CN107655963A - The quick determination method of coumarin kind compound is disabled in a kind of liquid distilled from honeysuckle flowers or lotus leaves aquatic products - Google Patents
The quick determination method of coumarin kind compound is disabled in a kind of liquid distilled from honeysuckle flowers or lotus leaves aquatic products Download PDFInfo
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- CN107655963A CN107655963A CN201710883224.5A CN201710883224A CN107655963A CN 107655963 A CN107655963 A CN 107655963A CN 201710883224 A CN201710883224 A CN 201710883224A CN 107655963 A CN107655963 A CN 107655963A
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/68—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using electric discharge to ionise a gas
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Abstract
The invention discloses the quick determination method that coumarin kind compound is disabled in a kind of liquid distilled from honeysuckle flowers or lotus leaves aquatic products, 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 2~3cm 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, formic acid solution 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 accurate, sensitive, and the field quick detection of coumarin kind compound is disabled suitable for liquid distilled from honeysuckle flowers or lotus leaves aquatic products.
Description
Technical field
The present invention relates to a kind of detection method of chemical substance, more particularly to disabling cumarin in a kind of liquid distilled from honeysuckle flowers or lotus leaves aquatic products
The quick determination method of class compound.
Background technology
China《Cosmetics safety technical specification》(version in 2015) and European Union's cosmetics regulation (EC 1223/2009) are clear and definite
It is in the cosmetics such as floral water to provide cumarin, 7- methylcoumarins, ayapanin and 7- ethyl -4- methylcoumarins
Banned substance.These above-mentioned materials violated may be added in corresponding liquid distilled from honeysuckle flowers or lotus leaves aquatic products to reach the work of increase product efficacy
With.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of accurate, sensitive, suitable for the floral water of field quick detection
The quick determination method of coumarin kind compound is disabled in product.
The quick determination method of coumarin kind compound is disabled in a kind of liquid distilled from honeysuckle flowers or lotus leaves aquatic products, is comprised 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 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 2~3cm of sample inlet front end
Place, sets the mass spectrometric parameter to be：Positive ion mode, capillary voltage 3.5kV；Set gas provide device air pressure be
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 30 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 coumarin kind compound is disabled in liquid distilled from honeysuckle flowers or lotus leaves aquatic products of the present invention, wherein, the spray
Mist sample is liquid distilled from honeysuckle flowers or lotus leaves water sample.
The quick determination method of coumarin kind compound is disabled in liquid distilled from honeysuckle flowers or lotus leaves aquatic products of the present invention, wherein, the taboo
Include cumarin, 7- methylcoumarins, ayapanin and 7- ethyl -4- methylcoumarins with coumarin kind compound.
The quick determination method of coumarin kind compound is disabled in liquid distilled from honeysuckle flowers or lotus leaves aquatic products of the present invention, wherein, determinand
The Information in Mass Spectra of matter is as shown in table 1.
The Information in Mass Spectra of the test substance of table 1
The quick determination method of coumarin kind compound is disabled in liquid distilled from honeysuckle flowers or lotus leaves aquatic products of the present invention, wherein, described the
One three-way 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 is closed, and right-hand member is connected with the left end of the horizontal tube of second three-way pipe, and through hole, institute are provided with the stator
The rear end for stating capillary pipe spray pipe passes from the through hole, is connected with the isocon.
The quick determination method of coumarin kind compound is disabled in liquid distilled from honeysuckle flowers or lotus leaves aquatic products of the present invention, wherein, described the
The VERTICAL TUBE of one three-way pipe provides device with the gas by pipeline and is connected, and the VERTICAL TUBE of second three-way pipe passes through pipeline
It is connected with the syringe pump.
The quick determination method of coumarin kind compound is disabled in liquid distilled from honeysuckle flowers or lotus leaves aquatic products of the present invention, wherein, described the
The interface of one three-way 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 μm.
The quick determination method of coumarin kind compound is disabled in liquid distilled from honeysuckle flowers or lotus leaves aquatic products of the present invention, wherein, the hair
The front end of tubule injection spray pipe is arranged in second three-way pipe, between the right-hand member of the horizontal tube of second three-way pipe away from
From for 1~3cm.
The quick determination method of coumarin kind compound is disabled in liquid distilled from honeysuckle flowers or lotus leaves aquatic products of the present invention, wherein, described
Flow control valve is provided with isocon.
The quick determination method of coumarin kind compound is disabled in liquid distilled from honeysuckle flowers or lotus leaves aquatic products of the present invention, wherein, the note
The liquid for penetrating pump introducing is formic acid solution.
