CN107389831A - The quick determination method of banned substance oestrone in a kind of spraying cosmetics - Google Patents
The quick determination method of banned substance oestrone in a kind of spraying cosmetics Download PDFInfo
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- CN107389831A CN107389831A CN201710881259.5A CN201710881259A CN107389831A CN 107389831 A CN107389831 A CN 107389831A CN 201710881259 A CN201710881259 A CN 201710881259A CN 107389831 A CN107389831 A CN 107389831A
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- oestrone
- way pipe
- determination method
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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Abstract
The invention discloses a kind of quick determination method of banned substance oestrone in cosmetics of spraying, comprise the following steps：Step 1: make the double threeway capillary pipe spray devices of open type；Step 2: the double threeway capillary pipe spray devices of the open type are placed at mass spectrometric 3~4cm of sample inlet front end, mass spectrometric parameter is set, presses the aerosol valve of the sample bottle, obtains mass spectrum response signal；Step 3: to improve the response of analyte, derivatization reagent is introduced by syringe pump, atomization gas dispels atomized drop, and end spaces mixes with sample before the capillary pipe spray pipe, improves the mass spectrum response signal of test substance.The method of the present invention is simple, quickly, the quick detection of banned substance oestrone suitable for the spraying cosmetics of field quick detection.
Description
Technical field
It is female more particularly to banned substance in one kind spraying cosmetics the present invention relates to a kind of detection method of chemical substance
The quick determination method of ketone.
Background technology
Spray product is to use extensive product during we live.Its product type mainly has two classes：One kind is by bottle
Interior gas provides the aerodynamic force spray product of spraying power, is also aerosol product, and a kind of in addition is by (manual) pressing of external force
The spray product of power is provided, is commonly called as pressing spray product.Product category is rich and varied, such as：The insecticide of agricultural and family expenses, head
The hair dyeing spraying of hair dyeing, spraying cosmetics, the medicinal herb spray etc. of traumatic injury of use in personal care.These products are in life
While offer facility living, also exist to human body and environment potentially hazardous.Spray product can play its effect mainly due to
Product contains specific chemical efficiency composition.However, in order to increase its effect, illegal businessman, which may illegally add some, to be had
The unauthorized substances of identical effect.In use, due to these products of inferior quality containing poisonous and harmful substance can by skin contact,
The modes such as eye contact, suction enter in human body, and the symptom such as caused dizziness, Nausea and vomiting, allergy, grave danger human body is good for
Health.China《Cosmetics safety technical specification》(version in 2015) and European Union cosmetics regulation (EC 1223/2009) clear stipulaties are female
Ketone is banned substance in cosmetics.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of convenient, efficient, suitable for the atomization of field quick detection
The method of banned substance oestrone in cosmetic.
The quick determination method of banned substance oestrone, comprises the following steps in a kind of spraying cosmetics：
Step 1: make the double threeway capillary pipe spray devices of open type；
The double threeway capillary pipe spray devices of the open type include the first three-way pipe and the second three-way pipe of series connection, in level
Side is upwardly formed sample channel, and capillary pipe spray pipe, the rear end of the capillary pipe spray pipe are provided with the sample channel
It is connected with one end of isocon, front end is arranged in the sample channel, close to the right-hand member of second three-way pipe, with described the
Form blending space between the right-hand member of two three-way pipes, the other end of the isocon by pipeline respectively with sample bottle and waste liquid bottle
It is connected, first three-way pipe provides device with gas by pipeline and is connected, and second three-way pipe passes through pipeline and syringe pump
It is connected, mass spectrograph is provided with the right side of second three-way pipe；
Step 2: the double threeway capillary pipe spray devices of the open type are placed in mass spectrometric 3~4cm of sample inlet front end
Place, sets the mass spectrometric parameter to be：Positive ion mode, capillary voltage 4kV；The air pressure for setting gas offer device is 30psi；
The aerosol valve of the sample bottle is pressed, obtains mass spectrum response signal；
Step 3: improve the response of analysans
The syringe pump introduces liquid, and fltting speed is 20 μ L/min, and atomization gas dispels atomized drop, in the capillary
End spaces mixes with sample before injection spray pipe, improves the mass spectrum response signal of test substance.
The quick determination method of banned substance oestrone in spraying cosmetics of the present invention, wherein, the nebulised sample
For cosmetics of spraying.
The quick determination method of banned substance oestrone in spraying cosmetics of the present invention, wherein, the matter of test substance
Spectrum information is as shown in table 1.
