CN108007926A - The quick determination method of glucocorticoid and application in a kind of cosmetics - Google Patents
The quick determination method of glucocorticoid and application in a kind of cosmetics Download PDFInfo
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- CN108007926A CN108007926A CN201711247742.4A CN201711247742A CN108007926A CN 108007926 A CN108007926 A CN 108007926A CN 201711247742 A CN201711247742 A CN 201711247742A CN 108007926 A CN108007926 A CN 108007926A
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- glucocorticoid
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- 239000003862 glucocorticoid Substances 0.000 title claims abstract description 48
- 239000002537 cosmetic Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 30
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 57
- 238000001514 detection method Methods 0.000 claims abstract description 17
- FSVCQIDHPKZJSO-UHFFFAOYSA-L nitro blue tetrazolium dichloride Chemical compound [Cl-].[Cl-].COC1=CC(C=2C=C(OC)C(=CC=2)[N+]=2N(N=C(N=2)C=2C=CC=CC=2)C=2C=CC(=CC=2)[N+]([O-])=O)=CC=C1[N+]1=NC(C=2C=CC=CC=2)=NN1C1=CC=C([N+]([O-])=O)C=C1 FSVCQIDHPKZJSO-UHFFFAOYSA-L 0.000 claims abstract description 13
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 9
- 238000000605 extraction Methods 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 125000000524 functional group Chemical group 0.000 abstract description 2
- 229940088597 hormone Drugs 0.000 description 6
- 239000005556 hormone Substances 0.000 description 6
- 230000008901 benefit Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 230000006870 function Effects 0.000 description 3
- 238000007689 inspection Methods 0.000 description 3
- 201000004624 Dermatitis Diseases 0.000 description 2
- 208000027418 Wounds and injury Diseases 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 230000001580 bacterial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 230000009849 deactivation Effects 0.000 description 2
- 229960003957 dexamethasone Drugs 0.000 description 2
- UREBDLICKHMUKA-CXSFZGCWSA-N dexamethasone Chemical compound C1CC2=CC(=O)C=C[C@]2(C)[C@]2(F)[C@@H]1[C@@H]1C[C@@H](C)[C@@](C(=O)CO)(O)[C@@]1(C)C[C@@H]2O UREBDLICKHMUKA-CXSFZGCWSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000001815 facial effect Effects 0.000 description 2
- JYGXADMDTFJGBT-VWUMJDOOSA-N hydrocortisone Chemical compound O=C1CC[C@]2(C)[C@H]3[C@@H](O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 JYGXADMDTFJGBT-VWUMJDOOSA-N 0.000 description 2
- 208000014674 injury Diseases 0.000 description 2
- 229960005205 prednisolone Drugs 0.000 description 2
- OIGNJSKKLXVSLS-VWUMJDOOSA-N prednisolone Chemical compound O=C1C=C[C@]2(C)[C@H]3[C@@H](O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 OIGNJSKKLXVSLS-VWUMJDOOSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229940037128 systemic glucocorticoids Drugs 0.000 description 2
- FUFLCEKSBBHCMO-UHFFFAOYSA-N 11-dehydrocorticosterone Natural products O=C1CCC2(C)C3C(=O)CC(C)(C(CC4)C(=O)CO)C4C3CCC2=C1 FUFLCEKSBBHCMO-UHFFFAOYSA-N 0.000 description 1
- VHRSUDSXCMQTMA-PJHHCJLFSA-N 6alpha-methylprednisolone Chemical compound C([C@@]12C)=CC(=O)C=C1[C@@H](C)C[C@@H]1[C@@H]2[C@@H](O)C[C@]2(C)[C@@](O)(C(=O)CO)CC[C@H]21 VHRSUDSXCMQTMA-PJHHCJLFSA-N 0.000 description 1
- 206010006187 Breast cancer Diseases 0.000 description 1
- 208000026310 Breast neoplasm Diseases 0.000 description 1
- MFYSYFVPBJMHGN-ZPOLXVRWSA-N Cortisone Chemical compound O=C1CC[C@]2(C)[C@H]3C(=O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 MFYSYFVPBJMHGN-ZPOLXVRWSA-N 0.000 description 1
- MFYSYFVPBJMHGN-UHFFFAOYSA-N Cortisone Natural products O=C1CCC2(C)C3C(=O)CC(C)(C(CC4)(O)C(=O)CO)C4C3CCC2=C1 MFYSYFVPBJMHGN-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- 241001062009 Indigofera Species 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 208000037093 Menstruation Disturbances Diseases 0.000 description 1
- 206010027339 Menstruation irregular Diseases 0.000 description 1
- -1 Methyllprednisolone Chemical compound 0.000 description 1
- 208000003251 Pruritus Diseases 0.000 description 1
- 241000700647 Variola virus Species 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- MOFINMJRLYEONQ-UHFFFAOYSA-N [N].C=1C=CNC=1 Chemical class [N].C=1C=CNC=1 MOFINMJRLYEONQ-UHFFFAOYSA-N 0.000 description 1
- 230000001780 adrenocortical effect Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 208000010668 atopic eczema Diseases 0.000 description 1
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
- 229960002537 betamethasone Drugs 0.000 description 1
