CN109725081A - Whether the discrimination method of Baical Skullcap root P.E is added in a kind of skin-care cosmetics - Google Patents
Whether the discrimination method of Baical Skullcap root P.E is added in a kind of skin-care cosmetics Download PDFInfo
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Abstract
The invention discloses the discrimination methods that Baical Skullcap root P.E whether is added in a kind of skin-care cosmetics.The following steps are included: using liquid chromatogram-level four bars-time-of-flight mass spectrometry (TOFMS), first use the radix scutellariae medicinal materials total ion chromatogram of full scan type collection separate sources different batches, parsing wherein shares and responds higher ingredient, determine common characteristic ingredient: scutelloside, wogonoside, baicalein and wogonin, using this 4 common characteristic ingredients as identification of indicator, and the cleavage of mass spectrum rule of this 4 common characteristic ingredients is studied, finally determine 8 characteristic ions of this 4 common characteristic ingredients；Detect cosmetic sample to be measured whether 8 characteristic ions containing this 4 characteristic components, to determine whether be added with Baical Skullcap root P.E.Method of the invention can be used to control and monitor the quality for being labeled with Baical Skullcap root P.E class cosmetics on cosmetics label.
Description
Technical field:
The invention belongs to analyze testing field, and in particular to whether add Baical Skullcap root P.E in a kind of skin-care cosmetics
Discrimination method.
Background technique:
Chinese herbal medicine is the treasure that China leaves, and Chinese herbal medicine class plant extracts is because having special efficacy, natural, nothing
It is malicious, without side-effects, using also more and more extensive in terms of cosmetics, many studies demonstrate that, in the Chinese herbal medicine of part containing it is anti-oxidant,
It removes free radical and nourishes crease-resistant isoreactivity ingredient.From ancient book Shennong's Herbal, " prescriptions worth thousand gold ", " medical secrets of official ", " herbal guiding principle
Mesh " etc. records discovery, now various Chinese herbal medicine beauty prescriptions all have outer feeding beauty functions for oral administration, by Chinese herbal medicine activity at
Divide extract to be properly applied in cosmetics, can achieve the effect that fine beauty.Radix scutellariae and its main chemical compositions baicalein
With scutelloside etc. have antibacterial, antimycotic, anti-inflammatory, antiallergy, it is anti-oxidant, remove free radical, uvioresistant, anti-radiation and inhibit
The bioactivity such as tyrosinase, it is more that numerous bioactivity makes collection freckle removing and whitening, sun-proof, antiallergic, anti-inflammatory and anti-aging
Imitate natural, efficient, the multifunctional cosmetics additive of unification.
With making rapid progress for science and technology, the development of current cosmetic field gradually tends to bioid and functionalization.It
Right functional cosmetics have complied with the trend and consumer psychology that people go back to nature." green " by be this century cosmetics master
Developing direction is wanted, visible on cosmetics major part label in the market to have " ×× extract ", addition Chinese medicine class natural products is opened
Hair cosmetics have formed world trends.But dazzling cosmetics are faced, how to identify in product whether be truly present this
A little natural materials are the problems wherein encountered, and the existing detection method about extract functional component, is high-efficient liquid phase color mostly
Spectrometry and tablets by HPLC-MS, and big multi-method is not fitted for Chinese medicine plant and drug products
The method that whether there is a certain Chinese herbal medicine in detection cosmetics is closed, in addition medicinal herb components are complicated, cannot be only according to a or two
Kind ingredient determines the presence of the Chinese medicine, brings difficulty to control of product quality because method is lacked, quality monitoring is also without related skill
Art support, brings opportunity to bad businessman is adulterated.Therefore, it needs to establish and be added specifically for plant in skin-care cosmetics
Object ingredient carries out mirror method for distinguishing.
Summary of the invention:
The purpose of the present invention is to overcome the defects in the prior art, provides in a kind of skin-care cosmetics whether add Huang
The discrimination method of a kind of reed mentioned in ancient books extract.
