CN107478731A - The pre-treating method of parabens preservative in a kind of detection cosmetics - Google Patents
The pre-treating method of parabens preservative in a kind of detection cosmetics Download PDFInfo
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- CN107478731A CN107478731A CN201610397207.6A CN201610397207A CN107478731A CN 107478731 A CN107478731 A CN 107478731A CN 201610397207 A CN201610397207 A CN 201610397207A CN 107478731 A CN107478731 A CN 107478731A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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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
- G01N30/08—Preparation using an enricher
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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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid 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
- G01N30/48—Sorbent materials therefor
- G01N2030/484—Solid sorbents
Abstract
The invention belongs to analytical chemistry field, is related to a kind of pre-treating method for detecting parabens preservative in cosmetics.The inventive method it include, the mesoporous magnetic graphene composite of synthesis of phenyl modification, graphenic surface synthesis ferroso-ferric oxide microballoon after acidified processing, again gained magnetic graphene Surface coating mesoporous silicon and simultaneously mesoporous inwall modification on phenyl, obtain the mesoporous magnetic graphene composite of phenyl modification, it has huge specific surface area, uniform pore-size distribution and good magnetic responsiveness, while its duct inwall has modified phenyl and has optionally been enriched with molecular structure the nipagin esters molecule containing phenyl ring；This method can carry out enrichment rapidly and efficiently to cosmetics small molecular parabens preservative, the problems such as overcoming conventional method analysis difficulty, take.
Description
Technical field
The invention belongs to analytical chemistry field, it is related to the pre-treating method of Determination of Preservatives in Cosmetics, and in particular to one kind is based on
The pre-treating method of parabens preservative in the mesoporous magnetic graphene composite enrichment detection cosmetics of phenyl modification.
Background technology
Prior art discloses cosmetics as daily living article, its safety in utilization is increasingly by the weight of people
Depending on.Parabens preservative is the most widely used a kind of preservative in presently commercially available cosmetics, but existing document report
Road claims the intake of excessive parabens preservative certain correlation may be presented with human breast cancer morbidity.Consumed to ensure
Person's health, every country launch respectively addition of the relevant regulations to parabens preservative in cosmetics and have carried out limitation control
System.
The cosmetics commonly used in daily life include toner, emulsion, face cream etc., and it forms complexity, and quality is sticky, has
Serious matrix effect and effective enrichment method etc. is lacked to small molecule parabens preservative so that relevant research runs into
Heavy bottleneck.For such complex sample, traditional pre-treating method mainly has liquid-liquid extraction or SPE etc., but this
A little methods often there is it is time-consuming, largely using organic solvent, lack the shortcomings of selectivity to target molecule.
Restrict access material SPE（RAM-SPE）It is a kind of new Sample Pretreatment Technique developed in recent years.Limit into Jie
Matter solid phase extraction adsorbentses have the volume exclusion function for macromolecular and the extraction function for small molecule analyte concurrently simultaneously,
This kind of adsorbent has hydrophilic extexine, and the aperture of specific dimensions can be obtained by controlling synthesis step.Meanwhile
Isolation technics based on magnetic material（MSPE）And a hot fields of recent domestic research, the technology is with a kind of magnetic
Property or magnetizable material are as adsorbent, and in extraction process, magnetic adsorbent is dispersed directly into sample solution, by mesh
Mark analyte is adsorbed onto scattered magnetic adsorbent surface, then makes target analytes and sample substrate in the presence of external magnetic field
Separation.
The sample substrate run into Determination of Preservatives in Cosmetics detection work based on prior art is excessively complicated, analysis time
Long, Extraction and enrichment process lacks the problems such as selective, and present inventor intends providing a kind of preceding place of Determination of Preservatives in Cosmetics
Reason method, and in particular to one kind is based on nipagin esters in the mesoporous magnetic graphene composite enrichment detection cosmetics of phenyl modification
The pre-treating method of class preservative.
The content of the invention
The purpose of the present invention is excessively complicated to solve the sample substrate of Determination of Preservatives in Cosmetics detection in the prior art, is divided
Time length is analysed, Extraction and enrichment process lacks the problems such as selective, there is provided a kind of pre-treating method of Determination of Preservatives in Cosmetics, specifically
It is related to parabens preservative in a kind of mesoporous magnetic graphene composite enrichment detection cosmetics based on phenyl modification
Pre-treating method.This method is reached by the technical step of uniqueness quickly excludes macromolecular interference in sample in the short time, and leads to
π-π the interactions crossed between the phenyl functional group of material and nipagin esters molecule carry out the richness of selectivity to nipagin esters
Collection.