- UREBDLICKHMUKA-DVTGEIKXSA-N betamethasone Chemical compound C1CC2=CC(=O)C=C[C@]2(C)[C@]2(F)[C@@H]1[C@@H]1C[C@H](C)[C@@](C(=O)CO)(O)[C@@]1(C)C[C@@H]2O UREBDLICKHMUKA-DVTGEIKXSA-N 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 210000000481 breast Anatomy 0.000 description 1
- 210000000038 chest Anatomy 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 125000000017 cortisol group Chemical group 0.000 description 1
- 229960004544 cortisone Drugs 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 208000030172 endocrine system disease Diseases 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000003163 gonadal steroid hormone Substances 0.000 description 1
- 230000003779 hair growth Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229960000890 hydrocortisone Drugs 0.000 description 1
- 230000001900 immune effect Effects 0.000 description 1
- 230000028993 immune response Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 201000010260 leiomyoma Diseases 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000004895 liquid chromatography mass spectrometry Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004630 mental health Effects 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 229960004584 methylprednisolone Drugs 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 229960004618 prednisone Drugs 0.000 description 1
- XOFYZVNMUHMLCC-ZPOLXVRWSA-N prednisone Chemical compound O=C1C=C[C@]2(C)[C@H]3C(=O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 XOFYZVNMUHMLCC-ZPOLXVRWSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000008591 skin barrier function Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000003270 steroid hormone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- GFNANZIMVAIWHM-OBYCQNJPSA-N triamcinolone Chemical compound O=C1C=C[C@]2(C)[C@@]3(F)[C@@H](O)C[C@](C)([C@@]([C@H](O)C4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 GFNANZIMVAIWHM-OBYCQNJPSA-N 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
Quick determination method and application the invention discloses glucocorticoid in a kind of cosmetics, including the configuration of sample extraction, detection reagent, detection;By the functional group of nitroblue tetrazolium chloride strong basicity methanol solution and glucocorticoid specific reaction occurs for the present invention, produce color, can quickly detect in sample whether contain glucocorticoid with sxemiquantitative, and substantial amounts of expense and large-scale equipment need not be spent, this method detection is quick, cheap, convenient, safe.
Description
Technical field
The invention belongs to cosmetics to detect detection technique field, more specifically, more particularly to a kind of cosmetics sugar cortex
The quick determination method of hormone, meanwhile, the invention further relates to a kind of application of the quick determination method of cosmetics glucocorticoid.
Background technology
Sex hormone is added in cosmetics can quickly realize the functions such as hair growth, chest enlarge, U.S. breast, whitening, but long-time service
The incidence that women suffers from breast cancer and fibroid can be improved, can also cause irregular menstruation, pigementation, thinning of skin etc. no
Good reaction.Glucocorticoid has the function that adjusting sugar, fat, the biosynthesis and metabolism of protein, and short-period used can make skin
The smooth fine and smooth, skin of skin is ruddy glossy in vain, plays beautification function, but the meeting of long-time service causes body endocrine system disorder,
And cause a series of side effects, such as hypertension, diabetes, variability eczema-like dermatitis etc., there are many people's care at present
Hormone face is also that main cause has at 3 points:First, glucocorticoid anti-inflammatory but not antibacterial, that is to say, that although of short duration inflammation disappears
Lose, but be that skin is benumbed in fact, cause the bacterial virus in the external world can arbitrarily to enter, skin bacterial flora imbalance is occurred,
This be also why long-time service and mad quick-fried small pox after disabling;Second, it can also suppress immune response, long-time service
The immunologic balance of skin can be destroyed so that after deactivation, the immune recovery of human body, the bounce-back of madness occurs, cause serious mistake
Quick state;Third, it can also reduce the synthesis of protein, so as to destroy skin barrier, capillary is stimulated so that after deactivation, go out
The problems such as existing skin is excessively thin, dry, itch, red blood silk.