The purpose of the present invention is be achieved through the following technical solutions:
Whether the discrimination method of Baical Skullcap root P.E is added in skin-care cosmetics of the invention, comprising the following steps: including
Following steps: using liquid chromatogram-level four bars-time-of-flight mass spectrometry (TOFMS), first different using full scan type collection separate sources
The radix scutellariae medicinal materials total ion chromatogram of batch, parsing wherein share and respond higher ingredient, determine common characteristic ingredient: yellow
A kind of reed mentioned in ancient books glycosides, wogonoside, baicalein and wogonin using this 4 common characteristic ingredients as identification of indicator, and study this 4 altogether
Have the cleavage of mass spectrum rule of characteristic component, finally determine 8 characteristic ions of this 4 common characteristic ingredients: scutelloside it is female from
Sub- m/z 447.0922 and corresponding daughter ion m/z 271.0614, the parent ion m/z 461.1078 of wogonoside and corresponding
Daughter ion m/z 285.0764, the parent ion m/z 271.0601 of baicalein and corresponding daughter ion m/z 123.0081, the Chinese are yellow
The parent ion m/z 285.0757 of a kind of reed mentioned in ancient books element and corresponding daughter ion m/z 270.0520；By cosmetic sample to be measured using ultrasound extraction
Take-high speed centrifugation processing after, using object ion scan pattern, compare product with radix scutellariae medicinal materials, carry out liquid chromatogram-level Four
Bar-time-of-flight mass spectrometry (TOFMS) measurement, if 8 characteristic ions containing this 4 common characteristic ingredients in cosmetic sample to be measured,
And retention time is consistent with reference substance, is judged to containing Baical Skullcap root P.E in the cosmetic sample to be measured, if cosmetics to be measured
8 characteristic ions that this 4 common characteristic ingredients are not contained in sample, are judged to being not added with Baical Skullcap root P.E.
Liquid chromatogram-level four bars-time-of-flight mass spectrometry (TOFMS) liquid phase chromatogram condition is preferred are as follows: chromatographic column:
Poroshell C18, flow velocity 0.3mL/min, column temperature are 30 DEG C, 5 μ L of input；Mobile phase: A is acetonitrile, and B is containing volume fraction
The 10mmol/L formic acid aqueous ammonium of 10% methanol of 0.1% formic acid and volume fraction, gradient elution program: the ratio of mobile phase A:
0-1min, 0%A；1-2min, 0%A-10%A；2-4min, 10%A-40%A；4-8min, 40%A-80%A；8-10min,
80%A-100%A；10-15min, 100%A；18-22min, 0%A.
Liquid chromatogram-level four bars-time-of-flight mass spectrometry (TOFMS) Mass Spectrometry Conditions are preferred are as follows: instrument are as follows:
Agilent1290 HPLC-6540-Q-TOF-MS: ion source are as follows: the bis- sources spray Jet Stream Agilent, positive ion electrospray is from mould
Formula, dry 300 DEG C of temperature degree, atomization gas pressure 275.8kPa, dry gas stream speed 8L/min, 350 DEG C of sheath temperature degree, flow velocity 11L/
Min, capillary voltage 3000V, capillary outlet voltage 120V, orifice potential 65V, octupole bar voltage 750V, scanning range m/
z100-1100；Reference ion cation are as follows: m/z121.0509,922.0098.
The present invention is using Baical Skullcap root P.E as object, by selecting contain in radix scutellariae medicinal materials four characteristic components as index
Ingredient, to identify the presence of Baical Skullcap root P.E in cosmetics, the high resolution mass spectrum of use has high quality accuracy and selectivity,
Greatly improve the accuracy of Qualitive test, the identification mark ingredient that can be simple and efficient, this method can be used to control and
The quality of Baical Skullcap root P.E class cosmetics is labeled on monitoring cosmetics label.
Chinese medicine often contained complex chemical composition, not ready-made measurement and judgment method, we have studied separate sources
Different batches radix scutellariae medicinal materials are made extract with water extraction and water extraction and alcohol precipitation method, are then tied with liquid chromatography-mass spectrography (LC-MS)
Chemical component therein is analyzed in the methods of synkaryon magnetic resonance (NMR), is had found shared ingredient, can be represented radix scutellariae medicinal materials, the area Ye Neng
Not in other similar medicinal material.
