CN102346104A - Preparation method of standard substance used for detecting aconitine in cosmetic - Google Patents
Preparation method of standard substance used for detecting aconitine in cosmetic Download PDFInfo
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- CN102346104A CN102346104A CN2011101801696A CN201110180169A CN102346104A CN 102346104 A CN102346104 A CN 102346104A CN 2011101801696 A CN2011101801696 A CN 2011101801696A CN 201110180169 A CN201110180169 A CN 201110180169A CN 102346104 A CN102346104 A CN 102346104A
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- aconitine
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Abstract
The invention relates to a preparation method of a standard substance used for detecting aconitine in cosmetic, which is characterized in that a cosmetic emulsion is mixed with an aconitine aqueous solution or a propylene glycol solution to form the standard substance used for detecting aconitine in cosmetic. The formula of the cosmetic emulsion comprises the following components by weight percentage: phase A: 72-78% of deionized water, 3-3.5% of propylene glycol and 0.20-0.25% of carbomer; phase B: 4.5-5% of stearic acid ester, 2-4% of cetostearyl alcohol and 10-14% of No.26 white oil; phase C: 1.20 to 1.25% of phenoxy ethanol and ethyl hexyl glycerin; and the concentration of the aconitine in the standard substance is 0.1-1.0g/100mL. The method has the advantages that: the aconitine and the cosmetic emulsion are mixed to form the standard substance for detecting the aconitine in the cosmetics; and the standard substance is the same as a aconitine-containing cosmetic sample in actual use, so that the detection of the aconitine in the cosmetics better accords with the state of the actual application, and the detection is more accurate.
Description
Technical field
The present invention relates to a kind of compound method that is used to detect the standard substance of cosmetics mesaconitine, this method is with aconitine, mixes through certain technical method and cosmetics cream frost, is formed for detecting the standard substance of cosmetics mesaconitine.
Background technology
Aconitine is the main toxic substance that is present in the plants such as monkshood, radix aconiti agrestis, monkshood.It is one of important leverage measure of cosmetics safety property that the cosmetics mesaconitine detects; The direct compound test method of present more employing; But; In practical application; Aconitine in the cosmetics is with after formula components is mixed; Have than big difference with compound test when detecting again Yu directly, can influence the degree of accuracy of detection.Compare with n-compound; The cosmetic standard material not only has the measurement standard of accurate value; Also have one or more enough all even characteristic values of well having confirmed; Traceability with value is to the detection level, the unified measured value that improve Cosmetic Manufacture, cosmetics check, to estimate and carry out personnel checking-up and management work standardization etc. for the cosmetics method of inspection of setting up all significant.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of compound method that is used to detect the standard substance of cosmetics mesaconitine; Aconitine is mixed with cosmetics cream frost through certain technical method, be formed for detecting the standard substance that the cosmetics mesaconitine detects.
The present invention solves the problems of the technologies described above the technical scheme of being taked: a kind of compound method that is used to detect the standard substance of cosmetics mesaconitine; The water or the propylene glycol solution of aconitine are mixed with cosmetics cream frost; Be formed for detecting the standard substance of cosmetics mesaconitine, wherein
The prescription of said cosmetics cream frost is by weight percentage:
A phase deionized water 72～78
Propylene glycol 3～3.5
Carbomer 0.20～0.25;
B phase stearate 4.5～5
16 alcohol 2～4
26# white oil 10～14;
C phase Phenoxyethanol and ethylhexyl glycerine 1.20～1.25;
The concentration of said aconitine in standard substance reaches 0.1～1.0 g/100mL.
Patent of the present invention through with the aconitine compound with after the cosmetic formulations composition mixes; The identical cosmetic sample that contains aconitine when processing with actual the use; Thereby make the detection of cosmetics mesaconitine is more met the state of practical application, and make detection more accurate.
Concrete, A mutually in, the content of deionized water can be 72,73,74,75,76,77 or 78%; The content of propylene glycol can be 3,3.1,3.2,3.3,3.4 or 3.5%; Carbomer 0.20,0.21,0.22,0.23,0.24 or 0.25%;
B mutually in, the content of stearate can be 4,4.1,4.2,4.3,4.4 or 4.5%; The content of 16 alcohol can be 2,2.5,3,3.5 or 4%; The content of 26# white oil can be 10,11,12,13 or 14%;
The content of the Phenoxyethanol of C phase and ethylhexyl glycerine can be 1.20,1.21,1.22,1.23,1.24 or 1.25%.
On the basis of such scheme, the compound method of cosmetics cream frost comprises the steps:
The first step: in advance the carbomer of A in mutually is uniformly dispersed in glycerine;
Second step: all the other components of A phase are added, be heated to more than 80 ℃, stir; With B each component mixing mutually, be heated to more than 80 ℃, stir;
The 3rd step: stir down, B is added to the A phase, homogeneous is more than 3 minutes;
The 4th step: stir down, be cooled to below 45 ℃, add the C phase, stir;
The 5th step: stir down, be cooled to room temperature, process cosmetics cream frost.
