CN104569187B - The detection method of whitening and speckle dispelling composition and device in cosmetics - Google Patents
The detection method of whitening and speckle dispelling composition and device in cosmetics Download PDFInfo
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Abstract
The present invention relates to the detection method of whitening and speckle dispelling composition in a kind of cosmetics and device, comprise the steps: cosmetics to be measured are added buffer salt solution, vibrate and extract to obtain corresponding extracting solution, the concentration of buffer salt solution is 0.01～0.03mol/L, and the buffer salt solution volume corresponding to every gram of cosmetics to be measured is 40～100mL；Extracting solution layering is taken supernatant, and filtering supernatant obtains extract solution；For mobile phase, extract solution is carried out chromatography with hydrophilic organic solvent and buffer salt solution and obtain chromatogram；Obtaining the content of whitening and speckle dispelling composition in cosmetics to be measured according to chromatogram and pre-rendered standard curve computing, standard curve is corresponding with magnesium L-ascorbyl-2-phosphate, kojic acid, hydroquinone, nicotiamide, Fructus Rubi glycosides, phenol, arbutin and glycyrrhizic acid dipotassium.The detection method of whitening and speckle dispelling composition and device in above-mentioned cosmetics, greatly improved simplification and the efficiency of detection.
Description
Technical field
The present invention relates to detection field, especially relate to detection method and the device of whitening and speckle dispelling composition in a kind of cosmetics.
Background technology
Development along with various skin-whitening Topical therapies, great majority employ more than one whitening and speckle dispelling composition for the cosmetics of skin-whitening, this is owing to a step of skin darkening is only played inhibitory action by a kind of whitening and speckle dispelling composition, needing links is control effectively so effectively to control skin darkening, namely " cooperative effect " whitening and speckle dispelling is theoretical.
The cross-reference of multiple whitening and speckle dispelling composition will also exist safety issue, and the particularly novel whitening and speckle dispelling composition appearance time is disorderly whole, lacks both effectiveness and malicious rational information reliably.It has been suggested that the cross-reference of whitening and speckle dispelling composition will disturb tyrosine in skin to convert to melanic normal enzyme with being excessively used, and then cause the untoward reaction of skin.Additionally, melanocyte in skin is had obvious cytotoxic effect by the whitening and speckle dispelling composition that overdose uses part novel.Bad businessman in market usually adopts disabled or low side whitening and speckle dispelling composition to pretend to be high-end whitening and speckle dispelling composition to add in cosmetics, and therefore, in cosmetics, the detection of whitening and speckle dispelling composition is particularly important.
Along with research deeply and cosmetics detection in the urgent need to, it is achieved cosmetics detect while multiple whitening and speckle dispelling composition.But at present the detection of whitening and speckle dispelling composition in cosmetics is focused primarily upon the whitening and speckle dispelling composition that detection is disabled, such as phenol, hydroquinone and kojic acid, also it is have small part to can be used for measuring arbutin, ascorbic acid and derivant thereof etc., and existing all whitening and speckle dispelling compositions cannot be detected, i.e. simultaneously magnesium L-ascorbyl-2-phosphate, kojic acid, hydroquinone, nicotiamide, Fructus Rubi glycosides, phenol, arbutin and glycyrrhizic acid dipotassium.
Summary of the invention
Based on this, it is necessary to provide one can detect existing all whitening and speckle dispelling compositions, i.e. the detection method of whitening and speckle dispelling composition in the cosmetics of magnesium L-ascorbyl-2-phosphate, kojic acid, hydroquinone, nicotiamide, Fructus Rubi glycosides, phenol, arbutin and glycyrrhizic acid dipotassium simultaneously.
Additionally, there is a need to provide one can detect existing all whitening and speckle dispelling compositions, i.e. the detecting device of whitening and speckle dispelling composition in the cosmetics of magnesium L-ascorbyl-2-phosphate, kojic acid, hydroquinone, nicotiamide, Fructus Rubi glycosides, phenol, arbutin and glycyrrhizic acid dipotassium simultaneously.
The detection method of whitening and speckle dispelling composition in a kind of cosmetics, comprise the steps: cosmetics to be measured are added buffer salt solution, vibrate and extract to obtain corresponding extracting solution, the concentration of described buffer salt solution is 0.01～0.03mol/L, and the buffer salt solution volume corresponding to every gram of cosmetics to be measured is 40～100mL；The layering of described extracting solution is taken supernatant, filters described supernatant and obtain extract solution；For mobile phase, described extract solution is carried out chromatography with hydrophilic organic solvent and buffer salt solution and obtain chromatogram；Obtaining the content of whitening and speckle dispelling composition in described cosmetics to be measured according to described chromatogram and pre-rendered standard curve computing, described standard curve is corresponding with magnesium L-ascorbyl-2-phosphate, kojic acid, hydroquinone, nicotiamide, Fructus Rubi glycosides, phenol, arbutin and glycyrrhizic acid dipotassium.