Compared with the prior art, the invention has the following advantages:
1) still can determine whether contain Baical Skullcap root P.E in skin-care cosmetics without detection method at present, headed by this method
Whether contain Baical Skullcap root P.E method in wound measurement cosmetics；
2) prior art generally use liquid chromatogram UV detector measurement skin-care cosmetics in Baical Skullcap root P.E at
Point, there is interference greatly, detection limit does not reach requirement, and causes result inaccuracy sensitivity not high.The method of the present invention uses liquid phase color
Spectrum-high resolution mass spectrum acquires data, obtains object ion total ion current figure (TIC), then with ion (EIC) processing is extracted, greatly
The selectivity and accuracy for the qualitative, quantitative that ground improves, the identification mark ingredient that can be simple and efficient, Monitoring lower-cut reach
0.1mg/kg。
3) the method for the present invention selects four kinds of property materials in scullcap plant as Judging index, and characteristic is strong, can be anti-
Reflect in product whether the truth containing the plant extracts, method solves whether really add in skin-care cosmetics
The problem of Baical Skullcap root P.E identification.
Detailed description of the invention:
Fig. 1 is Baical Skullcap root P.E total ion chromatogram.
Fig. 2 is Baical Skullcap root P.E characteristic ion figure.
Fig. 3 is Baical Skullcap root P.E characteristic ion figure in cosmetics.
Specific embodiment:
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Embodiment 1: characteristic component is selected
1, laboratory apparatus, main material and reagent
Agilent1290 HPLC-6540-Q-TOF-MS (Agilent company of the U.S.) is furnished with double-jet aeration electron spray ion
Source；The desk-top mechanical ultrasonic cleaner (Dongguan City ultrasonic equipment Co., Ltd) of KQ2200 type, Sai Duolisi TP-114 electronics
Balance (Sartorious company, the U.S.), Allegra 64R high speed freezing centrifuge (Beckman company), MS3 basic whirlpool
Mixer (German IKA company).Separate sources radix scutellariae medicinal materials, wherein tri- parts of A, B, C are to buy by oneself on the net, and D is purchased from great Can woods pharmacy,
E is purchased from Neptune occasion pharmacy, and F is purchased from extra large two paradise pharmacies, and 3 two parts of G, H, I are purchased from the peaceful medicinal material market in Guangzhou), it is identified equal
For radix scutellariae medicinal materials.Methanol, ethyl alcohol, acetonitrile are chromatography pure reagent (German Merck company), and water is secondary distilled water, ammonium formate and
Formic acid (Aladdin reagent).
2, sample pre-treatments
Radix scutellariae medicinal materials 0.1g is accurately weighed, is placed in 10mL volumetric flask, 80% methanol solution of volume fraction is added and is settled to
Scale, ultrasonic extraction 20min, filtering obtain the Baical Skullcap root P.E of 10mg/mL, to be measured.
3, liquid phase chromatogram condition
Chromatographic column: Poroshell C18 (2.1mm × 50mm, 2.7 μm), mobile phase: A is acetonitrile, and B is 10mmol/L first
Sour ammonium (0.1% formic acid containing volume fraction, 10% methanol of volume fraction) aqueous solution, gradient elution program: the ratio of mobile phase A:
0-1min, 0%A；1-2min, 0%A-10%A；2-4min, 10%A-40%A；4-8min, 40%A-80%A；8-10min,
80%A-100%A；10-15min, 100%A；18-22min, 0%A.Flow velocity 0.3mL/min, column temperature are 30 DEG C, 5 μ L of input.
4, Mass Spectrometry Conditions
Instrument are as follows: Agilent1290 HPLC-6540-Q-TOF-MS (Agilent company of the U.S.): ion source are as follows:
The bis- sources spray Jet Stream Agilent (Dual Jet Stream ESI), positive ion electrospray is from mode, dry gas (N2) temperature 300
DEG C, atomization gas (N2) pressure 275.8kPa, dry gas (N2) flow velocity 8L/min, 350 DEG C, flow velocity 11L/min of sheath temperature degree, capillary
Tube voltage 3000V, capillary outlet voltage (fragmentor) 120V, orifice potential (skimmer) 65V, octupole bar voltage
750V, scanning range m/z100-1100；Reference ion cation are as follows: m/z121.0509,922.0098.