The Information in Mass Spectra of the test substance of table 1
The quick determination method of banned substance oestrone in spraying cosmetics of the present invention, wherein, first threeway
Pipe and second three-way pipe include horizontal tube and VERTICAL TUBE, and the left end of the horizontal tube of first three-way pipe uses stator
Closing, right-hand member are connected with the left end of the horizontal tube of second three-way pipe, and through hole, the capillary are provided with the stator
The rear end of pipe injection spray pipe passes from the through hole, is connected with the isocon.
The quick determination method of banned substance oestrone in spraying cosmetics of the present invention, wherein, first threeway
The VERTICAL TUBE of pipe provides device by pipeline and the gas and is connected, the VERTICAL TUBE of second three-way pipe by pipeline with it is described
Syringe pump is connected.
The quick determination method of banned substance oestrone in spraying cosmetics of the present invention, wherein, first threeway
The interface of pipe and second three-way pipe is 1/8 inch or 1/16 inch；The internal diameter of the capillary pipe spray pipe is 10~200 μ
m。
The quick determination method of banned substance oestrone in spraying cosmetics of the present invention, wherein, the capillary spray
The front end of mist pipe is arranged in second three-way pipe, and the distance between right-hand member of horizontal tube of second three-way pipe is 1
~3cm.
The quick determination method of banned substance oestrone in spraying cosmetics of the present invention, wherein, in the isocon
On be provided with flow control valve.
The quick determination method of banned substance oestrone in spraying cosmetics of the present invention, wherein, the syringe pump draws
The liquid entered is methoxamine derivatization reagent.
The quick determination method difference from prior art of banned substance oestrone is in present invention spraying cosmetics：
The quick determination method of banned substance oestrone establishes a kind of double threeway capillary sprays in present invention spraying cosmetics
The detection method of banned substance oestrone in mist tandem ion-trap mass spectrum rapid screening spraying cosmetics, this method is convenient, efficient, fits
For field quick detection.
The quick determination method of banned substance oestrone is innovative in present invention spraying cosmetics and advantage is：
1st, present invention firstly provides the method for double threeway capillary pipe spray tandem mass spectrums, quick detection to spray in cosmetics
Banned substance oestrone.
2nd, the present invention is applied to the inspection using double threeway capillary pipe spray tandem mass spectrum detection spray product banned substances
Survey method, the response of oestrone is improved by introducing derivatization reagent, and the detection of oestrone is limited to 50 μ g/kg.
3rd, the present invention is without using Extraction solvent.
The quick determination method of banned substance oestrone is made further in the spraying cosmetics to the present invention below in conjunction with the accompanying drawings
Explanation.
Brief description of the drawings
Fig. 1 is the structural representation of the double threeway capillary pipe spray devices of open type in the present invention；
Fig. 2 is oestrone mass spectrogram in cosmetic spray products in the inventive method；
All English bilinguals occurred in the Figure of description of the present invention are as follows：
m/z：Karyoplasmic ratio；Relative abundance：Relative abundance；Intensity：Intensity；Estrone：Oestrone.
Embodiment
First three-way pipe and the second three-way pipe (the big Lip river gram of generation (Shanghai) fluid system Science and Technology Ltd.)；P-1000 types are micro-
Electrode draws instrument (Sutter companies of the U.S.)；Capillary pipe spray pipe (the sharp Feng chromatograms device Co., Ltd of Yongnian)；Bruker
AmaZon ion trap mass spectrometers (Bruker Dalton companies of the U.S.).
The quick determination method of banned substance oestrone, comprises the following steps in a kind of spraying cosmetics：
Step 1: make the double threeway capillary pipe spray devices of open type；
As shown in figure 1, the double threeway capillary pipe spray devices of open type include the first three-way pipe 1 and the second three-way pipe of series connection
2, sample channel is formed in the horizontal direction, is provided with capillary pipe spray pipe 3 on sample channel, after capillary pipe spray pipe 3
End is connected with one end of isocon 4, and front end is arranged in sample channel, close to the right-hand member of the second three-way pipe 2, with the second three-way pipe
Blending space is formed between 2 right-hand member, the other end of isocon 4 is connected with sample bottle 5 and waste liquid bottle 6 respectively by pipeline, the
One three-way pipe 1 provides device 7 with gas by pipeline and is connected, and the second three-way pipe 2 is connected by pipeline with syringe pump 8, second
The right side of three-way pipe 8 is provided with mass spectrograph 9；
It is below the optimal technical scheme of the double threeway capillary pipe spray devices of open type：
First three-way pipe 1 and the second three-way pipe 2 include horizontal tube and VERTICAL TUBE, a left side for the horizontal tube of the first three-way pipe 1
End is closed using stator 10, and right-hand member is connected with the left end of the horizontal tube of the second three-way pipe 2, is provided with stator 10 logical
Hole, the rear end of capillary pipe spray pipe 3 pass from through hole, are connected with isocon 4.
