquid Chromatography.
Chromatographiccondition: analytical column is Acclaim
tMrSLC 120 C18 (2.1 × 150 mm, 2.2 μm), moving phase is 10 mM ammonium formiates and 0.1% formic acid mixing buffered soln and 42% acetonitrile of 58%, flow velocity 0.3 mL/min, sample introduction 10 μ L, column temperature 30 ° of C, determined wavelength 230 nm.
Fig. 3 color atlas (A) is extraction sample introduction, and color atlas (B) is direct injection.As shown in Fig. 3 (B), soda pop sample is not before Solid-Phase Extraction, and the sample signal of detection is lower.As shown in Fig. 3 (A), soda pop sample is after fiber material provided by the invention carries out Solid-Phase Extraction, and each compound obtains good enrichment and is separated, and is not subject to impurity interference, and elution peak 1 is m-Salicylic acid successively; 2 is phenylformic acid; 3 is styracin; 4 is 2,4 dichlorophenoxyacetic acid; 5 is m-TrifluoromethylcinnaAcid Acid, and the rate of recovery is respectively 85.7%, 95.1%, 97.4%, 96.8% and 106.1%, and the relative standard deviation of extractive analysis is less than 8%, illustrates that this Solid-Phase Extraction material is applicable to the analysis of soda pop.
Embodiment 4: the polyacrylamide immobilization ionic liquid capillary monolithic column prepared by checking example 2 is to the Solid-Phase Extraction performance of carboxylic acid compound, with prepared polyacrylamide immobilization ionic liquid capillary monolithic column for spe medium, Ultra Performance Liquid Chromatography is adopted to analyze mineral water.
Mineral water sample preparation: measure mineral water 1 mL, 10 mL are caused with the hydrochloric acid buffer solution dilution of pH 6.3, after the nylon leaching film of 0.45 μm, add the extraction of the PCA of the m-Salicylic acid of 0.02 μ g/mL and 0.01 μ g/mL, P-hydroxybenzoic acid, forulic acid and 2-hydroxyl-3-naphthoic acid standardized solution sample introduction.
Extraction conditions: adopt the capillary monolithic column that example 2 is made, first rinse with water, by the hydrochloric acid buffer solution equilibration capillary integral post of pH 6.3, with flow velocity loading 60 min of 13.3 μ L/min, finally adopt formic acid and the 40% acetonitrile mixing solutions of 10%, with flow velocity wash-out 10 min of 4 μ L/min, collect elutriant, after 5000 rpm high speed centrifugations, analyze with Ultra Performance Liquid Chromatography.
Chromatographiccondition: analytical column is Acclaim
tMrSLC 120 C18 (2.1 × 150 mm, 2.2 μm), the 0.1% first aqueous acid that mobile phase A is; Mobile phase B is pure acetonitrile, gradient: 0-4 min 35%B, 4-4.1 min 35%B-80%B, 4.1-12 min 80%B; Flow velocity 0.3 mL/min, sample introduction 10 μ L, column temperature 30 ° of C, determined wavelength 254 nm.
Fig. 4 color atlas (A) is extraction sample introduction, and color atlas (B) is direct injection.As shown in Fig. 4 (B), mineral water sample, not before Solid-Phase Extraction, does not detect sample signal, lower than the detectability of Ultra Performance Liquid Chromatography.As shown in Figure 4 (A), mineral water sample is after fiber material provided by the invention carries out Solid-Phase Extraction, and each compound obtains good enrichment and is separated, and is not subject to impurity interference, and elution peak 1 is PCA successively; 2 is P-hydroxybenzoic acid; 3 is m-Salicylic acid; 4 is forulic acid; 5 is 2-hydroxyl-3-naphthoic acid, and the rate of recovery is respectively 81.3%, 92.6%, 97.3%, 90.7% and 84.2%, and the relative standard deviation of extractive analysis is less than 10%, illustrates that this Solid-Phase Extraction material is applicable to the analysis of mineral water.
Claims (7)
1. polyacrylamide immobilization ion liquid polymer, it is characterized in that: by glycidyl methacrylate, acrylamide, N, N '-methylene-bisacrylamide and 1-aminopropyl-3-Methylimidazole villaumite are made, and the elementary cell of described polyacrylamide immobilization ion liquid polymer chemical structural formula is:
。
2. the synthetic method of polyacrylamide immobilization ion liquid polymer according to claim 1, is characterized in that comprising the following steps:
The active amino that epoxy group(ing) glycidyl methacrylate contained and 1-aminopropyl-3-Methylimidazole villaumite contain reacts in formamide soln, form the monomer of band ion liquid functional group, add monomeric acrylamide, linking agent N subsequently, N '-methylene-bisacrylamide, under the existence of pore-creating agent polyoxyethylene glycol, then add initiator Diisopropyl azodicarboxylate formation polyacrylamide immobilization ion liquid polymer.