The present invention is combined RAM-SPE technologies with MSPE technologies, and synthesis of phenyl modifies mesoporous magnetic graphene composite
And there is huge specific surface area, uniform pore-size distribution for the detection of parabens preservative in cosmetics, the material
And good magnetic responsiveness, and modified in mesoporous inwall with phenyl functional group.Answered with the mesoporous magnetic graphene of phenyl modification
When condensation material is handled the cosmetic sample of complexity, the small molecule nipagin esters containing phenyl ring can enter material in structure
In duct and by being resided in the π-π of modification group interaction in duct, while polysaccharide in sample substrate, protein etc.
By exclusion outside duct, having adsorbed the material of target molecule can be separated rapidly after interaction with the target molecules macromolecular in externally-applied magnetic field, then be fitted
When eluting solvent target molecule is eluted.The present invention can enter to the small molecule nipagin esters in the cosmetic base of complexity
Row is rapidly and effectively enriched with, so as to overcome analysis difficulty, it is time-consuming the problems such as, also opened for the application of composite nano materials
New approach.
Specifically, in a kind of detection cosmetics of the invention parabens preservative pre-treating method, it includes
Step：
1）The mesoporous magnetic graphene composite of synthesis of phenyl modification：
（1）Graphene uniform is dispersed in concentrated nitric acid and carries out acidification, cleaning, vacuum drying；
（2）Will（1）Resulting acidifying graphite alkene and anhydrous sodium acetate, PEG-20000, trisodium citrate, six trichloride hydrates
The common pyroreaction of iron makes the modification of ferroso-ferric oxide microballoon in graphenic surface.With washes of absolute alcohol, vacuum drying after reaction；
（3）Will（2）Gained magnetic graphene is dispersed in water together with cetyl trimethylammonium bromide, regulation pH to weak base
Property, the mixture of tetraethyl orthosilicate and ethanol is added under heating stirring, adds tetraethyl orthosilicate and the ethoxy of phenyl base three afterwards
The mixture of base silane, continue after reacting 6-18 hours, clean up, the mesoporous magnetic graphene composite wood of obtained phenyl modification
Material.
2）Parabens preservative in cosmetics is carried out using the mesoporous magnetic graphene composite of phenyl modification
Enrichment, separation, extraction and analysis；
（1）The mesoporous magnetic graphene composite of appropriate phenyl modification is taken, is added in 0.1-5mL cosmetic samples and fully mixed
Close, parabens preservative is entered inside material duct, pass through π-π interaction selectivity with phenyl functional group in duct
Ground is combined and resided therein；
（2）Material is separated and collected into material, supernatant discarding by applying an external magnetic field；
（3）0.1-1 mL eluents are added into material and are sufficiently mixed 1-10 minutes, nipagin esters are mesoporous from phenyl modification
It is eluted out inside the duct of magnetic graphene composite, is detected after eluent filtering into liquid chromatogram.
The present invention is entered in the mesoporous magnetic graphene composite of phenyl modification parabens preservative in cosmetics
Row enrichment, separation, extraction and analysis, have the following advantages that：
（1）Synthesized the mesoporous magnetic graphene composite of phenyl modification has huge as magnetic ram-SPE adsorbents, the material
Big specific surface area（200-400 cm2 g-1）, uniform pore-size distribution（2-4 nm）And good magnetic responsiveness.Its inwall
The parabens preservative containing phenyl ring in molecular structure can be optionally enriched with by having modified phenyl.
（2）Using the mesoporous magnetic graphene composite of phenyl modification, parabens preservative carries out richness in cosmetics
Collection, separation, extraction and analysis analysis process are quick, simple to operate.Excluded by the mesoporous step of volume exclusion effect one big in matrix
The interference of molecule.
（3）This method many experiments verify that accuracy rate is high, and detection limit is low, and detection range is wide, hence it is evident that locates before shortening sample
Manage the time.This method disclosure satisfy that the international and domestic testing requirements detected to parabens preservative in cosmetics.
Brief description of the drawings
Fig. 1 is the technology of the present invention flow chart.
Fig. 2 is the synthetic route chart of the mesoporous magnetic graphene composite of phenyl modification.
Fig. 3 is the transmission electron microscope photo of the mesoporous magnetic graphene composite of phenyl modification in embodiment.