Wherein in an embodiment, described according to described chromatogram and pre-rendered standard curve computing obtain in described cosmetics to be measured before the step of the content of whitening and speckle dispelling composition, described method also includes: weigh magnesium L-ascorbyl-2-phosphate respectively, kojic acid, hydroquinone, nicotiamide, Fructus Rubi glycosides, phenol, arbutin and these eight kinds of whitenings of glycyrrhizic acid dipotassium are dispelled composition, its molecular weight is: magnesium L-ascorbyl-2-phosphate molecular weight 759.22, kojic acid molecular weight 142.11, hydroquinone molecular weight 110.11, nicotiamide molecular weight 122.13, Fructus Rubi glycosides molecular weight 326.33, phenol 94.11, arbutin molecular weight 272.25, glycyrrhizic acid dipotassium molecular weight 899.13；Dissolve described whitening and speckle dispelling composition respectively and obtain the standard reserving solution corresponding to each whitening and speckle dispelling composition with preparation；Pipette each 1～5mL of the standard reserving solution corresponding to magnesium L-ascorbyl-2-phosphate, nicotiamide and phenol, arbutin, hydroquinone, Fructus Rubi are sweet, each 2～10mL of standard reserving solution corresponding to glycyrrhizic acid dipotassium, and the standard reserving solution 3mL corresponding to kojic acid is to volumetric flask, and adopt described buffer salt solution constant volume, then stepwise dilution is to obtain the standard working solution of several concentration point；Respectively the standard working solution of each concentration point is carried out chromatography and obtain reference colour spectrogram；The standard curve obtained corresponding to each whitening and speckle dispelling composition is drawn by described reference colour spectrogram.
Wherein in an embodiment, described buffer salt solution is potassium dihydrogen phosphate.
Wherein in an embodiment, duration of oscillation is the 30-60 second.
Wherein in an embodiment, described in be extracted as supersound extraction, described extraction time is 15-25 minute.
Wherein in an embodiment, being layered as of extracting solution is centrifuged layering, and rotating speed is not less than 5000rpm, and centrifugation time is not less than 10 minutes, and described filtration adopts micropore water system membrane filtration, and the aperture of described micropore water system membrane filtration is not more than 0.45 micron.
Wherein in an embodiment, described mobile phase is methanol and potassium dihydrogen phosphate.
Wherein in an embodiment, described chromatography adopts high performance liquid chromatograph.
The detecting device of whitening and speckle dispelling composition in a kind of cosmetics, including: mechanical arm, cosmetics to be measured are added buffer salt solution, and the concentration of described buffer salt solution is 0.01～0.03mol/L, and the buffer salt solution volume corresponding to every gram of cosmetics to be measured is 40～100mL；Oscillator, concussion obtains extracting solution；Pipettor, extracts the supernatant of the described extracting solution of layering；Filter, filters described supernatant and obtains extract solution；The processor being connected with described mechanical arm, described oscillator, described pipettor, described filter respectively, for mobile phase, described extract solution is carried out chromatography with hydrophilic organic solvent and buffer salt solution and obtain chromatogram, described chromatogram and pre-rendered standard curve computing obtain the content of whitening and speckle dispelling composition in described cosmetics to be measured, and described standard curve is corresponding with magnesium L-ascorbyl-2-phosphate, kojic acid, hydroquinone, nicotiamide, Fructus Rubi glycosides, phenol, arbutin and glycyrrhizic acid dipotassium.
Wherein in an embodiment, also include: the gravity sensor being connected with described processor, weigh these the eight kinds of whitenings of magnesium L-ascorbyl-2-phosphate, kojic acid, hydroquinone, nicotiamide, Fructus Rubi glycosides, phenol, arbutin and glycyrrhizic acid dipotassium respectively to dispel composition, its molecular weight is: magnesium L-ascorbyl-2-phosphate molecular weight 759.22, kojic acid molecular weight 142.11, hydroquinone molecular weight 110.11, nicotiamide molecular weight 122.13, Fructus Rubi glycosides molecular weight 326.33, phenol 94.11, arbutin molecular weight 272.25, glycyrrhizic acid dipotassium molecular weight 899.13.
