CN109211888A - The rapid detection method of glucocorticoid in a kind of cosmetics - Google Patents
The rapid detection method of glucocorticoid in a kind of cosmetics Download PDFInfo
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- CN109211888A CN109211888A CN201811097181.9A CN201811097181A CN109211888A CN 109211888 A CN109211888 A CN 109211888A CN 201811097181 A CN201811097181 A CN 201811097181A CN 109211888 A CN109211888 A CN 109211888A
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- cosmetics
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- 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
Abstract
The invention discloses a kind of rapid detection methods of glucocorticoid in cosmetics, specific reaction is occurred by the functional group of nitroblue tetrazolium chloride strong basicity methanol solution and glucocorticoid, generate color, it can quickly detect in sample and whether contain glucocorticoid, in the preparation step of sample, saturated sodium chloride solution is added into cosmetics, and it is extracted with acetonitrile, later by using potassium ferrocyanide cooperation zinc acetate as clarifying agent, the impurity that the zinc ferrocyanide generated using zinc acetate and ferrocyanide nak response precipitates to hold under the arm away or adsorb cosmetics itself, interfering substance and macromolecular substances, extraction effect is good, testing result is accurate, this method detection is quick, using safe, it is easy to operate.
Description
Technical field
The invention belongs to cosmetics detection detection technique field more particularly to a kind of quick inspections of cosmetics glucocorticoid
Survey method.
Background technique
Glucocorticoid has the function of the biosynthesis and metabolism of adjusting sugar, fat, protein, and short-period used can make skin
The smooth exquisiteness of skin, skin is white ruddy glossy, plays beautification function, but what is be used for a long time will lead to body endocrine system disorder,
And leading to a series of side effects, such as variability eczema-like dermatitis etc., main cause has at 3 points: first is that glucocorticoid is anti-inflammatory but
Not antibacterial, caused immunosuppression mechanism can make cutaneous autoimmune system by a degree of damage, reduce siberian crabapple
The invasion and injury united to extraneous bacterium, virus, microorganism etc. to body；Second is that it can also inhibit immune response, it is used for a long time
The immunologic balance of skin can be destroyed, so that mad compensatory reinforcement occurs in the immune recovery of human body after deactivating, is caused tight
The allergic state of weight；Third is that its synthesis that can also reduce protein stimulates capillary to destroy skin barrier, after deactivating
Skin is set the problems such as excessively thin cuticula, dry, itch, red capillary occur.Therefore, China " cosmetics health specification " (2007
Version), the glucocorticoids such as clobetasol propionate, dexamethasone and betamethasone are to forbid the nocuousness being added in cosmetics
Ingredient.
In recent years, for the safety problem of the cosmetics also concern increasingly by society and supervision department.As the country
The main supervision department of cosmetics, state food pharmaceuticals administration general bureau do not conform to per average annual repeatedly publication about commercially available cosmetics
The notice of lattice, it is exceeded etc. for main detection item containing glucocorticoid, antibiotic, heavy metal and microorganism with detection.Unqualified production
In product, adds the facial mask class of glucocorticoid in violation of rules and regulations and acne eliminating cream class product accounts for big specific gravity.Currently, sugared cortical hormone in cosmetics
Element is detected to be analyzed usually using high performance liquid chromatography or liquid chromatograph mass spectrography, cumbersome, Check-Out Time is long, no
The requirement quickly detected suitable for superintendent office, testing agency, a large amount of samples in all kinds of mechanisms scene.
Existing patent directly extracts the glucocorticoid in cosmetics using methanol, however in view of cosmetics itself
Matrix is more complicated, containing a large amount of surfactant, directlys adopt methanol and extracts that impurity is more, and influence factor is more, be easy
Cause testing result wrong.For this purpose, it is proposed that a kind of rapid detection method of glucocorticoid, to solve above-mentioned background technique
In the problem of mentioning.