5, LC-Q-TOF-MS is measured
It is yellow using full scan type collection using liquid chromatogram-level four bars-flight time mass spectrum (LC-Q-TOF-MS) method
Total ion chromatogram (TIC) (see figure 1) of a kind of reed mentioned in ancient books extract, obtains the total ion current of nine parts of radix scutellariae medicinal materials (sample A-I)
Chromatogram, then instrument Masshunter work station analyzing and processing data is used, the response analyzed in total ion chromatogram is higher
Shared ion, and retrieve the molecular formula of shared ion, find the compound that shared ion is belonged to, determine common characteristic at
Point: scutelloside, wogonoside, baicalein and wogonin, characteristic component is high-visible (see Fig. 2) after extracted ion processing,
Wherein wogonoside and wogonin contain a pair of of isomer respectively.Using this 4 common characteristic ingredients as identification of indicator,
And the cleavage of mass spectrum rule of this 4 common characteristic ingredients is studied, finally determine 8 characteristic ions of this 4 common characteristic ingredients:
The parent ion m/z of the parent ion m/z 447.0922 of scutelloside and corresponding daughter ion m/z 271.0614, wogonoside
The parent ion m/z 271.0601 and corresponding daughter ion m/ of 461.1078 and corresponding daughter ion m/z 285.0764, baicalein
The parent ion m/z 285.0757 and corresponding daughter ion m/z 270.0520 (being shown in Table 1) of z 123.0081, wogonin.
14 characteristic component Information in Mass Spectra of table
| Serial number | Components Name | No. CAS | Retention time/min | Molecular formula | Molecular weight | Quasi-molecular ion | Secondary fragment daughter ion |
| 1 | Scutelloside | 21967-41-9 | 5.9 | C21H18O11 | 446.0846 | 447.0922 | 271.0614 |
| 2 | Wogonoside | 51059-44-0 | 6.7 | C22H20O11 | 460.1002 | 461.1078 | 285.0764 |
| 3 | Baicalein | 491-67-8 | 8.5 | C15H10O5 | 270.0525 | 271.0601 | 123.0081 |
| 4 | Wogonin | 632-85-9 | 10.4 | C6H12O5 | 284.0681 | 285.0757 | 270.0520 |
Embodiment 2: whether Baical Skullcap root P.E is added in identification " ×× board SPA is reluctant to part microscopic carvings Face-protecting mask "
This product label ingredient are as follows: water, butanediol, glycerol, β-polydextrose, Natrulon H-10, PEG-12 methyl polysilicone
Alkane, PPG-20 cross-linked polymer, bermuda lily flower extract, Gotu Kola P.E, Gentrin Knotweed P.E, radix scutellariae root extract etc.
Totally 23 ingredients.To the product, using ultrasonic extraction-high speed centrifugation processing, and liquid chromatogram-level four bars-flight time is combined
Mass spectrum (LC-Q-TOF-MS) technology identifies in cosmetics whether add Baical Skullcap root P.E, and concrete scheme is as follows: one, experiment instrument
Device and device
Agilent1290 HPLC-6540-Q-TOF-MS (Agilent company of the U.S.) is furnished with double-jet aeration electron spray ion
Source；The desk-top mechanical ultrasonic cleaner (Dongguan City ultrasonic equipment Co., Ltd) of KQ2200 type, Sai Duolisi TP-114 electronics
Balance (Sartorious company, the U.S.), Allegra 64R high speed freezing centrifuge (Beckman company), MS3basic whirlpool
Mixer (German IKA company).
Two, main material and reagent
Standard items: radix scutellariae control medicinal material, scutelloside are purchased from National Institute for Food and Drugs Control.Methanol, ethyl alcohol, acetonitrile
For chromatography pure reagent (German Merck company), water is secondary distilled water, ammonium formate and formic acid (Aladdin reagent).
Three, experimental method
1, the preparation of sample solution
2g (being accurate to 0.001g) sample is accurately weighed, in 25mL color-comparison tube, addition 5mL water, 2 grams of sodium chloride,
It is placed in vortex oscillator and is uniformly mixed, add methanol constant volume to scale, ultrasonic extraction 20min obtains extracting solution and all turns
Enter in 50mL centrifuge tube, 10000r/min is centrifuged 5min, crosses 0.45 μm of filter membrane, obtains sample solution, to be measured.