The detection method of whitening and speckle dispelling composition and device in above-mentioned cosmetics, cosmetics to be measured are added concentration is in the buffer salt solution that buffer salt solution volume is 100mL corresponding to 0.01～0.03mol/ and every gram of cosmetics to be measured, vibrate and extract and obtain corresponding extracting solution, extracting solution layering is taken supernatant, filter this supernatant and obtain extract solution, with hydrophilic organic solvent and buffer salt solution be the relative extract solution of mobile phase row chromatography obtain chromatogram, and then by with magnesium L-ascorbyl-2-phosphate, kojic acid, hydroquinone, nicotiamide, Fructus Rubi glycosides, phenol, the arbutin standard curve corresponding with glycyrrhizic acid dipotassium carries out computing and obtains the content of each whitening and speckle dispelling composition in cosmetics to be measured, achieve existing whitening and speckle dispelling composition, i.e. magnesium L-ascorbyl-2-phosphate, kojic acid, hydroquinone, nicotiamide, Fructus Rubi glycosides, phenol, detect while arbutin and glycyrrhizic acid dipotassium, simplification and the efficiency of detection are greatly improved.
Accompanying drawing explanation
Fig. 1 is the flow chart of the detection method of whitening and speckle dispelling composition in cosmetics in an embodiment；
Fig. 2 is the flow chart of the detection method of whitening and speckle dispelling composition in cosmetics in another embodiment；
Fig. 3 is the standard curve of magnesium L-ascorbyl-2-phosphate；
Fig. 4 is the standard curve of arbutin；
Fig. 5 is the standard curve of kojic acid；
Fig. 6 is the standard curve of hydrogen ester；
Fig. 7 is the standard curve of nicotiamide；
Fig. 8 is the standard curve of Fructus Rubi glycosides；
Fig. 9 is the standard curve of phenol；
Figure 10 is the standard curve of glycyrrhizic acid dipotassium；
The standard solution liquid chromatogram of eight kinds of whitening and speckle dispelling compositions that Figure 11 provides for embodiment one；
Figure 12 is liquid type cosmetics (bare substrate) liquid chromatogram in embodiment two cosmetics to be measured；
Figure 13 is cream kind cosmetics (bare substrate) liquid chromatogram in embodiment two cosmetics to be measured；
Figure 14 is gel-like cosmetics (bare substrate) liquid chromatogram in embodiment two cosmetics to be measured；
The liquid chromatogram of eight kinds of whitening and speckle dispelling compositions that Figure 15 is whitening emulsion in embodiment two cosmetics to be measured, solidifying white toner/smoothing toner is corresponding；
Figure 16 is the cosmetics moisturizing emulsion liquid chromatogram that embodiment three adds eight kinds of whitening and speckle dispelling compositions；
Figure 17 is the cosmetics whitening cream liquid chromatogram that embodiment three adds eight kinds of whitening and speckle dispelling compositions；
Figure 18 is the cosmetics whitening curry liquid chromatogram that embodiment three adds eight kinds of whitening and speckle dispelling compositions；
Figure 19 is 7 kinds of preservative and 8 kinds of whitening and speckle dispelling compositions reference colour spectrogram under same chromatographic condition in test two cosmetics to be measured；
Figure 20 be embodiment cosmetics cosmetics in the schematic diagram of detecting device of whitening and speckle dispelling composition.
Detailed description of the invention
Mainly in combination with specific embodiment, the detection method of whitening and speckle dispelling composition in cosmetics is described in further detail below.
As it is shown in figure 1, the detection method of whitening and speckle dispelling composition in the cosmetics of an embodiment, comprise the steps:
Cosmetics to be measured are added buffer salt solution by step 110, and vibration is also extracted to obtain corresponding extracting solution.
Step 130, takes supernatant by extracting solution layering, filters this supernatant and obtain extract solution.
Step 150, carries out chromatography for mobile phase to extract solution with hydrophilic organic solvent and buffer salt solution and obtains chromatogram.
Step 170, obtains the content of whitening and speckle dispelling composition in cosmetics to be measured according to chromatogram and pre-rendered standard curve computing.
The solution of this buffer salt solution is 0.01～0.03mol/L, and the buffer salt solution volume corresponding to every gram of cosmetics to be measured is 40～100mL, and the best is 100mL.In a preferred embodiment, this buffer salt solution is potassium dihydrogen phosphate.
Further, the duration of oscillation in step 110 is the 30-60 second, is extracted as supersound extraction, and extraction time is 15-25 minute.
Adopt potassium dihydrogen phosphate as Extraction solvent, its molar concentration is 0.02mol/L, pH=6.95, and supersound extraction 20min is conducive to cosmetics to be measured to be uniformly dispersed, can effectively extract these eight kinds of whitening and speckle dispelling compositions of magnesium L-ascorbyl-2-phosphate in cosmetics to be measured, kojic acid, hydroquinone, nicotiamide, Fructus Rubi glycosides, phenol, arbutin and glycyrrhizic acid dipotassium, and these eight kinds of whitening and speckle dispelling compositions can remain stable in a long time at this ph, being suitable for batch samples detection, in cosmetics to be measured, liposoluble substance is less is dissolved in extracting solution.