Summary of the invention
The purpose of the invention is to overcome the problems of the prior art, a kind of the fast of glucocorticoid in cosmetics is provided
Fast detection method.
The object of the present invention is to provide a kind of rapid detection methods of glucocorticoid in cosmetics, including walk as follows
It is rapid:
S1, the preparation of sample:
1-2g cosmetics are taken, 2-5mL saturated sodium chloride solution is added, is extracted, is stirred and evenly mixed with the acetonitrile solution of 2-10mL
After be centrifuged, collect supernatant liquid, repeat to merge all supernatant liquids of collection after extracting 2 times, and as first extracting solution, in ancient times
The distilled water of 5-10mL is added in secondary extracting solution, after mixing, the potassium ferrocyanide solution of 0.2mL and the zinc acetate of 0.2mL is added
Solution mixes, and centrifugation takes supernatant liquid as final extracting solution；
S2, the preparation of detection reagent:
Nitroblue tetrazolium chloride is dissolved in the methanol solution for the sodium hydroxide that solvent is 50-400g/kg, chlorination nitro four
Nitrogen azoles indigo plant methanol solution 0.1-2g/L, as detection reagent；
S3, detection method:
In final extracting solution, the drop of strong base solution 2 that nitroblue tetrazolium chloride is dissolved in methanol is added, observation color becomes
Change, the aobvious blue of solution colour or blue-green indicate have glucocorticoid or glucocorticoid concentration to be higher than detection limit in sample.
Preferably, cosmetics are liquid or cosmetics in S1, and liquid make-up taken amount is 1-2mL, emulsus makeup
Product taken amount is 1-2g.
Preferably, the centrifugation is using medical centrifuge, model Microfuge16 benchtop microcentrifuge.
Compared with prior art, the beneficial effects of the present invention are:
The purpose of the present invention is to provide a kind of rapid detection methods 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, generates color, can be fast with sxemiquantitative
Speed detects whether contain glucocorticoid in sample, and in the preparation step of sample, saturated sodium-chloride is added into cosmetics
Solution is simultaneously extracted with acetonitrile, utilizes zinc acetate [Zn as clarifying agent by using potassium ferrocyanide cooperation zinc acetate later
(CH3COO)2·2H2O] precipitated with the zinc ferrocyanide that ferrocyanide nak response generates it is miscellaneous come what is held under the arm away or adsorb cosmetics itself
Matter, interfering substance and macromolecular substances, extraction effect is good, and testing result is accurate, and this method detection is quick, uses safe, behaviour
Make easy.
Specific embodiment
Specific embodiments of the present invention will be described in detail below, it is to be understood that protection scope of the present invention is not
It is restricted by specific implementation.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creativeness
Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of labour.Following embodiment and comparative examples
In, if not specified, what the method or reagent used can obtain for this field conventional means, it should be noted that
The present invention is centrifuged using medical centrifuge, model Microfuge16 benchtop microcentrifuge.
Embodiment 1
The rapid detection method of glucocorticoid, includes the following steps: in a kind of cosmetics of the present embodiment
S1, the preparation of sample:
1g cosmetics are taken, 5mL saturated sodium chloride solution is added, is extracted with the acetonitrile solution of 10mL, is centrifuged after stirring and evenly mixing,
It repeats to take supernatant liquid after extracting 2 times or supernatant is first extracting solution and merges first extracting solution, be added into extracting solution
After mixing, the potassium ferrocyanide solution of 0.2mL and the acetic acid zinc solution of 0.2mL is added in the distilled water of 10mL, is mixed, and centrifugation takes
Supernatant liquid or supernatant are final extracting solution；
S2, the preparation of detection reagent:
Nitroblue tetrazolium chloride is dissolved in the methanol solution for the sodium hydroxide that solvent is 50-400g/kg, chlorination nitro four
Nitrogen azoles indigo plant methanol solution 0.1-2g/L, as detection reagent；
S3, detection method:
In final extracting solution, the drop of strong base solution 2 that nitroblue tetrazolium chloride is dissolved in methanol is added, observation color becomes
Change, the aobvious blue of solution colour or blue-green indicate have glucocorticoid or glucocorticoid concentration to be higher than detection limit in sample.