2, the preparation of reference substance solution
Scutelloside standard items 5.0mg (being accurate to 0.01mg) is weighed in 10mL volumetric flask, with 80% methanol of volume fraction
Solution dissolution and constant volume, are made into the standard reserving solution of 0.5mg/mL.Facing the used time with 80% methanol solution of volume fraction is configured to institute
Serial hybrid standard working solution is needed, 4 DEG C are kept in dark place.Radix scutellariae control medicinal material 0.1g is weighed, is placed in 10mL volumetric flask, is added
80% methanol solution of volume fraction is settled to scale, ultrasonic extraction 20min, and filtering obtains the (control of 10mg/mL radix scutellariae extracting solution
Product solution), then dilute to obtain 10,1,0.1mg/L reference substance solution, it is to be measured.
3, it detects
Respectively by above-mentioned sample solution and reference substance solution liquid chromatogram-level four bars-flight time mass spectrum (LC-Q-
TOF-MS) method is measured.The total ion chromatogram (TIC) of sample is collected using object ion scan pattern, is extracted
Object ion obtain object ion EIC figure (see Fig. 3), this 4 features of scutelloside, wogonoside, baicalein and wogonin at
The parent ion and corresponding daughter ion divided is shown in Table 1.Final Baical Skullcap root P.E content is counted by index of scutelloside, i.e., with radix scutellariae
Glycosides is standard specimen, extracts the peak area that scutelloside quasi-molecular ion (m/z447.0922) is obtained, and external standard method is calculated.Chromatography and
Mass Spectrometry Conditions are as follows:
3.1 chromatographic condition
Chromatographic column: Poroshell C18 (2.1mm × 50mm, 2.7 μm), mobile phase: A is acetonitrile, and B is 10mmol/L first
Sour ammonium (0.1% formic acid containing volume fraction, 10% methanol of volume fraction) aqueous solution, gradient elution, the ratio of mobile phase A: 0-
1min, 0%A；1-2min, 0%A-10%A；2-4min, 10%A-40%A；4-8min, 40%A-80%A；8-10min,
80%A-100%A；10-15min, 100%A；18-22min, 0%A.Flow velocity 0.3mL/min, column temperature are 30 DEG C, 5 μ L of input.
3.2 Mass Spectrometry Conditions
Instrument are as follows: Agilent1290 HPLC-6540-Q-TOF-MS (Agilent company of the U.S.): ion source are as follows:
The bis- sources spray Jet Stream Agilent (Dual Jet Stream ESI), positive ion electrospray is from mode, dry gas (N2) temperature 300
DEG C, atomization gas (N2) pressure 275.8kPa, dry gas (N2) flow velocity 8L/min, 350 DEG C, flow velocity 11L/min of sheath temperature degree, capillary
Tube voltage 3000V, capillary outlet voltage (fragmentor) 120V, orifice potential (skimmer) 65V, octupole bar voltage
750V, scanning range m/z100-1100；Reference ion cation are as follows: m/z121.0509,922.0098.
4, linearly with method detection limit
Use a kind of film sample extracting solution without Baical Skullcap root P.E for solvent, preparing scutelloside mass concentration is
0.001, the series standard working solution of 0.005,0.01,0.025,0.05,0.1,0.25,0.50,1.0,2.5,5.0mg/L,
Under the present embodiment experiment condition, scutelloside is quantified, it is dense with scutelloside quasi-molecular ion peak area (Y) and corresponding quality
Spend (X, μ gmL-1) response relation, obtain equation of linear regression and related coefficient.
5, the method rate of recovery and precision
Using blank facial mask as mark-on matrix, by the present embodiment experimental condition carry out it is basic, normal, high (0.05,0.1,
1.0mg/L) three pitch-based spheres, each horizontal parallel measure 6 times, calculate recovery of standard addition and precision.
6, the measurement of actual sample
The qualitative and quantitative detection of four kinds of common characteristic ingredients is carried out to the product using the present embodiment method.
Four, measurement result
1, measurement obtains the linear equation of scutelloside are as follows: Y=49108X+387.3, correlation coefficient r 0.9994,
Linear good in the range of 0.05-2.5mg/L, standard solution detection is limited to 0.025mg/L, and the detection in sample is limited to 0.1mg/
kg.It is 89.6% that 6 times, which measure obtained average recovery of standard addition, and precision is less than 6.9%.
2, the EIC figure of reference substance and sample is compared, scutelloside, wogonoside, baicalein and the Chinese is not detected in sample
These four characteristic components of baicalein, therefore, it is determined that being not added with Baical Skullcap root P.E in the cosmetics.