Further, in step 130, being layered as of extracting solution is centrifuged layering, and its rotating speed is not less than 5000rpm, and centrifugation time is not less than 10 minutes, filters and adopts micropore water system membrane filtration, and the aperture of micropore water system membrane filtration is not more than 0.45 micron.
Further, the mobile phase in step 150 is methanol and potassium dihydrogen phosphate, and wherein, the concentration of potassium dihydrogen phosphate is 0.02mol/L, pH=6.95.Chromatography adopts high performance liquid chromatograph.
Concrete, high performance liquid chromatograph adopts diode array detector, and its detection wavelength is 270nm, quantified by external standard method.
Gradient elution will be adopted when measuring extract liquid, its gradient elution program is: 0-8min, mass concentration is the methanol of 8%, 8-15min, being the methanol of 65% by the methanol that mass concentration is 8% to mass concentration, 15-18min, is the methanol of 8% by the methanol that mass concentration is 65% to mass concentration, 18-25min, mass concentration is the methanol of 8%.
Extract liquid and mobile phase initial strength be suitable, it is to avoid the Compound Retention time skew caused because sample solvent changes strength of mobile phase and peak stretching.
Adopting methanol and potassium dihydrogen phosphate during efficient liquid phase chromatographic analysis is mobile phase, gradient elution, diode array detector detects, its detection wavelength is 270nm, and eight kinds of whitening and speckle dispelling compositions separate good with this understanding, and analysis time is short, sensitivity is higher, therefore under the process of cosmetics to be measured and chromatographic condition, the appearance time of preservative common in cosmetics to be measured and these eight kinds of whitening and speckle dispelling composition appearance time non-overlappings, effectively eliminate the interference of all the other components in cosmetics to be measured.
Pre-rendered standard curve is corresponding with magnesium L-ascorbyl-2-phosphate, kojic acid, hydroquinone, nicotiamide, Fructus Rubi glycosides, phenol, arbutin and glycyrrhizic acid dipotassium.
The peak area of a certain whitening and speckle dispelling composition is analyzed by high performance liquid chromatograph, obtaining whitening and speckle dispelling composition kind contained in cosmetics to be measured and concentration with standard curve contrast, the film making then through sampling amount and extraction volume can obtain the content of whitening and speckle dispelling composition in cosmetics to be measured.
Wherein, the content of whitening and speckle dispelling composition in cosmetics to be measured can be obtained according to equation below calculating:
In formula: the content of a certain whitening anti-freckle agent in ω cosmetics, unit is milligrams per kilogram (g/kg)；
C is a certain whitening and speckle dispelling agent concentration from the liquid to be measured that standard curve obtains, and unit is milligrams per liter (mg/L)；
V sample constant volume, unit is milliliter (mL)；
The sampling amount of m sample, unit is gram (g).
In cosmetics as above in the detection method of whitening and speckle dispelling composition, the mensuration lower bound of each whitening and speckle dispelling composition is: 0.5g/kg (magnesium L-ascorbyl-2-phosphate, nicotiamide, phenol), 1.0g/kg (arbutin, hydroquinone, Fructus Rubi glycosides, glycyrrhizic acid dipotassium), 0.3g/kg (kojic acid).
Further, before step 170 as above, as in figure 2 it is shown, the method also comprises the steps:
Step 210, weigh these the eight kinds of whitenings of magnesium L-ascorbyl-2-phosphate, kojic acid, hydroquinone, nicotiamide, Fructus Rubi glycosides, phenol, arbutin and glycyrrhizic acid dipotassium respectively to dispel composition, wherein the mass ratio between each composition is: magnesium L-ascorbyl-2-phosphate molecular weight 759.22, kojic acid molecular weight 142.11, hydroquinone molecular weight 110.11, nicotiamide molecular weight 122.13, Fructus Rubi glycosides molecular weight 326.33, phenol 94.11, arbutin molecular weight 272.25, glycyrrhizic acid dipotassium molecular weight 899.13.
Step 230, dissolves whitening and speckle dispelling composition respectively and obtains the standard reserving solution corresponding to each whitening and speckle dispelling composition with preparation.
Step 250, pipettes each 1～5mL of the standard reserving solution corresponding to magnesium L-ascorbyl-2-phosphate, nicotiamide and phenol, and the best is 5mL；Arbutin, hydroquinone, Fructus Rubi are sweet, each 2～10mL of standard reserving solution corresponding to glycyrrhizic acid dipotassium, the best is 10mL, and the standard reserving solution 3mL corresponding to kojic acid is to volumetric flask, and adopt buffer salt solution constant volume, then stepwise dilution is to obtain the standard working solution of several concentration point.
