CN106918653A - A kind of large volume sample injection-non-uniform electric field of glucocorticoid micro emulsion Electrokinetic Chromatography method sweeps collection on-line concentration - Google Patents
A kind of large volume sample injection-non-uniform electric field of glucocorticoid micro emulsion Electrokinetic Chromatography method sweeps collection on-line concentration Download PDFInfo
- Publication number
- CN106918653A CN106918653A CN201511004782.7A CN201511004782A CN106918653A CN 106918653 A CN106918653 A CN 106918653A CN 201511004782 A CN201511004782 A CN 201511004782A CN 106918653 A CN106918653 A CN 106918653A
- Authority
- CN
- China
- Prior art keywords
- sample
- glucocorticoid
- micro emulsion
- electric field
- capillary
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
-
- 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
Abstract
A kind of non-uniform electric field of large volume sample injection one the invention discloses glucocorticoid micro emulsion Electrokinetic Chromatography method sweeps collection on-line concentration, glucocorticoid (metacortandracin is determined using collection (REFS) combination on-line preconcentration is swept using micro emulsion Electrokinetic Chromatography method (MEEKC) and large volume sample injection (LVSI) non-uniform electric field under forward voltage, hydrocortisone, prednisolone, betamethasone), the background buffer containing micro emulsion particle is first full of in the capillary of efficient capillary electrophoresis apparatus, then one section of sample solution is introduced in the way of hydrodynamic injection from arrival end, and apply positive voltage, so as to realize metacortandracin in sample, hydrocortisone, prednisolone, the on-line preconcentration of betamethasone.The present invention has sensitivity higher and more preferable separating degree than conventional MEEKC method of separating and assaying.Experimental result shows that the method consumption sample amount is few, and method economy is quick, realizes the Capillary Electrophoretic Determination of trace glucocorticoid.
Description
Technical field
The invention belongs to technical field of analysis and detection, disclose and sweep technology of the set associative with online gathering and measuring glucocorticoid using micro emulsion Electrokinetic Chromatography method and the non-uniform electric field of large volume sample injection using under forward voltage.
Background technology
Glucocorticoid (glucocorticoids) is steroid hormone of the class by adrenocortical secretion, it is adrenal cortex hormones drug, with important physiologically active, such as anti-inflammatory and antiallergy, reduce capillary wall and membrane passage, reduce inflammatory ooze out wait act on.Some businessmans can play the effect of skin whitening, moisturizing for the addition glucocorticoid in some cosmetics that speculates.But the cosmetics that long-term use contains glucocorticoid can produce the side effects such as facial follicles atrophy, telangiectasis, and human facial skin is caused serious harm.Hence set up the quality control of economic, the quick and highly sensitive detection method for cosmetics of glucocorticoid in cosmetics, it is ensured that using for cosmetics is safe significant.The measure main method of glucocorticoid has high performance liquid chromatography, SPE-liquid chromatography, LC/MS and capillary electrophoresis etc..Wherein high performance liquid chromatography is most common method, but the method needs more complicated sample pretreatment process removal matrix, and liquid chromatograph and liquid-phase chromatographic column are expensive, and the operating cost of instrument is also higher.Capillary electrophoresis detects glucocorticoid, such as China Patent Publication No. CN 102778494, publication date on November 14th, 2012,6 kinds of methods of cortin in entitled a kind of separation determination skin-care cosmetics of innovation and creation, this application case discloses 6 kinds of methods of hormone in a kind of separation determination skin-care cosmetics of knowing clearly.Fluticasone propionate, Triamcinolone acetonide, cortisone acetate, dexamethasone, 6 kinds of methods of hormone of hydrocortisone and metacortandracin in Microemulsions capillary electrophoresis (MEEKC) separation determination cosmetics with ionic liquid and beta-schardinger dextrin as additive.Its weak point is, the relatively low detection for being not suitable for trace glucocorticoid of the method sensitivity.Thus it is necessary to set up that a kind of simple, quick, sensitivity is high and detection method of low cost.