Embodiment 2
The rapid detection method of glucocorticoid, includes the following steps: in a kind of cosmetics of the present embodiment
S1, the preparation of sample:
1mL liquid make-up is taken, 2mL saturated sodium chloride solution is added, is extracted with the acetonitrile solution of 2mL, after stirring and evenly mixing
Centrifugation repeats to take supernatant liquid after extracting 2 times or supernatant is first extracting solution and merges first extracting solution, adds into extracting solution
After mixing, the potassium ferrocyanide solution of 0.2mL and the acetic acid zinc solution of 0.2mL is added in the distilled water for entering 5mL, is mixed, centrifugation,
It takes supernatant liquid or supernatant is final extracting solution；
S2, the preparation of detection reagent:
Nitroblue tetrazolium chloride is dissolved in the methanol solution for the sodium hydroxide that solvent is 50-400g/kg, chlorination nitro four
Nitrogen azoles indigo plant methanol solution 0.1-2g/L, as detection reagent；
S3, detection method:
In final extracting solution, the drop of strong base solution 2 that nitroblue tetrazolium chloride is dissolved in methanol is added, observation color becomes
Change, the aobvious blue of solution colour or blue-green indicate have glucocorticoid or glucocorticoid concentration to be higher than detection limit in sample.
Embodiment compliance test result:
Using the method for embodiment 1 and embodiment 2 detect following 10 kinds of glucocorticoid types include: hydrocortisone,
Betamethasone, dexamethasone, triamcinolone, dexamethasone acetate, cortisone acetate, fludrocortisone acetate, prednisolone, fluorine
Prednisolone, Methyllprednisolone, the above are current common violated addition types.
Each 1.0mg of each standard substance is accurately weighed, 10mL is settled to ethyl alcohol dissolution, obtains 0.1mg/mL standard solution, so
It is diluted to 5 μ g/mL step by step with ethyl alcohol afterwards, obtains standard working solution.
The step of preparation of detection reagent and detection method are with embodiment 1.Itself the result shows that, to above-mentioned 10 kinds sugared cortical hormones
The drop of strong base solution 2 that nitroblue tetrazolium chloride is dissolved in methanol is added in the standard working solution of element, observes color change, Suo Yourong
The aobvious blue of liquid color or blue-green, i.e., above-mentioned 10 kinds of glucocorticoids can detect, the inspection of glucocorticoid in liquid make-up
Rising limit is 1 μ g/mL, and the detection of glucocorticoid is limited to 1 μ g/g in cosmetics.
Comparative example 1
This comparative example is only that the preparation method of sample is different from the difference of embodiment 1, this comparative example uses following sample
Preparation:
1g cosmetics are taken, is extracted with the methanol solution of 10mL, is centrifuged after stirring and evenly mixing, repeat to take upper liquid after extracting 2 times
Body or supernatant are extracting solution and combined extract.
Comparative example 2
This comparative example is only that the preparation method of sample is different from the difference of embodiment 1, this comparative example uses following sample
Preparation:
1g cosmetics are taken, 5mL saturated sodium chloride solution is added, is extracted with the acetonitrile solution of 10mL, is centrifuged after stirring and evenly mixing,
It repeats to take supernatant liquid after extracting 2 times or supernatant is extracting solution and merges the extracting solution extracted twice.
Comparative example compliance test result:
Using the method for comparative example 1 and comparative example 2 detect following 10 kinds of glucocorticoid types include: hydrocortisone,
Betamethasone, dexamethasone, triamcinolone, dexamethasone acetate, cortisone acetate, fludrocortisone acetate, prednisolone, fluorine
Prednisolone, Methyllprednisolone.