Step 270, carries out chromatography to the standard working solution of each concentration point respectively and obtains reference colour spectrogram.
Step 290, is drawn the standard curve obtained corresponding to each whitening and speckle dispelling composition by reference colour spectrogram.
By the detection method of whitening and speckle dispelling composition in cosmetics as above and device, process simple, chromatograph interference is little, highly sensitive, analysis speed is fast, quickly can measure the whitening and speckle dispelling composition existed in cosmetics simultaneously, contribute to setting up the safe and sanitary of whitening and speckle dispelling product and functional component appraisement system, provide technical support for cosmetics quality supervision.
It is below specific embodiment part:
Embodiment one:
Set up eight kinds of whitening and speckle dispelling ingredient standard curves
Accurately weigh magnesium L-ascorbyl-2-phosphate (99.0%), kojic acid (99.9%), hydroquinone (99.0%), nicotiamide (99.9%), Fructus Rubi glycosides (99.1%), phenol (99.5%) each 200mg, arbutin (96.6%) 207mg, glycyrrhizic acid dipotassium (83.1%) 241mg, it is transferred to respectively in the volumetric flask of 100mL with after water dissolution, it is settled to scale, is configured to standard reserving solution.Pipette magnesium L-ascorbyl-2-phosphate, nicotiamide, each 5.0mL of phenol Standard storing solution respectively, arbutin, hydroquinone, Fructus Rubi glycosides, each 10.0mL of glycyrrhizic acid dipotassium standard reserving solution, in kojic acid standard reserving solution 3.0mL to 100mL volumetric flask, it is settled to scale with potassium dihydrogen phosphate (0.02mol/L, pH=6.95), then stepwise dilution is 5.0,10.0,20.0,50.0,100.0mg/L；10.0,20.0,50.0,100.0,200.0mg/L；The standard working solution of 3.0,6.0,15.0,30.0,60.0mg/L totally 5 concentration point.Take 10 μ L standard working solution to measure by high-efficient liquid phase chromatogram condition.
Liquid phase chromatogram condition
High performance liquid chromatograph, band diode array detector (Agilent1100 type, Agilent company of the U.S.)；
Chromatographic column: ZorbaxEclipseXDB-C18,250mm × 4.6mm, 5.0 μm；
Mobile phase: A potassium dihydrogen phosphate (0.02mol/L, pH=6.95)+B methanol；
Gradient elution: 0-8min, 8% methanol, 8-15min, by 8% methanol to 65% methanol, 15-18min, by 65% methanol to 8% methanol, 18-25min, 8% methanol；
Column temperature: 25 DEG C；
Flow velocity: 1.0mL/min；
Detection wavelength: 270nm,
Sample size: 10L.
With 8 kinds of whitening and speckle dispelling Component peak area (Y) for vertical coordinate, standard solution mass concentration (X, mg/L) is abscissa drawing standard working curve.8 kinds of whitening and speckle dispelling components regression equations are: y=11836.2x5.85 (magnesium L-ascorbyl-2-phosphate)；Y=2233.2x+1.60 (arbutin)；Y=25294.9x36.76 (kojic acid)；Y=4357.8x+4.23 (hydroquinone)；Y=10197.4x+2.31 (nicotiamide)；Y=1641.6x+0.56 (Fructus Rubi glycosides)；Y=8888.5x+0.56 (phenol)；Y=2941.0x+2.55 (glycyrrhizic acid dipotassium).8 kinds of whitening and speckle dispelling ingredient standard curve such as Fig. 3 are to shown in 10, and in standard curve concentration range, 8 kinds of whitening and speckle dispelling become partial correlation coefficient to be all higher than 0.999, in good linear relationship.The mensuration lower bound of 8 kinds of whitening and speckle dispelling compositions is: 0.5g/kg (magnesium L-ascorbyl-2-phosphate, nicotiamide, phenol), 1.0g/kg (arbutin, hydroquinone, Fructus Rubi glycosides, glycyrrhizic acid dipotassium), 0.3g/kg (kojic acid), fully meets 8 kinds of whitening and speckle dispelling composition detection requirements of cosmetics.
Embodiment two:
The detection of whitening and speckle dispelling composition in cosmetics
(1) sample pretreating
Take about 0.500g cosmetics to be measured in 50mL color-comparison tube, add 20mL potassium dihydrogen phosphate (0.02mol/L, pH=6.95), supersound extraction 20min, be transferred in 50mL volumetric flask, be settled to scale.Taking 10mL solution after mixing in 15mL centrifuge tube, centrifugal 10min under 12000r/min rotating speed, supernatant crosses 0.22 μm of filter membrane, and filtrate is extract solution, to be determined.Cosmetics to be measured are the kinds such as moisture retention water liquid, whitening cream, whitening curry, moisture saver mask.