3. synthetic method according to claim 2, the mass ratio that it is characterized in that described glycidyl methacrylate and 1-aminopropyl-3-Methylimidazole villaumite is 1:1 ~ 1:3, described acrylamide and N, N '-methylene-bisacrylamide is 1:1:1 ~ 1:3:3 with the mass ratio of the monomer that band ion liquid functional is rolled into a ball.
4. polyacrylamide immobilization ion liquid polymer according to claim 1 prepares the method for capillary monolithic column, it is characterized in that comprising the following steps:
A, first by quartz capillary successively through persalt, water, sodium hydroxide, water, washed with methanol, and after drying, add after being with the silicone hydroxyl on the methanol solution of γ-2-methyl allyl acyloxypropyl trimethoxysilane and capillary wall to react, dry up stand-by, obtain the kapillary through vinyl modified;
The active amino that b, epoxy group(ing) glycidyl methacrylate contained and 1-aminopropyl-3-Methylimidazole villaumite contain reacts in methane amide, form the monomer of band ion liquid functional group, add monomeric acrylamide, linking agent N subsequently, N '-methylene-bisacrylamide, under the existence of pore-creating agent PEG8000, PEG10000, add initiator Diisopropyl azodicarboxylate, obtain polyacrylamide immobilization ionic liquid solution;
The polyacrylamide immobilization ionic liquid solution prepared is injected into above-mentioned in the kapillary of vinyl modified, polyreaction 20 ~ 24 hours in 65 ~ 80 DEG C of waters bath with thermostatic control, use polymkeric substance in washed with methanol kapillary again, obtain polyacrylamide immobilization ionic liquid capillary monolithic column.
5. polyacrylamide immobilization ion liquid polymer prepares the method for capillary monolithic column according to claim 1, it is characterized in that monomer methacrylic acid glycidyl ester and acrylamide, linking agent N, N '-methylene-bisacrylamide, at pore-creating agent PEG8000, under the existence of PEG10000 and methane amide, add initiator Diisopropyl azodicarboxylate, above-mentioned solution is injected in the quartz capillary of vinyl modified, react in the water bath with thermostatic control of 65 DEG C and generate acrylamide-N in 24 hours, N '-methylene-bisacrylamide-glycidyl methacrylate polymkeric substance, use the unreacted function monomer of washed with methanol and linking agent subsequently, integral post is balanced again with buffered soln, finally, the integral post of above synthesis is slowly rinsed with the ionic liquid 1-aminopropyl-3-Methylimidazole villaumite that buffered soln dissolves, by immobilized in integral post for described ionic liquid 1-aminopropyl-3-Methylimidazole villaumite, obtain polyacrylamide immobilization ionic liquid capillary monolithic column.
6. method according to claim 5, is characterized in that described acrylamide, N, N '-mass ratio between methylene-bisacrylamide and glycidyl methacrylate is 1:1:1 ~ 1:3:3; The mass ratio of described acrylamide-N, N '-methylene-bisacrylamide-glycidyl methacrylate polymkeric substance and 1-aminopropyl-3-Methylimidazole villaumite is 1:1 ~ 1:3.
7. the polyacrylamide immobilization ionic liquid capillary monolithic column that method prepares according to any one of claim 4-6, for the method for Solid-Phase Extraction carboxylic acid compound, is characterized in that comprising the following steps:
Polyacrylamide immobilization ionic liquid capillary monolithic column is first used distilled water flushing, then uses the hydrochloride buffer equilibration capillary integral post of pH 6.3; By carboxylic acid compound with after flow velocity loading 60 ~ 80 min of 10 ~ 13.3 μ L/min, the formic acid of employing 10% and 40% acetonitrile mixing solutions are with flow velocity wash-out 4 ~ 10 min of 4 ~ 10 μ L/min, elutriant will be collected with after 5000 ~ 6000 rpm whizzer high speed centrifugations, carry out stratographic analysis with Ultra Performance Liquid Chromatography instrument.
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| CN104549181B (en) * | 2015-02-06 | 2017-01-11 | 武汉大学 | Preparation method and application of hydrophilic methacrylamide polymer monolithic column |
| CN105148559B (en) * | 2015-09-09 | 2017-02-01 | 宁波工程学院 | Preparation of embedded attapulgite capillary monolithic column and method for using capillary monolithic column for solid phase micro extraction |
| CN105771318A (en) * | 2016-05-05 | 2016-07-20 | 福州大学 | Ionic liquid functionalized organic polymerized monolithic column and preparation method thereof |
| CN107684905B (en) * | 2017-09-20 | 2020-11-03 | 宁波工程学院 | Preparation method of organic-inorganic hybrid monolithic column based on attapulgite and application of organic-inorganic hybrid monolithic column in separation |
| CN115290806B (en) * | 2022-08-01 | 2024-05-28 | 宁波工程学院 | Method for solid phase extraction of biogenic amine by hydrophilic effect and cation exchange |
| CN115332631B (en) * | 2022-10-12 | 2023-03-24 | 常州目天智储科技有限公司 | High-voltage electrolyte and high-voltage lithium ion battery |
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