The content of the invention
In order to solve above-mentioned the deficiencies in the prior art part, set associative is swept with online gathering and measuring glucocorticoid (metacortandracin using micro emulsion Electrokinetic Chromatography method and the non-uniform electric field of large volume sample injection using under forward voltage the invention provides one kind, hydrocortisone, prednisolone, betamethasone) technology.Technology consumption sample amount is few, economical quick, has the advantages that sensitivity and more preferable separating degree higher.
The purpose of the present invention is realized by following technical scheme：The background buffer containing micro emulsion particle is first full of in the capillary of efficient capillary electrophoresis apparatus, one section of sample solution is then introduced in the way of hydrodynamic injection from arrival end, and apply positive voltage, so as to realize metacortandracin in sample, hydrocortisone, prednisolone, the on-line preconcentration of betamethasone.The preparation of optimal background buffer in scheme：It is mother liquor using 30mmol/L boric acid-borate buffer solution (pH=8.2), prepare the mass ratio 2.4% (w/w) of SDS, the mass ratio 0.6% (w/w) of normal octane, the background buffer of the mass ratio 6.6% (w/w) of n-butanol.Ultrasonic 20min obtains final product optimal background buffer.Test solution is constituted during the mixed standard solution of hormone is dissolved in into sample substrate；Best sample matrix solution：60mmol/L sodium dihydrogen phosphates, are 3.6 with 0.1mmol/L NaOH and phosphorus acid for adjusting pH.During specific sample determination, after sample is extracted through methyl alcohol, extract solution is dissolved in sample substrate.The sample introduction pressure of hydrodynamic injection is 12.3kPa, and sample injection time is 95s；Capillary two ends insertion background buffer in and apply positive voltage, separation voltage is 9.6kV.
Brief description of the drawings
Fig. 1 is metacortandracin for micro emulsion Electrokinetic Chromatography Fig. 1 of standard items mixed liquor, and 2 is hydrocortisone, and 3 is prednisolone, and 4 is betamethasone
Fig. 2 is the large volume sample injection of the Electrokinetic Chromatography method of the mixed liquor of standard items --- non-uniform electric field sweeps that to integrate chromatogram 1 be metacortandracin, and 2 is hydrocortisone, and 3 is prednisolone, and 4 is betamethasone
Specific embodiment
Embodiment 1：
(1) instrument：TH-3100 efficient capillary electrophoresis apparatus；It is split tunnel to use non-coating quartz capillary (total length is 65cm, effective length 50cm, column internal diameter 50um).
(2) preparation of hormone standard liquid：Metacortandracin accurately is weighed, hydrocortisone, prednisolone, each 20.0mg of betamethasone is placed in 10.00mL volumetric flasks, plus after methyl alcohol ultrasonic dissolution, be cooled to room temperature, then add methanol dilution to scale, obtained final product after shaking up.4 DEG C of preservations of lucifuge.Standard items mixed liquor to be measured is made, the titer of various concentrations is diluted to when using as needed.
(3) preparation of background buffer：It is mother liquor using 30mmol/L boric acid-borate buffer solution (pH=8.2), prepare the mass ratio 2.4% (w/w) of SDS, the mass ratio 0.6% (w/w) of normal octane, the background buffer of the mass ratio 6.6% (w/w) of n-butanol.Ultrasonic 20min obtains final product optimal background buffer.
(4) prepared by sample solution：Cosmetic sample 1.0g accurately is weighed in 50mL centrifuge tubes, 15mL methyl alcohol is added thereto to, 5min, ultrasonic 20min is fully vibrated, 10mL n-hexanes are added, 10min is vibrated, 8min is centrifuged in 8000r/min, discard upper strata n-hexane layer；Add 10mL n-hexanes and repeat aforesaid operations, lower layer methanol solution is concentrated under reduced pressure into about 1mL at 45 DEG C.10mL is settled to sample substrate solution, sample solution is obtained final product.