The VERTICAL TUBE of first three-way pipe 1 provides device 7 with gas by pipeline and is connected, and the VERTICAL TUBE of the second three-way pipe 2 is led to
Pipeline is crossed with syringe pump 8 to be connected.
The interface of first three-way pipe 1 and the second three-way pipe 2 is 1/8 inch or 1/16 inch；The internal diameter of capillary pipe spray pipe 3
For 10~200 μm.
The front end of capillary pipe spray pipe 3 is arranged in the second three-way pipe 2, with the right-hand member of the horizontal tube of the second three-way pipe 2 it
Between distance be 1~3cm.
Flow control valve is provided with isocon 4.
Step 2: the double threeway capillary pipe spray devices of open type are placed at 3~4cm of sample inlet front end of mass spectrograph 9, if
The parameter for putting mass spectrograph 9 is：Positive ion mode, capillary voltage 4kV；The air pressure for setting gas offer device 7 is 30psi；Press
The aerosol valve of sample bottle 5 is pressed, obtains mass spectrum response signal；
Step 3: improve the response of analyte
Syringe pump 8 introduces liquid, and fltting speed is 20 μ L/min, and atomization gas dispels atomized drop, in capillary pipe spray pipe 3
Preceding end spaces mixes with sample, improves the mass spectrum response signal of test substance.
Nebulised sample in sample bottle 5 is spraying cosmetic sample.
The Information in Mass Spectra of test substance is as shown in table 1.
The Information in Mass Spectra of the test substance of table 1
The liquid that syringe pump 8 introduces is methoxamine derivatization reagent.
The chemical information of test substance is as shown in table 2：
The chemical information of the test substance of table 2
Mass spectrogram is as shown in Figure 2.
Analyte analyzation condition of the present invention is positive ion mode, and it is to be measured to improve to usually introduce derivatization reagent
The response of thing.This patent is related to the method for such a raising response.
Double threeway capillary pipe spray devices wherein introduce atomization gas all the way, and another way introduces derivatization reagent methoxamine.Through
Determine, the oestrone in cosmetics of spraying is significantly improved by derivative reaction, response.After testing, determined with about 3 times of signal to noise ratio
The detection of oestrone is limited to 50 μ g/kg.
Specific detection method application：
First, spray cosmetics in oestrone quick detection.
The first step：Make the double threeway capillary pipe spray devices of open type；
Second step：：The making of positive, various concentrations are added into the spraying toner for being free of estrone after testing
Estrone standard liquid, positive is prepared.
Double threeway capillary quick determination methods：By positive spraying cosmetic water sample and the double threeway capillary pipe sprays of open type
Device connects.The internal diameter of capillary pipe spray pipe 3 is 20 μm, is 3cm, air pressure 30psi apart from the injection port of mass spectrograph 9 distance.Mass spectrum
Condition is set as：Positive ion mode, capillary voltage 4kV.Product aerosol valve is pressed, obtains mass spectrum response signal.
3rd step：Improve the response of analysans
Syringe pump 8 introduces 100mM methoxamine derivatization reagent, and fltting speed is 20 μ L/min, and atomization gas dispels atomization
Methoxamine drop, derivative reaction occurs for end spaces before capillary pipe spray pipe 3, improves the mass spectrum response signal of oestrone, it spreads out
Mass spectrogram is as shown in Figure 2 after biochemistry.
Before derivatization, the parent ion of oestrone is m/z 271.3, and big by noise jamming, response is low.Filled by the present invention
Put, introduce methoxamine derivatization reagent, the monitoring parent ion selection of oestrone is m/z 300.2, and corresponding daughter ion is m/z
252.8, response significantly improves 24 times compared with underivatized.
Above concrete application is only citing, is not to limit, and all parameters selection within the scope of the present invention has obtained phase
As result.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to the model of the present invention
Enclose and be defined, on the premise of design spirit of the present invention is not departed from, technical side of the those of ordinary skill in the art to the present invention
The various modifications and improvement that case is made, it all should fall into the protection domain of claims of the present invention determination.