Each 1.0mg of each standard substance is accurately weighed, 10mL is settled to ethyl alcohol dissolution, obtains 0.1mg/mL standard solution, so
It is diluted to 5 μ g/mL step by step with ethyl alcohol afterwards, obtains standard working solution.
The step of preparation of detection reagent and detection method are with embodiment 1.Itself the result shows that, to above-mentioned 10 kinds sugared cortical hormones
The drop of strong base solution 2 that nitroblue tetrazolium chloride is dissolved in methanol is added in the standard working solution of element, observes color change, wherein
The aobvious blue of the color of six kinds of solution or blue-green, respectively dexamethasone acetate, cortisone acetate, fludrocortisone acetate, first
Base prednisone, betamethasone and dexamethasone, other four kinds of solution do not develop the color, i.e., above-mentioned 10 kinds of glucocorticoids only have six kinds can
Detection, there is a certain error for testing result.
Application Example:
Randomly select all kinds of cosmetics that domestic in the market and South Korea produces, detected totally 40 batch sample, by embodiment 1
The method measures glucocorticoid.Wherein, 10 domestic face packs and 10 Korea Spro produce in face packs respectively by
It detects to contain glucocorticoid in 4 and 6 samples；Wherein, 10 domestic acne eliminating creams and 10 Korea Spro produce in acne eliminating cream respectively
It detects to contain glucocorticoid in 5 and 7 samples.It can be seen that glucocorticosteroid hormone recall rate is higher in cosmetics.
Testing result is shown in Tables 1 and 2.
The testing result of glucocorticoid in 1 facial mask of table
The testing result of glucocorticoid in 2 acne eliminating cream of table
| Sample ID | Testing result | Sample ID | Testing result |
| No. 1 domestic acne eliminating cream | + | No. 1 Korea Spro produces acne eliminating cream | - |
| No. 2 domestic acne eliminating creams | - | No. 2 Korea Spro produce acne eliminating cream | - |
| No. 3 domestic face acne eliminating creams | + | No. 3 Korea Spro produce acne eliminating cream | + |
| No. 4 domestic acne eliminating creams | - | No. 4 Korea Spro produce acne eliminating cream | - |
| No. 5 domestic acne eliminating creams | + | No. 5 Korea Spro produce acne eliminating cream | - |
| No. 6 domestic acne eliminating creams | - | No. 6 Korea Spro produce acne eliminating cream | - |
| No. 7 domestic acne eliminating creams | + | No. 7 Korea Spro produce acne eliminating cream | + |
| No. 8 domestic acne eliminating creams | - | No. 8 Korea Spro produce acne eliminating cream | - |
| No. 9 domestic acne eliminating creams | + | No. 9 Korea Spro produce acne eliminating cream | + |
| No. 10 domestic acne eliminating creams | - | No. 10 Korea Spro produce acne eliminating cream | - |
Using same:
As a result judge:
Negative (-): having colour developing, indicates have glucocorticoid or glucocorticoid concentration to be higher than detection limit in sample.
Positive (+): without colour developing, indicate that glucocorticoid concentration is lower than detection limit or without glucocorticoid in sample.
If positive as the result is shown, need to use national related official method further progress experimental analysis to confirm.