(5) chromatographic condition：Microemulsion is running buffer with step 3, using hydrodynamic injection, sample introduction pressure 12.3kPa, sample injection time 95s, and 20 DEG C of running temperature, Detection wavelength is 230nm.
(6) enrichment times：Metacortandracin, hydrocortisone, prednisolone, the on-line preconcentration multiple of betamethasone can reach 853,893,933 and 925 times respectively.
Claims (4)
1. the background buffer containing micro emulsion particle is first full of in the capillary of efficient capillary electrophoresis apparatus, then from arrival end pressing
The mode of power sample introduction introduces one section of test solution, and applies positive voltage, and so as to realize metacortandracin in detection object, hydrocortisone sprinkles
Ni Songlong, the on-line preconcentration of betamethasone.
2. method according to claim 1, it is characterized in that the preparation of optimal background buffer：Using 30mmol/L boric acid-
Borate buffer solution (pH=8.2) be mother liquor, prepare SDS mass ratio 2.4% (w/w), the mass ratio 0.6% (w/w) of normal octane,
The background buffer of the mass ratio 6.6% (w/w) of n-butanol, ultrasonic 20min obtains final product optimal background buffer.
3. method according to claim 1, it is characterized in that constituting examination during the mixed standard solution of hormone is dissolved in into sample substrate
Liquid, best sample matrix solution：60mmol/L sodium dihydrogen phosphates, with 0.1mmol/L NaOH and phosphorus acid for adjusting pH
It is 3.6, during specific sample determination, after sample is extracted through methyl alcohol, extract solution is dissolved in sample substrate.
4. method according to claim 1, it is characterized in that the sample introduction pressure of hydrodynamic injection is 12.3kPa, sample injection time is 95
s；Capillary two ends insertion background buffer in and apply positive voltage, separation voltage is 9.6kV.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511004782.7A CN106918653A (en) | 2015-12-28 | 2015-12-28 | A kind of large volume sample injection-non-uniform electric field of glucocorticoid micro emulsion Electrokinetic Chromatography method sweeps collection on-line concentration |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511004782.7A CN106918653A (en) | 2015-12-28 | 2015-12-28 | A kind of large volume sample injection-non-uniform electric field of glucocorticoid micro emulsion Electrokinetic Chromatography method sweeps collection on-line concentration |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106918653A true CN106918653A (en) | 2017-07-04 |
Family
ID=59455302
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201511004782.7A Pending CN106918653A (en) | 2015-12-28 | 2015-12-28 | A kind of large volume sample injection-non-uniform electric field of glucocorticoid micro emulsion Electrokinetic Chromatography method sweeps collection on-line concentration |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106918653A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007110656A2 (en) * | 2006-03-29 | 2007-10-04 | Medigen Biotechnology Corporation | Methods and apparatus for genotyping |
| CN102706971A (en) * | 2010-12-09 | 2012-10-03 | 江南大学 | A method for analysis of corticosteroids in cosmetics utilizing reverse microemulsion electrokinetic chromatography by taking an ionic liquid as an additive |
| CN102778494A (en) * | 2012-06-01 | 2012-11-14 | 江南大学 | Method for separating and detecting six cortical hormones in skin-care cosmetic |
-
2015
- 2015-12-28 CN CN201511004782.7A patent/CN106918653A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007110656A2 (en) * | 2006-03-29 | 2007-10-04 | Medigen Biotechnology Corporation | Methods and apparatus for genotyping |
| CN102706971A (en) * | 2010-12-09 | 2012-10-03 | 江南大学 | A method for analysis of corticosteroids in cosmetics utilizing reverse microemulsion electrokinetic chromatography by taking an ionic liquid as an additive |