It can be seen from the above that illegal addition disabling hormone in cosmetics, can make us produce dependence to this product, cause long-term
Our health can be caused serious injury after use, or even destroy the future of a people indirectly.
In recent years, the inspection for cosmetics is also more and more concerned, and especially glucocorticoid and detection is interesting,
There is relevant report both at home and abroad.Glucocorticoid is a kind of steroid hormone by adrenocortical secretion, also can be by chemical method
It is artificial synthesized.What is used at present has:Cortisone, hydrocortisone, prednisone, prednisolone, methylprednisolone, Methyllprednisolone, fluorine
Prednisolone, fluoxyprednisolone, betamethasone, dexamethasone etc..Glucocorticoid can be made up of the method for chemical synthesis, such as
Dexamethasone is the new hormone after being chemically modified to hydrocortisone structure, so different glucocorticoids can lead to
This mode is crossed to obtain, between be also to have the common part that is connected.The detection method of glucocorticoid generally uses liquid phase color at present
Spectrometry and liquid chromatography mass spectrometric method, these method detection cycles length, is all to rely on large-scale instrument and equipment.For consumers, machine is sent
Structure detects, and relatively expensive check fee and cumbersome process are difficult to receive, so quick detect for fright bootleg business, OK
Political affairs law enforcement, consumer's self-test are very necessary.For this reason, it is proposed that a kind of quick determination method of glucocorticoid, with solution
State the problem of being mentioned in background technology.
The content of the invention
It is an object of the invention to provide a kind of quick determination method of glucocorticoid in cosmetics, by chlorination nitro four
Specific reaction occurs for the functional group of nitrogen azoles indigo plant strong basicity methanol solution and glucocorticoid, produces color, can be fast with sxemiquantitative
Speed detects whether contain glucocorticoid in sample, and need not spend substantial amounts of expense and large-scale equipment, and this method detection is fast
It is fast, cheap, convenient, safe.
To achieve the above object, the present invention provides following technical solution:
The quick determination method of glucocorticoid, includes the following steps in a kind of cosmetics:
1) glucocorticoid in cosmetics is extracted with methanol;
2) aqueous slkali of nitroblue tetrazolium chloride is added into extracting solution, observes solution colour.
In the present invention in cosmetics glucocorticoid rapid assay methods, specifically comprise the following steps:
1) preparation of sample:Cosmetics 1-2g or so is taken, the extraction of 2-10mL methanol is added, passes through hand vibration after mixing
Afterwards;Fluid sample directly takes 1-2mL to add methanol 2mL;Supernatant liquid, supernatant or filtrate are taken, this is extracting solution.
2) detection reagent configures:Strong base solution (the naoh concentration for the methanol that configuration nitroblue tetrazolium chloride is dissolved in
For 50-400g/kg) in, nitroblue tetrazolium chloride methanol solution 0.1-2g/L.This is detection reagent.
3) detect:In extracting solution, the strong base solution 2 for adding the methanol that nitroblue tetrazolium chloride is dissolved in drips, and observes face
Color change.Solution colour shows blueness or blue-green, and explanation may contain glucocorticoid, and different glucocorticoid color changes is omited
Have any different.
The examination inspection of glucocorticoid whether is added in cosmetics are examined it is an object of the invention to provide the above method
Application in testing.
Another object of the present invention is to provide the above method to prepare the application of glucocorticoid quick testing reagent kit.
The technique effect and advantage of the present invention:Compared with the existing technology, the present invention has the advantages that:
1) it is quick, easy:Extraction process 1 minute, chromogenic reaction 30 seconds, whole operation process is completed in 5 minutes, relatively
It is much simple and efficient in liquid chromatogram, LC-MS method (at least 2-3 hour), and without reference substance.
2) specificity is strong, accuracy rate is high:According to method validation as a result, the common cosmetics pair such as toner, facial mask, facial cleanser
The detection of glucocorticoid is detectable.
3) it is quick on the draw:The minimum detectability of this experiment material to be checked reaches 1 μ g of clinical minimum effective dose, therefore uses
This method checks that whether adding glucocorticoid component in cosmetics has enough sensitivity.