Claims (9)
- A kind of 1. quick determination method of banned substance oestrone in cosmetics of spraying, it is characterised in that：Comprise the following steps：Step 1: make the double threeway capillary pipe spray devices of open type；The double threeway capillary pipe spray devices of the open type include the first three-way pipe (1) and the second three-way pipe (2) of series connection, in water Square sample channel is upwardly formed, capillary pipe spray pipe (3), the capillary pipe spray pipe are provided with the sample channel (3) rear end is connected with the one end of isocon (4), and front end is arranged in the sample channel, close to second three-way pipe (2) Right-hand member, blending space is formed between the right-hand member of second three-way pipe (2), the other end of the isocon (4) passes through pipe Road is connected with sample bottle (5) and waste liquid bottle (6) respectively, and first three-way pipe (1) provides device (7) phase by pipeline and gas Even, second three-way pipe (2) is connected by pipeline with syringe pump (8), and matter is provided with the right side of second three-way pipe (8) Spectrometer (9)；Step 2: the double threeway capillary pipe spray devices of the open type are placed at 3~4cm of sample inlet front end of mass spectrograph (9), Set mass spectrograph (9) parameter be：Positive ion mode, capillary voltage 4kV；Set gas provide device (7) air pressure be 30psi；The aerosol valve of the sample bottle (5) is pressed, obtains mass spectrum response signal；Step 3: improve the response of analyte：The syringe pump (8) introduces liquid, and fltting speed is 20 μ L/min, and atomization gas dispels atomized drop, in the capillary End spaces mixes with sample before injection spray pipe (3), improves the mass spectrum response signal of test substance.
- 2. the quick determination method of banned substance oestrone in spraying cosmetics according to claim 1, it is characterised in that：Institute It is spraying cosmetics to state the nebulised sample in sample bottle (5).
- 3. the quick determination method of banned substance oestrone in spraying cosmetics according to claim 3, it is characterised in that：The Information in Mass Spectra of the test substance of table 1The Information in Mass Spectra of test substance is as shown in table 1.
- 4. the quick determination method of banned substance oestrone in spraying cosmetics according to claim 3, it is characterised in that：Institute Stating the first three-way pipe (1) and second three-way pipe (2) includes horizontal tube and VERTICAL TUBE, the water of first three-way pipe (1) The left end of flat pipe is closed using stator (10), and right-hand member is connected with the left end of the horizontal tube of second three-way pipe (2), described Through hole is provided with stator (10), the rear end of the capillary pipe spray pipe (3) passes from the through hole, with the isocon (4) it is connected.
- 5. the quick determination method of banned substance oestrone in spraying cosmetics according to claim 4, it is characterised in that：Institute The VERTICAL TUBE for stating the first three-way pipe (1) is connected by pipeline with gas offer device (7), second three-way pipe (2) VERTICAL TUBE is connected by pipeline with the syringe pump (8).
- 6. the quick determination method of banned substance oestrone in spraying cosmetics according to claim 5, it is characterised in that：Institute The interface for stating the first three-way pipe (1) and second three-way pipe (2) is 1/8 inch or 1/16 inch；The capillary pipe spray pipe (3) internal diameter is 10~200 μm.
- 7. the quick determination method of banned substance oestrone in spraying cosmetics according to claim 6, it is characterised in that：Institute The front end for stating capillary pipe spray pipe (3) is arranged in second three-way pipe (2), the horizontal tube with second three-way pipe (2) The distance between right-hand member be 1~3cm.
- 8. the quick determination method of banned substance oestrone in spraying cosmetics according to claim 7, it is characterised in that： Flow control valve is provided with the isocon (4).
- 9. the quick determination method of banned substance oestrone in spraying cosmetics according to claim 8, it is characterised in that：Institute The liquid for stating syringe pump (8) introducing is methoxamine derivatization reagent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710881259.5A CN107389831B (en) | 2017-09-26 | 2017-09-26 | Method for rapidly detecting forbidden substance estrone in spray cosmetics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710881259.5A CN107389831B (en) | 2017-09-26 | 2017-09-26 | Method for rapidly detecting forbidden substance estrone in spray cosmetics |
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| CN107389831A true CN107389831A (en) | 2017-11-24 |
| CN107389831B CN107389831B (en) | 2020-01-21 |
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| CN201710881259.5A Active CN107389831B (en) | 2017-09-26 | 2017-09-26 | Method for rapidly detecting forbidden substance estrone in spray cosmetics |
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