To sum up, in a kind of cosmetics provided by the invention glucocorticoid rapid detection method, by four nitrogen of chlorination nitro
Specific reaction occurs for the functional group of azoles indigo plant strong basicity methanol solution and glucocorticoid, generates color, can be quick with sxemiquantitative
Detect whether contain glucocorticoid in sample, in the preparation step of sample, it is molten that saturated sodium-chloride is added into cosmetics
Liquid is simultaneously extracted with acetonitrile, utilizes zinc acetate [Zn as clarifying agent by using potassium ferrocyanide cooperation zinc acetate later
(CH3COO)2·2H2O] precipitated with the zinc ferrocyanide that ferrocyanide nak response generates it is miscellaneous come what is held under the arm away or adsorb cosmetics itself
Matter, interfering substance and macromolecular substances, extraction effect is good, and testing result is accurate, and this method detection is quick, uses safe, behaviour
Make easy.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (4)
1. the rapid detection method of glucocorticoid in a kind of cosmetics, characterized by the following steps:
S1, the preparation of sample:
Take 1-2g cosmetics, 2-5mL saturated sodium chloride solution be added, extracted with the acetonitrile solution of 2-10mL, after stirring and evenly mixing from
The heart collects supernatant liquid, repeats all supernatant liquids for merging collection after extracting 2 times, and as first extracting solution, past to mention for the first time
The distilled water that 5-10mL is added in liquid is taken, after mixing, the potassium ferrocyanide solution of 0.2mL and the acetic acid zinc solution of 0.2mL is added,
It mixes, centrifugation takes supernatant liquid as final extracting solution；
S2, the preparation of detection reagent:
Nitroblue tetrazolium chloride is dissolved in the methanol solution for the sodium hydroxide that solvent is 50-400g/kg, chlorination nitro tetrazole
Blue methanol solution 0.1-2g/L, as detection reagent；
S3, detection method:
The drop of strong base solution 2 that nitroblue tetrazolium chloride is dissolved in methanol is added in final extracting solution, observes color change, solution
The aobvious blue of color or blue-green indicate have glucocorticoid or glucocorticoid concentration to be higher than detection limit in sample.
2. the rapid detection method of glucocorticoid in a kind of cosmetics according to claim 1, it is characterised in that: in S1
Cosmetics are liquid or cosmetics, and liquid make-up taken amount is 1-2mL, and cosmetics taken amount is 1-2g.
3. the rapid detection method of glucocorticoid in a kind of cosmetics according to claim 1, it is characterised in that: described
Centrifugation is using medical centrifuge, model Microfuge16 benchtop microcentrifuge.
4. the rapid detection method of glucocorticoid in a kind of cosmetics according to claim 1, it is characterised in that: sugared skin
Matter hormone includes hydrocortisone, betamethasone, dexamethasone, triamcinolone, dexamethasone acetate, cortisone acetate, acetic acid
Fludrocortison, prednisolone, fluprednisolone, Methyllprednisolone.
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| CN201811097181.9A CN109211888A (en) | 2018-09-20 | 2018-09-20 | The rapid detection method of glucocorticoid in a kind of cosmetics |
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| CN201811097181.9A CN109211888A (en) | 2018-09-20 | 2018-09-20 | The rapid detection method of glucocorticoid in a kind of cosmetics |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112485244A (en) * | 2020-10-14 | 2021-03-12 | 中国食品药品检定研究院 | Application of 3,3',5,5' -tetramethylbenzidine in detection of benzoyl peroxide in acne-removing cosmetics |
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| CN106443019A (en) * | 2016-08-31 | 2017-02-22 | 广东省药品检验所 | Method for rapidly detecting multiple glucocorticoids in cosmetics |
| CN108007926A (en) * | 2017-12-01 | 2018-05-08 | 温州科技职业学院 | The quick determination method of glucocorticoid and application in a kind of cosmetics |
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2018
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106443019A (en) * | 2016-08-31 | 2017-02-22 | 广东省药品检验所 | Method for rapidly detecting multiple glucocorticoids in cosmetics |
| CN108007926A (en) * | 2017-12-01 | 2018-05-08 | 温州科技职业学院 | The quick determination method of glucocorticoid and application in a kind of cosmetics |
Non-Patent Citations (1)
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112485244A (en) * | 2020-10-14 | 2021-03-12 | 中国食品药品检定研究院 | Application of 3,3',5,5' -tetramethylbenzidine in detection of benzoyl peroxide in acne-removing cosmetics |
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