Embodiment 3: whether Baical Skullcap root P.E is added in identification " the fresh and alive bright vigor frost that shines of ×× board oriental cherry energy "
The present embodiment, which is indicated with " ×× board oriental cherry energy is fresh and alive shine bright vigor frost " for object, in label, that " radix scutellariae mentions
Take object ".
Its concrete scheme is as follows:
One, laboratory apparatus and device
Agilent1290 HPLC-6540-Q-TOF-MS (Agilent company of the U.S.) is furnished with double-jet aeration electron spray ion
Source；The desk-top mechanical ultrasonic cleaner (Dongguan City ultrasonic equipment Co., Ltd) of KQ2200 type, Sai Duolisi TP-114 electronics
Balance (Sartorious company, the U.S.), Allegra 64R high speed freezing centrifuge (Beckman company), MS3 basic whirlpool
Mixer (German IKA company).
Two, main material and reagent
Standard items: radix scutellariae control medicinal material, scutelloside are purchased from National Institute for Food and Drugs Control.Methanol, ethyl alcohol, acetonitrile
For chromatography pure reagent (German Merck company), water is secondary distilled water, ammonium formate and formic acid (Aladdin reagent).
Three, experimental method
1, the preparation of sample solution
2g (being accurate to 0.001g) sample is accurately weighed, in 25mL color-comparison tube, addition 5mL water, 2 grams of sodium chloride,
It is placed in vortex oscillator and is uniformly mixed, add methanol constant volume to scale, ultrasonic extraction 20min obtains extracting solution and all turns
Enter in 50mL centrifuge tube, 10000r/min is centrifuged 5min, crosses 0.45 μm of filter membrane, obtains sample solution, to be measured.
2, the preparation of reference substance solution
Scutelloside standard items 5.0mg (being accurate to 0.01mg) is weighed in 10mL volumetric flask, with 80% methanol of volume fraction
Solution dissolution and constant volume, are made into the standard reserving solution of 0.5mg/mL.Facing the used time with 80% methanol solution of volume fraction is configured to institute
Serial hybrid standard working solution is needed, 4 DEG C are kept in dark place.Radix scutellariae control medicinal material 0.1g is weighed, is placed in 10mL volumetric flask, is added
80% methanol solution of volume fraction is settled to scale, ultrasonic extraction 20min, and filtering obtains the (control of 10mg/mL radix scutellariae extracting solution
Product solution), it is to be measured.
3, it detects
Respectively by above-mentioned sample solution and reference substance solution liquid chromatogram-level four bars-flight time mass spectrum (LC-Q-
TOF-MS) method is measured.The total ion chromatogram (TIC) of sample is collected using object ion scan pattern, is extracted
Object ion obtains object ion EIC figure, this 4 characteristic components of scutelloside, wogonoside, baicalein and wogonin it is female from
Sub and corresponding daughter ion is shown in Table 1.Final Baical Skullcap root P.E content is counted by index of scutelloside, i.e., is mark with scutelloside
Sample, extracts the peak area that scutelloside quasi-molecular ion (m/z447.0922) is obtained, and external standard method is calculated.Chromatography and mass spectrum item
Part is as follows: 3.1 chromatographic conditions
Chromatographic column: Poroshell C18 (2.1mm × 50mm, 2.7 μm), mobile phase: A is acetonitrile, and B is 10mmol/L first
Sour ammonium (0.1% formic acid containing volume fraction, 10% methanol of volume fraction) aqueous solution, gradient elution, the ratio of mobile phase A: 0-
1min, 0%A；1-2min, 0%A-10%A；2-4min, 10%A-40%A；4-8min, 40%A-80%A；8-10min,
80%A-100%A；10-15min, 100%A；18-22min, 0%A.Flow velocity 0.3mL/min, column temperature are 30 DEG C, 5 μ L of input.