On the basis of such scheme; The water of said aconitine or propylene glycol solution concentration are 1～3 g/100mL; The water or the propylene glycol solution of aconitine are slowly joined in the cosmetics cream frost; And make the ultimate density of aconitine in standard substance reach 0.1～1.0 g/100mL, keep temperature constant under 15～25 ℃ of conditions with minimum water evaporates, slowly to stir.
Concrete; The water of aconitine or propylene glycol solution concentration can be 1,1.2,1.4,1.6,1.8,2,2.2,2.4,2.6,2.8 or 3 g/100mL, and the ultimate density of aconitine in standard substance can be 0.1,0.2,0.3,0.4,0.5,0.6,0.7,0.8,0.9 or 1.0%.
The invention has the beneficial effects as follows:
The present invention mixes aconitine with cosmetics cream frost; Be formed for detecting the standard substance of cosmetics mesaconitine; This standard substance contains aconitine when using with reality cosmetic sample is identical; Thereby make the detection of cosmetics mesaconitine is more met the state of practical application, and make detection more accurate.
Embodiment
A kind of compound method that is used to detect the standard substance of cosmetics mesaconitine is mixed the propylene glycol solution and the cosmetics cream frost of aconitine, is formed for detecting the standard substance of cosmetics mesaconitine, wherein,
The prescription of said cosmetics cream frost is by weight percentage:
The compound method of cosmetics cream frost comprises the steps:
The first step: in advance the carbomer of A in mutually is uniformly dispersed in glycerine;
Second step: all the other components of A phase are added, be heated to more than 80 ℃, stir; With B each component mixing mutually, be heated to more than 80 ℃, stir;
The 3rd step: stir down, B is added to the A phase, homogeneous is more than 3 minutes;
The 4th step: stir down, be cooled to below 45 ℃, add the C phase, stir;
The 5th step: stir down, be cooled to room temperature, process cosmetics cream frost.
Embodiment 1
Be mixed with cosmetics cream frost according to prescription and preparation technology in the table.Aconitine is mixed with 2g/100mL water (propylene glycol) solution; Water (propylene glycol) solution that will contain aconitine then slowly joins in the cream frost; Make the ultimate density of aconitine reach 0.1 g/100mL, under the condition that keeps temperature constant and minimum water evaporates, slowly stir packing.
Embodiment 2
Be mixed with cosmetics cream frost according to prescription and preparation technology in the table.Aconitine is mixed with the propylene glycol solution of 2g/100mL; The propylene glycol solution that will contain aconitine then slowly joins in the cream frost; Make the ultimate density of aconitine reach 0.5 g/100mL, under the condition that keeps temperature constant and minimum water evaporates, slowly stir packing.
Embodiment 3
Be mixed with cosmetics cream frost according to prescription and preparation technology in the table.Aconitine is mixed with the propylene glycol solution of 2g/100mL; The propylene glycol solution that will contain aconitine then slowly joins in the cream frost; Make the ultimate density of aconitine reach 1.0 g/100mL, under the condition that keeps temperature constant and minimum water evaporates, slowly stir packing.
The purity of used aconitine is more than 98%.
Standard substance of the present invention is used to detect the uniformity testing of cosmetics mesaconitine:
Homogeneity is the most basic attribute of standard substance; Project (GB/T15000.9-94) is randomly drawed the n bottle to the standard substance of being developed according to " standard model work guide rule (5): chemical constitution standard model technology general rule "; With wherein one bottle as basic contrast points; All the other n-1 bottles adopt corresponding mathematical statistics method that the homogeneity of each standard substance is studied as check point.。
1.1 uniformity testing method
With F method of inspection and t method of inspection.
Specific practice is: in 16 bottles of samples that extract, optional one bottle of basic contrast points of conduct is done the measurement of one group of 15 Hypaconitine content altogether; All the other 15 bottles as the checkpoint, every bottle of measurement of making a Hypaconitine content; Difference calculating mean value and variance.
Significant difference with F method of inspection check this variance of taking a sample has following judgment formula:
In the formula:
S
1 2The variance of-checkpoint
S
2 2The variance of-contrast points
F α (ν
1, ν
2)-given level of significance α and degree of freedom (ν
1, ν
2) the critical value of statistical test, F α (14,14)=2.48 tables look-up;
ν-degree of freedom, ν=n-1.
When satisfying formula (1), then there is not significant difference in two groups variance.
The significant difference of t method of inspection check this mean value of taking a sample has following judgment formula:
In the formula:
x
1The average value measured of-checkpoint;
x
2The average value measured of-contrast points;
When satisfying formula (2), there is not significant difference in two groups mean value.
1.2 sampling number
The total number of samples of each species N is 200 bottles, according to 3
to calculate the number of samples, randomly selected 18 bottles, which take 16 bottles for homogeneity testing.
1.3 sample mode
Press table of random numbers sample drawn, remove repetition and useless, extract 16 bottles of samples.
1.4 check instrument
High performance liquid chromatograph, model: Agilent 1100.
If there is not significant difference in the assay of F method of inspection and t method of inspection, illustrate that then this standard substance is uniform.