(2) chromatographic condition
High performance liquid chromatograph, band diode array detector (Agilent1100 type, Agilent company of the U.S.)；
Chromatographic column: ZorbaxEclipseXDB-C18,250mm × 4.6mm, 5.0 μm；
Mobile phase: A potassium dihydrogen phosphate (0.02mol/L, pH=6.95)+B methanol；
Gradient elution: 0-8min, 8% methanol, 8-15min, by 8% methanol to 65% methanol, 15-18min, by 65% methanol to 8% methanol, 18-25min, 8% methanol；
Column temperature: 25 DEG C；
Flow velocity: 1.0mL/min；
Detection wavelength: 270nm,
Sample size: 10L.
(3) Specimen Determination
Take 10 μ L cosmetics product extract solutions to be measured to measure by high-efficient liquid phase chromatogram condition, record retention time and the peak area of chromatographic peak.
Eight kinds of whitening and speckle dispelling ingredient standard collection of illustrative plates are referring to accompanying drawing 11.As can be seen from the figure eight kinds of whitening and speckle dispelling composition appearance times successively are magnesium L-ascorbyl-2-phosphate (2.104min), arbutin (4.502min), kojic acid (4.778min), hydroquinone (6.404min), nicotiamide (7.092min), Fructus Rubi glycosides (15.574min), phenol (16.991min), glycyrrhizic acid dipotassium (18.403min).Accompanying drawing 12～14 is bare substrate sample moisture retention water liquid, whitening cream, whitening curry chromatograph collection of illustrative plates, does not all contain 8 kinds of whitening and speckle dispelling compositions.Accompanying drawing 15 is eight kinds of whitening and speckle dispelling ingredient standard collection of illustrative plates and sample whitening emulsion, solidifying white toner/smoothing toner chromatograph collection of illustrative plates, and cosmetics measurement result to be measured contains magnesium L-ascorbyl-2-phosphate, arbutin and glycyrrhizic acid dipotassium.
(4) result calculates
Bring the peak area treating cosmetics product extracting solution liquid chromatogram into standard curve in embodiment one to obtain treating the mass concentration of whitening and speckle dispelling composition in cosmetics, draw the content of a certain whitening anti-freckle agent in cosmetics according to formula calculated below:
In formula: the content of a certain whitening and speckle dispelling composition in ω cosmetics, unit is milligrams per kilogram (g/kg)；
C is a certain whitening and speckle dispelling constituent concentration from the liquid to be measured that standard curve obtains, and unit is milligrams per liter (mg/L)；
V cosmetics constant volume to be measured, unit is milliliter (mL)；
The sampling amount of m cosmetics to be measured, unit is gram (g).
Being computed, in certain cosmetics whitening emulsion to be measured, magnesium L-ascorbyl-2-phosphate content is 0.56g/kg；In solidifying white toner/smoothing toner, niacinamide content is 2.36g/kg, and glycyrrhizic acid dipotassium content is 1.03g/kg.
Embodiment three:
The detection of 8 kinds of whitening and speckle dispelling compositions in the cosmetics to be measured of the whitening and speckle dispelling composition of interpolation variable concentrations
(1) sample pretreating
Using liquid type, cream kind and the gel-like cosmetics to be measured of originating identical with embodiment two as bare substrate, preparation containing 1 times of detection lower bound, 2 times of detection lower bounds, 5 times of detection three variable concentrations of lower bound the cosmetic sample of whitening anti-freckle agent.
Accurately weigh about 0.500g cosmetics to be measured in 50mL color-comparison tube, add 20mL potassium dihydrogen phosphate (0.02mol/L, pH=6.95), supersound extraction 20min, be transferred in 50mL volumetric flask, be settled to scale.Taking 10mL solution after mixing in 15mL centrifuge tube, centrifugal 10min under 12000r/min rotating speed, supernatant crosses 0.22 μm of filter membrane, and filtrate is extract solution, to be determined.
(2) chromatographic condition
High performance liquid chromatograph, band diode array detector (Agilent1100 type, Agilent company of the U.S.)；
Chromatographic column: ZorbaxEclipseXDB-C18,250mm × 4.6mm, 5.0 μm；
Mobile phase: A potassium dihydrogen phosphate (0.02mol/L, pH=6.95)+B methanol；
Gradient elution: 0-8min, 8% methanol, 8-15min, by 8% methanol to 65% methanol, 15-18min, by 65% methanol to 8% methanol, 18-25min, 8% methanol；
Column temperature: 25 DEG C；
Flow velocity: 1.0mL/min；
Detection wavelength: 270nm,
Sample size: 10L.