Embodiment
The following examples are the further explanations to the present invention, rather than limit the scope of the present invention.
Embodiment 1. is applied to the oxybenzene first in enrichment toner using the mesoporous magnetic graphene composite of phenyl modification
Ester, Nipasol：
（1）The synthesis of the mesoporous magnetic graphene composite of phenyl modification：
1）0.30 g graphene platelets are distributed in 100 mL concentrated nitric acids, 60oStirred 7 hours under C, the stone after treating
Black alkene with deionized water clean to pH in neutrality, 50oCollected after C vacuum drying stand-by；
2）Graphene, 1.8 g anhydrous sodium acetates, 1.0 g added in 100 mL reactors after 150 mg acidifications
PEG-20000,150 mg trisodium citrates, 150 mg Iron(III) chloride hexahydrates, 40 mL ethylene glycol, it is small to be ultrasonically treated 2
When, 200 DEG C reaction 12 h after absolute ethyl alcohol wash 5 times, 50oCollected after C vacuum drying stand-by；
3）75 mg magnetic graphenes, 750 mg cetyl trimethylammonium bromides, 75 mL are added in 1L round-bottomed flasks to go
Ionized water adds 600 mL deionized waters and the mol L of 75 mL 0.01 after being ultrasonically treated 30 min-1NaOH solution continues ultrasound 5
60 DEG C of stirred in water bath react 30 min after min, and 3.75 mL tetraethyl orthosilicates/absolute ethyl alcohol (volume ratio is slowly added dropwise:
1/4) solution, continue that 150 μ L tetraethyl orthosilicates and 100 μ L phenyltriethoxy silanes are slowly added dropwise after reacting 30 min
Alkane, 60 DEG C of stirred in water bath are reacted 12 hours；
4）Product to be collected to separate in magnetic field, deionized water is washed 3 times, and absolute ethyl alcohol washs 3 times, and redisperse is in acetone,
In 50oC flows back to remove cetyl trimethylammonium bromide.The obtained mesoporous magnetic graphene composite of phenyl modification is 50
DEG C vacuum drying, in case use；
（2）The mesoporous magnetic graphene composite of phenyl modification is applied to methyl hydroxybenzoate, Nipasol in enrichment toner：
1) sample treatment：
In 4 mL EP pipes, add the mesoporous magnetic graphene composite of 16 mg phenyl modifications and 2 mL toners, it is ultrasonic at
Reason makes target molecule fully be combined with material in 2 minutes, and the magnetic composite is isolated in after-applied external magnetic field, and discards
Clearly, 200 μ L acetonitriles are added into material as eluent, 4 minutes after-applied external magnetic fields is ultrasonically treated and isolates condensation material
And eluent is collected, 200 μ L acetonitriles are added into material, elutes and collects with method, merges eluent twice, is carried out after filtering
High-efficient liquid phase analysis；
2) chromatographic condition：
Chromatographic column：TSKgel ODS-100V C18 column (150 mm × 4.6 mm, 5μm;TOSOH, Japan)；
Mobile phase：A：Acetonitrile solution, B：0.01 mol L-1Ammonium acetate solution, A:B（v:v）=50:50；
Sample size：10 μL；Flow velocity：1 mL min-1；Column temperature：30 ℃；Detection wavelength：254 nm；
Run time：8 min.
Testing result shows that this method is using the mesoporous magnetic graphene composite of phenyl modification as magnetic ram-SPE
Adsorbent, the material have huge specific surface area, uniform pore-size distribution and good magnetic responsiveness, and its inwall is modified
Phenyl can optionally be enriched with the parabens preservative containing phenyl ring in molecular structure；Enrichment, separation, extraction and analysis mistake
Journey is quick, simple to operate；The interference of macromolecular in matrix is excluded by the mesoporous step of volume exclusion effect one, and accuracy rate is high,
Detection limit is low, and detection range is wide, hence it is evident that shortens time for sample pretreatment.
Claims (9)
1. a kind of pre-treating method for detecting parabens preservative in cosmetics, it is characterised in that it includes step：
1）The mesoporous magnetic graphene composite of synthesis of phenyl modification：
2）Parabens preservative in cosmetics is enriched with using the mesoporous magnetic graphene composite of phenyl modification.