3.2 Mass Spectrometry Conditions
Instrument are as follows: Agilent1290 HPLC-6540-Q-TOF-MS (Agilent company of the U.S.): ion source are as follows:
The bis- sources spray Jet Stream Agilent (Dual Jet Stream ESI), positive ion electrospray is from mode, dry gas (N2) temperature 300
DEG C, atomization gas (N2) pressure 275.8kPa, dry gas (N2) flow velocity 8L/min, 350 DEG C, flow velocity 11L/min of sheath temperature degree, capillary
Tube voltage 3000V, capillary outlet voltage (fragmentor) 120V, orifice potential (skimmer) 65V, octupole bar voltage
750V, scanning range m/z100-1100；Reference ion cation are as follows: m/z121.0509,922.0098.
Four, measurement result
The EIC figure of reference substance and sample is compared (Qualitative Identification), sample contains scutelloside, wogonoside, baicalein
With the parent ion and corresponding daughter ion of wogonin this 4 kinds of characteristic components, and retention time is consistent with reference substance.Quantitative result
Content is 0.50mg/kg in terms of scutelloside, therefore, it is determined that there is addition Baical Skullcap root P.E in the cosmetics.
2 are shown in Table applied to Baical Skullcap root P.E test result in more cosmetics:
Baical Skullcap root P.E test result in the different cosmetics of table 2
Claims (3)
1. whether adding the discrimination method of Baical Skullcap root P.E in a kind of skin-care cosmetics, which comprises the following steps:
Using liquid chromatogram-level four bars-time-of-flight mass spectrometry (TOFMS), the radix scutellariae of full scan type collection separate sources different batches is first used
Medicinal material total ion chromatogram, parsing wherein share and respond higher ingredient, and determine common characteristic ingredient: scutelloside, the Chinese are yellow
A kind of reed mentioned in ancient books glycosides, baicalein and wogonin using this 4 common characteristic ingredients as identification of indicator, and study this 4 common characteristic ingredients
Cleavage of mass spectrum rule, finally determine 8 characteristic ions of this 4 common characteristic ingredients: the parent ion m/z of scutelloside
The parent ion m/z 461.1078 and corresponding daughter ion of 447.0922 and corresponding daughter ion m/z 271.0614, wogonoside
M/z 285.0764, the parent ion m/z 271.0601 of baicalein and corresponding daughter ion m/z 123.0081, wogonin
Parent ion m/z 285.0757 and corresponding daughter ion m/z 270.0520；Cosmetic sample to be measured is used into ultrasonic extraction-height
After fast centrifugal treating, using object ion scan pattern, product is compared with radix scutellariae medicinal materials, carry out liquid chromatogram-level four bars-flight
The measurement of time mass spectrum method, if 8 characteristic ions containing this 4 common characteristic ingredients in cosmetic sample to be measured, and retain
Time is consistent with reference substance, is judged to containing Baical Skullcap root P.E in the cosmetic sample to be measured, if in cosmetic sample to be measured
8 characteristic ions without containing this 4 common characteristic ingredients, are judged to being not added with Baical Skullcap root P.E.
2. discrimination method according to claim 1, which is characterized in that the liquid chromatogram-level four bars-flight time matter
The liquid phase chromatogram condition of spectrometry are as follows: chromatographic column: Poroshell C18, flow velocity 0.3mL/min, column temperature are 30 DEG C, 5 μ L of input；Stream
Dynamic phase: A is acetonitrile, and B is the 10mmol/L formic acid aqueous ammonium containing 10% methanol of 0.1% formic acid of volume fraction and volume fraction,
Gradient elution, the ratio of mobile phase A: 0-1min, 0%A；1-2min, 0%A-10%A；2-4min, 10%A-40%A；4-
8min, 40%A-80%A；8-10min, 80%A-100%A；10-15min, 100%A；18-22min, 0%A.
3. discrimination method according to claim 1, which is characterized in that the liquid chromatogram-level four bars-flight time matter
The Mass Spectrometry Conditions of spectrometry are as follows: instrument are as follows: Agilent1290HPLC-6540-Q-TOF-MS: ion source are as follows: the bis- spray Jet of Agilent
The source Stream, positive ion electrospray is from mode, dry 300 DEG C of temperature degree, atomization gas pressure 275.8kPa, dry gas stream speed 8L/min,
350 DEG C, flow velocity 11L/min, capillary voltage 3000V of sheath temperature degree, capillary outlet voltage 120V, orifice potential 65V, octupole
Bar voltage 750V, scanning range m/z100-1100；Reference ion cation are as follows: m/z121.0509,922.0098.
Priority Applications (1)
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