(3) Specimen Determination
Take 10 μ L sample extract solutions to measure by high-efficient liquid phase chromatogram condition, record retention time and the peak area of chromatographic peak.
Accompanying drawing 16～18 respectively contains the moisture retention water liquid of the whitening and speckle dispelling composition of three concentration, whitening cream, whitening curry sample chromatogram figure.Contrast with accompanying drawing 11, add the cosmetic sample substrate to be measured of eight kinds of whitening and speckle dispelling compositions, all corresponding whitening and speckle dispelling composition detected at each self-corresponding appearance time.
(4) result calculates, to obtain the content of each whitening and speckle dispelling composition.
By by the effect of the detection method of whitening and speckle dispelling composition in these cosmetics of following experimental verification:
Test one:
The detection limit of eight kinds of whitening and speckle dispelling compositions, mensuration lower bound, the response rate and precision in cosmetics to be measured
Detection limit (Limitofdetection) refers to that certain particular analysis method is in Cmin or the minima that can detect test substance from sample.Calculating according to 4 times of signal to noise ratios (S/N), eight kinds of whitening and speckle dispelling compositions of this method are respectively as follows: vitamin magnesium phosphorate (1.6mg/L), arbutin (3.4mg/L), kojic acid (1.5mg/L), hydroquinone (3.4mg/L), nicotiamide (2.2mg/L), Fructus Rubi glycosides (3.5mg/L), phenol (1.0mg/L), glycyrrhizic acid dipotassium (3.2mg/L).Measure lower bound and refer to the lower limit for specific method and the detection by quantitative of sample.Standard curve range of linearity minimum point is the mensuration lower bound of eight kinds of whitening and speckle dispelling compositions: 0.5g/kg (magnesium L-ascorbyl-2-phosphate, nicotiamide, phenol), 1.0g/kg (arbutin, hydroquinone, Fructus Rubi glycosides, glycyrrhizic acid dipotassium), 0.3g/kg (kojic acid).
The cosmetics to be measured of the whitening and speckle dispelling composition detecting lower bound, 2 times of detection lower bounds, 5 times of detection three variable concentrations of lower bound containing 1 times of Example three preparation, every kind of cosmetics to be measured take 6 parts and carry out recovery testu, do blank experiment simultaneously, with the response rate more than 95% for standard；Precision refers under the test condition of regulation, same homogeneous sample, through repeatedly degree of closeness between sampling and measuring acquired results.Precision generally represents by relative standard deviation (RSD).Test result indicate that, each component average recovery rate scope is between 95%～110%, and relative standard deviation is between 0.22%～2.53%, and method recovery of standard addition, precision are in Table 1.
The table 1:8 kind whitening anti-freckle agent response rate and Precision Experiment (n=6)
Test two:
Interference experiment
Often adding various preservative in cosmetics and prolong the normal shelf-life, conventional preservative has: benzoic acid, benzyl alcohol, phenoxyethanol, P-hydroxybenzoic acid first, second, third, butyl ester.The detection of these 7 kinds of preservative also conventional water or methanol solution extract, and buffer salt carries out high performance liquid chromatography detection as mobile phase.Therefore investigated in an experiment and gone out peak situation under these 7 kinds of preservative chromatographic conditions of the present invention, prepared certain density 7 kinds of preservative hybrid standards, measure with 8 kinds of whitening and speckle dispelling composition agent simultaneously.Chromatogram is shown in Figure 19.Solid line peak is 8 kinds of compounds, and dotted line peak is preservative.7 kinds of preservative have peak between about 7.5min and 17-18min, and other times do not go out peak.By collection of illustrative plates it can be seen that the mensuration of 7 kinds of preservative retention times not jamming target compound in cosmetics.
Based on said method, in conjunction with accompanying drawing 20, there is a need to provide the detecting device of whitening and speckle dispelling composition in cosmetics, including: mechanical arm, oscillator, pipettor, filter and processor.Above-mentioned each device is placed and is supported on platform, and processor controls mechanical arm and captures cosmetics to be measured, and sends the vibration of order-driven agitator and obtain extracting solution；Processor controls pipettor according to predetermined instruction and extracts supernatant, and transmit to filter filtration, and obtaining extract solution, last processor gets chromatogram, obtain the content of whitening and speckle dispelling composition in cosmetics to be measured with pre-rendered standard curve computing simultaneously, complete detection.