2. the pre-treating method as described in claim 1, it is characterised in that described step 1）In, by graphene dispersion dense
After carrying out acidification in nitric acid, magnetic is obtained with ferroso-ferric oxide microballoon by reacting modification on the acidifying graphite alkene surface of gained
Property graphene, then the coating mesoporous silicon of its previous step and simultaneously mesoporous inwall modify with functional group phenyl.
3. the pre-treating method as described in claim 1, it is characterised in that described step 2）In, add in cosmetic sample
Enter the composite, mixing makes target molecule enter material duct inwall and adsorbed thereon, and material is isolated under magnetic fields
Material, supernatant discarding, then detected into material after addition elution target molecule into chromatographic system analysis.
4. pre-treating method according to claim 1, it is characterised in that in methods described, 0.1-0.5 g graphenes is equal
Even be dispersed in 50-200 mL concentrated nitric acids carries out acidification in 30-80 DEG C of heating stirring reaction.
5. pre-treating method according to claim 1, it is characterised in that in methods described, take the acidifying graphite alkene of gained
0.1-0.5 g and 0.5-5 g anhydrous sodium acetates, 0.5-5 g PEG-20000,0.1-0.5 g trisodium citrates, 0.1-0.5 g
Iron(III) chloride hexahydrate reacts 6-24 h at 100-300 DEG C jointly makes ferroso-ferric oxide microballoon modify in graphenic surface, is made
Magnetic graphene.
6. pre-treating method according to claim 1, it is characterised in that in methods described, take 20-200 mg magnetic graphites
Alkene is dispersed in water with 0.1-2.0 g cetyl trimethylammonium bromides, regulation pH to alkalescent, under 30-80 DEG C of heating stirring
The mixture of 1.0-6.0 mL tetraethyl orthosilicates and ethanol is added, volume ratio 0.2-10.0, is adding 0.1-3.0 mL afterwards just
The mixture of silester and phenyl ethyl triethoxy silicane alkane, volume ratio 0.2-10.0, continue heating stirring reaction 6-18 hours.
7. pre-treating method according to claim 1, it is characterised in that in methods described, into 0.5-5 mL cosmetics
Add the mesoporous magnetic graphene composite of 1-100 mg phenyl modifications.
8. pre-treating method according to claim 1, it is characterised in that in methods described, added into cosmetics compound
After material, ultrasound or vortex mixed 0.1-10 minutes.
9. pre-treating method according to claim 1, it is characterised in that in methods described, to having adsorbed target molecule
Material, by adding 0.1-10 mL eluting solvents and ultrasound or vortex mixed 0.1-15 minutes are eluted.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108693262A (en) * | 2018-04-13 | 2018-10-23 | 佛山市梅雨科技有限公司 | A kind of assay method of Determination of Preservatives in Cosmetics |
| CN111474248A (en) * | 2019-12-19 | 2020-07-31 | 沈阳药科大学 | Method for determining four preservatives in cosmetics |
| CN112337446A (en) * | 2020-10-19 | 2021-02-09 | 南通大学 | Small ball capable of quickly removing preservative as well as preparation method and application thereof |
| CN113358793A (en) * | 2021-06-24 | 2021-09-07 | 北海市食品药品检验所 | Method for detecting content of preservative in cosmetics |
| CN114235983A (en) * | 2021-11-23 | 2022-03-25 | 鲁东大学 | Method for removing and detecting nipagin ester based on covalent organic framework adsorbent |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108693262A (en) * | 2018-04-13 | 2018-10-23 | 佛山市梅雨科技有限公司 | A kind of assay method of Determination of Preservatives in Cosmetics |
| CN111474248A (en) * | 2019-12-19 | 2020-07-31 | 沈阳药科大学 | Method for determining four preservatives in cosmetics |
| CN112337446A (en) * | 2020-10-19 | 2021-02-09 | 南通大学 | Small ball capable of quickly removing preservative as well as preparation method and application thereof |
| CN112337446B (en) * | 2020-10-19 | 2023-10-31 | 南通大学 | Pellet capable of rapidly removing preservative as well as preparation method and application thereof |
| CN113358793A (en) * | 2021-06-24 | 2021-09-07 | 北海市食品药品检验所 | Method for detecting content of preservative in cosmetics |
| CN114235983A (en) * | 2021-11-23 | 2022-03-25 | 鲁东大学 | Method for removing and detecting nipagin ester based on covalent organic framework adsorbent |
| CN114235983B (en) * | 2021-11-23 | 2023-10-10 | 鲁东大学 | Method for removing and detecting nipagin ester based on covalent organic framework adsorbent |
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