| CN102778494A (en) * | 2012-06-01 | 2012-11-14 | 江南大学 | Method for separating and detecting six cortical hormones in skin-care cosmetic |
Non-Patent Citations (3)
| Title |
|---|
| CHIEN-YUAN KUO等: "Micellar electrokinetic chromatography for simultaneous determination of six corticosteroids in commercial pharmaceuticals", 《J. SEP. SCI.》 * |
| 孙雪婷等: "微乳毛细管电色谱电动进样-场放大堆积法检测化妆品中糖皮质激素", 《分析化学》 * |
| 盛建伟: "微乳毛细管电动色谱微乳微结构的研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Brachet et al. | Optimisation of accelerated solvent extraction of cocaine and benzoylecgonine from coca leaves | |
| Qi et al. | Rapid and sensitive determination of anthraquinones in Chinese herb using 1-butyl-3-methylimidazolium-based ionic liquid with β-cyclodextrin as modifier in capillary zone electrophoresis | |
| Shen et al. | Determination of tobacco alkaloids by gas chromatography–mass spectrometry using cloud point extraction as a preconcentration step | |
| CN104807920B (en) | A kind of test kit is using the application in 10 steroids hormones in high performance liquid chromatography tandem mass spectrum technology for detection serum | |
| CN105181784B (en) | A kind of method of 40 kinds of violated antibiotic in rapid screening cosmetics | |
| CN104297410B (en) | A kind of Liquid Chromatography-Tandem Mass Spectrometry detects the method for abscisic acid and jasmonic in fresh tobacco leaves | |
| CN105047519B (en) | In-situ spraying ionization device | |
| He et al. | An online field-amplification sample stacking method for the determination of β2-agonists in human urine by CE-ESI/MS | |
| CN102243220A (en) | Nanospray capillary high pressure liquid chromatographic column and its preparation method | |
| Zhang et al. | On-line sample concentration and determination of cationic alkaloids in human plasma by micelle to solvent stacking in capillary zone electrophoresis | |
| CN102778494A (en) | Method for separating and detecting six cortical hormones in skin-care cosmetic | |
| Chen et al. | Determination of glycosides and sugars in Moutan Cortex by capillary electrophoresis with electrochemical detection | |
| CN204925031U (en) | Open -type ionizationoun atomizer | |
| Wang et al. | Separation and on-line concentration of saponins from Panax notoginseng by micellar electrokinetic chromatography | |
| CN102944617A (en) | Method for determining sex hormone content in cosmetic | |
| Gao et al. | Sensitive determination of four β2-agonists in pig feed by capillary electrophoresis using on-line sample preconcentration with contactless conductivity detection | |
| CN103792270B (en) | A kind of extraction of the parathion-methyl based on N-octylpyridinium hexafluorophosphoric acid salt electrode and detection method | |
| CN102706971A (en) | A method for analysis of corticosteroids in cosmetics utilizing reverse microemulsion electrokinetic chromatography by taking an ionic liquid as an additive | |
| CN102680617A (en) | Method for detecting adrenal hormone content | |
| Ding et al. | Separation and determination of four ganoderic acids from dried fermentation mycelia powder of Ganoderma lucidum by capillary zone electrophoresis | |
| Gao et al. | Sensitive determination of verticine and verticinone in Bulbus Fritillariae by ionic liquid assisted capillary electrophoresis–electrochemiluminescence system | |
| CN103954705A (en) | Method for measuring content of allantoin contained in Chinese traditional medicine rhizoma dioscoreae and rhizoma dioscoreae-containing preparation | |
| CN106918653A (en) | A kind of large volume sample injection-non-uniform electric field of glucocorticoid micro emulsion Electrokinetic Chromatography method sweeps collection on-line concentration | |
| Lin et al. | Comparison between micellar electrokinetic chromatography and HPLC for the determination of Betamethasone Dipropionate, Clotrimazole and their related substances | |
| Liu et al. | Separation and determination of alpinetin and cardamonin in Alpinia katsumadai Hayata by flow injection–micellar electrokinetic chromatography |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170704 |