Mechanical arm, adds buffer salt solution cosmetics to be measured, and the concentration of buffer salt solution is 0.01～0.03mol/L, and the buffer salt solution volume corresponding to every gram of cosmetics to be measured is 40～100mL；
Oscillator, concussion obtains extracting solution；
Pipettor, extracts the supernatant of the extracting solution of layering；
Filter, filtering supernatant obtains extract solution；
The processor being connected with mechanical arm, oscillator, pipettor, filter respectively, for mobile phase, extract solution is carried out chromatography with hydrophilic organic solvent and buffer salt solution and obtain chromatogram, chromatogram and pre-rendered standard curve computing obtain the content of whitening and speckle dispelling composition in cosmetics to be measured, and standard curve is corresponding with magnesium L-ascorbyl-2-phosphate, kojic acid, hydroquinone, nicotiamide, Fructus Rubi glycosides, phenol, arbutin and glycyrrhizic acid dipotassium.
Additionally, in cosmetics, the detecting device of whitening and speckle dispelling composition also includes: the gravity sensor being connected with described processor, weigh these the eight kinds of whitenings of magnesium L-ascorbyl-2-phosphate, kojic acid, hydroquinone, nicotiamide, Fructus Rubi glycosides, phenol, arbutin and glycyrrhizic acid dipotassium respectively to dispel composition, its molecular weight is: magnesium L-ascorbyl-2-phosphate molecular weight 759.22, kojic acid molecular weight 142.11, hydroquinone molecular weight 110.11, nicotiamide molecular weight 122.13, Fructus Rubi glycosides molecular weight 326.33, phenol 94.11, arbutin molecular weight 272.25, glycyrrhizic acid dipotassium molecular weight 899.13.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that, for the person of ordinary skill of the art, without departing from the inventive concept of the premise, it is also possible to making some deformation and improvement, these broadly fall into protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (1)
1. the detecting device of whitening and speckle dispelling composition in cosmetics, it is characterised in that including:
Mechanical arm, adds buffer salt solution cosmetics to be measured, and the concentration of described buffer salt solution is 0.01～0.03mol/L, and the buffer salt solution volume corresponding to every gram of cosmetics to be measured is 40～100mL；
Oscillator, concussion obtains extracting solution；
Pipettor, extracts the supernatant of the described extracting solution of layering；
Filter, filters described supernatant and obtains extract solution；
The processor being connected with described mechanical arm, described oscillator, described pipettor, described filter respectively, for mobile phase, described extract solution is carried out chromatography with hydrophilic organic solvent and buffer salt solution and obtain chromatogram, described chromatogram and pre-rendered standard curve computing obtain the content of whitening and speckle dispelling composition in described cosmetics to be measured, and described standard curve is corresponding with magnesium L-ascorbyl-2-phosphate, kojic acid, hydroquinone, nicotiamide, Fructus Rubi glycosides, phenol, arbutin and glycyrrhizic acid dipotassium；
Also include: the gravity sensor being connected with described processor, weigh these the eight kinds of whitenings of magnesium L-ascorbyl-2-phosphate, kojic acid, hydroquinone, nicotiamide, Fructus Rubi glycosides, phenol, arbutin and glycyrrhizic acid dipotassium respectively to dispel composition, its molecular weight is: magnesium L-ascorbyl-2-phosphate molecular weight 759.22, kojic acid molecular weight 142.11, hydroquinone molecular weight 110.11, nicotiamide molecular weight 122.13, Fructus Rubi glycosides molecular weight 326.33, phenol 94.11, arbutin molecular weight 272.25, glycyrrhizic acid dipotassium molecular weight 899.13；
Described mechanical arm, described oscillator, described pipettor and described filter are placed and are supported on platform, and described processor controls described mechanical arm and captures cosmetics to be measured, and described processor sends oscillator vibration described in order-driven and obtains extracting solution；Described processor controls described pipettor according to predetermined instruction and extracts supernatant, and transmit to the filtration of described filter, and obtain extract solution, last described processor gets described chromatogram, obtain the content of whitening and speckle dispelling composition in cosmetics to be measured with described pre-rendered standard curve computing simultaneously, complete detection.
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| CN106908356A (en) * | 2017-03-02 | 2017-06-30 | 深圳天祥质量技术服务有限公司 | The assay method of 1,4 Dihydroxybenzene migration amounts in a kind of non-stick pan sample |
| CN107727751A (en) * | 2017-10-09 | 2018-02-23 | 北京军秀咨询有限公司 | The detection method and device of whitening spot-removing composition in a kind of cosmetics |
| CN109115761A (en) * | 2018-11-15 | 2019-01-01 | 广州智汇生物科技有限公司 | The detection method of tranexamic acid in cosmetics |
| CN112684050A (en) * | 2020-12-24 | 2021-04-20 | 上海微谱检测技术有限公司 | Research on determination method of whitening functional components in cosmetics |
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