Data by table 1 and table 2 can know, in level of significance α=0.05, the degree of freedom of inspection group and contrast groups is (F under 14 the situation
0.05(14,14)=2.48, t
(0.05,28)=2.05), the mensuration result of two kinds of contents levels all meets formula (1) and formula (2).Therefore can judge two groups of results' mensuration variance indifference, measure the mean value indifference.
Claims (3)
1. compound method that is used to detect the standard substance of cosmetics mesaconitine is characterized in that: the water or the propylene glycol solution of aconitine mixed with cosmetics cream frost, is formed for detecting the standard substance of cosmetics mesaconitine, wherein,
The prescription of said cosmetics cream frost is by weight percentage:
A phase deionized water 72～78
Propylene glycol 3～3.5
Carbomer 0.20～0.25;
B phase stearate 4.5～5
16 alcohol 2～4
26# white oil 10～14;
C phase Phenoxyethanol and ethylhexyl glycerine 1.20～1.25;
The concentration of said aconitine in standard substance reaches 0.1～1.0 g/100mL.
2. the compound method that is used to detect the standard substance of cosmetics mesaconitine according to claim 1 is characterized in that: the compound method of cosmetics cream frost comprises the steps:
The first step: in advance the carbomer of A in mutually is uniformly dispersed in glycerine;
Second step: all the other components of A phase are added, be heated to more than 80 ℃, stir; With B each component mixing mutually, be heated to more than 80 ℃, stir;
The 3rd step: stir down, B is added to the A phase, homogeneous is more than 3 minutes;
The 4th step: stir down, be cooled to below 45 ℃, add the C phase, stir;
The 5th step: stir down, be cooled to room temperature, process cosmetics cream frost.
3. the compound method that is used to detect the standard substance of cosmetics mesaconitine according to claim 1; It is characterized in that: the water of said aconitine or propylene glycol solution concentration are 1～3 g/100mL; The water or the propylene glycol solution of aconitine are slowly joined in the cosmetics cream frost; And make the ultimate density of aconitine in standard substance reach 0.1～1.0 g/100mL, keep temperature constant under 15～25 ℃ of conditions with minimum water evaporates, slowly to stir.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011101801696A CN102346104A (en) | 2011-06-30 | 2011-06-30 | Preparation method of standard substance used for detecting aconitine in cosmetic |
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| CN2011101801696A CN102346104A (en) | 2011-06-30 | 2011-06-30 | Preparation method of standard substance used for detecting aconitine in cosmetic |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102721597A (en) * | 2012-07-16 | 2012-10-10 | 上海相宜本草化妆品股份有限公司 | Method for preparing standard substance for detecting imperatorin in cosmetics |
| CN103630436A (en) * | 2013-12-03 | 2014-03-12 | 中山鼎晟生物科技有限公司 | Standard substance used for detecting preservative in cosmetics and preparation method thereof |
| CN104390839A (en) * | 2014-12-12 | 2015-03-04 | 中国计量科学研究院 | Reference material for cream cosmetics containing heavy metal element mercury and preparation method of reference material |
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| CN101904803A (en) * | 2010-09-03 | 2010-12-08 | 上海市计量测试技术研究院 | Method for preparing standard substance for detecting preservative in cosmetic |
| CN101912351A (en) * | 2010-09-03 | 2010-12-15 | 上海相宜本草化妆品有限公司 | Method for preparing standard substance for detecting heavy metal in cosmetics |
| CN101936835A (en) * | 2010-09-03 | 2011-01-05 | 上海相宜本草化妆品有限公司 | Method for preparing standard substance for detecting scurf removing agent in cosmetics |
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2011
- 2011-06-30 CN CN2011101801696A patent/CN102346104A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101904806A (en) * | 2010-09-03 | 2010-12-08 | 上海市计量测试技术研究院 | Method for preparing standard substance for detecting antibiotics in cosmetics |
| CN101904803A (en) * | 2010-09-03 | 2010-12-08 | 上海市计量测试技术研究院 | Method for preparing standard substance for detecting preservative in cosmetic |
| CN101912351A (en) * | 2010-09-03 | 2010-12-15 | 上海相宜本草化妆品有限公司 | Method for preparing standard substance for detecting heavy metal in cosmetics |
| CN101936835A (en) * | 2010-09-03 | 2011-01-05 | 上海相宜本草化妆品有限公司 | Method for preparing standard substance for detecting scurf removing agent in cosmetics |
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| CN102721597A (en) * | 2012-07-16 | 2012-10-10 | 上海相宜本草化妆品股份有限公司 | Method for preparing standard substance for detecting imperatorin in cosmetics |
| CN103630436A (en) * | 2013-12-03 | 2014-03-12 | 中山鼎晟生物科技有限公司 | Standard substance used for detecting preservative in cosmetics and preparation method thereof |
| CN104390839A (en) * | 2014-12-12 | 2015-03-04 | 中国计量科学研究院 | Reference material for cream cosmetics containing heavy metal element mercury and preparation method of reference material |
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Application publication date: 20120208 |