4) it is applied widely:This method can be used for fluid sample and solid sample cosmetics and this method can be used.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, below in conjunction with specific embodiment, to this
Invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, not
For limiting the present invention.Based on the embodiments of the present invention, those of ordinary skill in the art are not before creative work is made
All other embodiments obtained are put, belong to the scope of protection of the invention.
The quick determination method of glucocorticoid, includes the following steps in a kind of cosmetics:
1) glucocorticoid in cosmetics is extracted with methanol;
2) aqueous slkali of nitroblue tetrazolium chloride is added into extracting solution, observes solution colour.
In the present invention in cosmetics glucocorticoid rapid assay methods, specifically comprise the following steps:
1) preparation of sample:Cosmetics 1-2g is taken, the extraction of 2-10mL methanol is added, passes through hand vibration after stirring and evenly mixing
Afterwards;Fluid sample directly takes 1-2mL to add methanol 2mL.Take supernatant liquid, supernatant or filtrate extracting solution the most;
2) detection reagent configures:The methanol that nitroblue tetrazolium chloride is dissolved in the sodium hydroxide that solvent is 50-400g/kg is molten
In liquid, nitroblue tetrazolium chloride methanol solution 0.1-2g/L, as detection reagent;
3) detect:In extracting solution, the strong base solution 2 for adding the methanol that nitroblue tetrazolium chloride is dissolved in drips, and observes face
Color change;Solution colour shows blueness or blue-green, and different glucocorticoid color changes is slightly distinguished.
It is an object of the invention to provide the above method whether glucocorticoid is added in cosmetics are examined
Application in examination inspection.
Another object of the present invention is to provide the above method to prepare the application of glucocorticoid quick testing reagent kit.
Application example
Present invention also offers a kind of application of the quick determination method of glucocorticoid in cosmetics.Randomly select market
Upper various cosmetics, most sample in detected totally 30 batch samples, measure glucocorticoid as stated above.
It is detected to contain glucocorticoid in 9 and 10 samples respectively in 15 domestic samples and 15 South Korea's samples.It can be seen from the above that
Glucocorticosteroid hormone recall rate is higher in cosmetics.Glucocorticosteroid hormone is added in cosmetics, skin can be made to this generation dependence
Property, long this cause skin or even the physical and mental health of oneself irreversible injury using meeting, so quickly being examined personally for
Survey with regard to it is particularly important that.
The cosmetics of and South Korea domestic in the market production respectively choose the detection of 15 kinds of progress glucocorticoids, and detection structure is such as
Shown in following table
+ represent positive, detect glucocorticoid;- represent negative sample, glucocorticoid is not detected
Finally it should be noted that:The foregoing is only a preferred embodiment of the present invention, is not intended to limit the invention,
Although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, it still may be used
To modify to the technical solution described in foregoing embodiments, or equivalent substitution is carried out to which part technical characteristic,
Within the spirit and principles of the invention, any modification, equivalent replacement, improvement and so on, should be included in the present invention's
Within protection domain.
Claims (4)
- A kind of 1. quick determination method of glucocorticoid in cosmetics, it is characterised in that:Include the following steps:1) glucocorticoid in cosmetics is extracted with methanol;2) aqueous slkali of nitroblue tetrazolium chloride is added into extracting solution, observes solution colour.
- 2. the quick determination method of glucocorticoid in a kind of cosmetics as claimed in claim 1, it is characterised in that:Including with Lower step:1) preparation of sample:Take cosmetics 1-2g, add the extraction of 2-10mL methanol, after stirring and evenly mixing by hand vibration after;Liquid Body sample directly takes 1-2mL to add methanol 2mL;Take supernatant liquid, supernatant or filtrate extracting solution the most;2) detection reagent configures:Nitroblue tetrazolium chloride is dissolved in the methanol solution for the sodium hydroxide that solvent is 50-400g/kg In, nitroblue tetrazolium chloride methanol solution 0.1-2g/L, as detection reagent;3) detect:In extracting solution, the strong base solution 2 for adding the methanol that nitroblue tetrazolium chloride is dissolved in drips, and observation color becomes Change;Solution colour shows blueness or blue-green, and different glucocorticoid color changes is slightly distinguished.
- 3. the quick determination method of glucocorticoid is quickly examined preparing glucocorticoid in the cosmetics described in claim 1 Application in kit.
- 4. the sieve of the quick determination method of glucocorticoid glucocorticoid in cosmetics in the cosmetics described in claim 1 The application checked in testing.
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