The quick determination method difference from prior art of coumarin kind compound is disabled in liquid distilled from honeysuckle flowers or lotus leaves aquatic products of the present invention
It is：
The quick determination method that coumarin kind compound is disabled in liquid distilled from honeysuckle flowers or lotus leaves aquatic products of the present invention establishes a kind of double threeway hairs
The detection method of coumarin kind compound, this method are disabled in tubule electrospray tandem ion trap mass spectrometry rapid screening liquid distilled from honeysuckle flowers or lotus leaves aquatic products
Accurately, it is sensitive, suitable for field quick detection.
The quick determination method novelty and advantage that coumarin kind compound is disabled in liquid distilled from honeysuckle flowers or lotus leaves aquatic products of the present invention are：
1st, present invention firstly provides the method for double threeway capillary pipe spray tandem mass spectrums, in quick detection liquid distilled from honeysuckle flowers or lotus leaves aquatic products
Disable coumarin kind compound.
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, by introducing H+Each substance responds value is improved, each material detection is limited between 30 or 50 μ g/kg.
3rd, the present invention is without using Extraction solvent.
4th, material of the present invention includes cumarin, 7- methylcoumarins, ayapanin and 7- ethyl -4- first
Butylcoumariii.
The quick determination method that coumarin kind compound is disabled in the liquid distilled from honeysuckle flowers or lotus leaves aquatic products of the present invention is made below in conjunction with the accompanying drawings
Further illustrate.
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 floral water spray product banned substance mass spectrogram in the inventive method, wherein a) cumarin, b) 7- methyl is fragrant
Legumin, c) ayapanin, d) 7- ethyls -4- methylcoumarins.
All English bilinguals occurred in the Figure of description of the present invention are as follows：
m/z：Karyoplasmic ratio；Relative abundance：Relative abundance；Coumarin：Cumarin；7-
Methylcoumarin：7- methylcoumarins；7-Methoxycoumarin：Ayapanin；7-Ethoxy-4-
methylcoumarin：7- ethyl -4- methylcoumarins.
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 coumarin kind compound is disabled in a kind of liquid distilled from honeysuckle flowers or lotus leaves aquatic products, is comprised the following steps：
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 2~3cm of sample inlet front end of mass spectrograph 9, if
The parameter for putting mass spectrograph 9 is：Positive ion mode, capillary voltage 3.5kV；The air pressure for setting gas offer device 7 is 30psi；
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 30 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 liquid distilled from honeysuckle flowers or lotus leaves water sample.
Disabling coumarin kind compound includes cumarin, 7- methylcoumarins, ayapanin and 7- ethyl -4- first
Butylcoumariii.
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 formic acid solution.
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, usually introduces H+Analyte response can be improved
Value, its response can be improved for the low analyte of response by derivative reaction.This patent is related to such a improve and responded
The method of value.
Double threeway capillary pipe spray devices wherein introduce atomization gas all the way, and another way introduces formic acid and (provides H+).After measured
Analyte response in liquid distilled from honeysuckle flowers or lotus leaves water sample significantly improves.After testing, the detection limit of each material is determined with about 3 times of signal to noise ratio, it
Detection be limited to 30 or 50 μ g/kg.
Specific detection method application：
First, in floral water cumarin quick determination method.
The first step：Make the double threeway capillary pipe spray devices of open type；
Second step：The making of positive, commission aerosol manufacturer make various concentrations positive.
Double threeway capillary quick determination methods：By positive aerosol sample and the double threeway capillary pipe spray devices of open type
Connection.The internal diameter of capillary pipe spray pipe 3 is 20 μm, is 2cm, air pressure 30psi apart from the injection port of mass spectrograph 9 distance.Mass Spectrometry Conditions
It is set as：Positive ion mode, capillary voltage 3.5kV.Product aerosol valve is pressed, obtains mass spectrum response signal.
3rd step：Improve the response of analyte
Syringe pump 8 introduces formic acid, and fltting speed is 30 μ L/min, and atomization gas dispels atomization formic acid drop, sprayed in capillary
End spaces provides a large amount of H before mist pipe 3+, improve the mass spectrum response signal of cumarin.
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 (10)
1. the quick determination method of coumarin kind compound is disabled in a kind of liquid distilled from honeysuckle flowers or lotus leaves aquatic products, it is characterised in that：Including following step
Suddenly：
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 2~3cm of sample inlet front end of mass spectrograph (9),
Set mass spectrograph (9) parameter be：Positive ion mode, capillary voltage 3.5kV；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 30 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 coumarin kind compound, its feature are disabled in liquid distilled from honeysuckle flowers or lotus leaves aquatic products according to claim 1
It is：Nebulised sample in the sample bottle (5) is liquid distilled from honeysuckle flowers or lotus leaves water sample.
3. the quick determination method of coumarin kind compound, its feature are disabled in liquid distilled from honeysuckle flowers or lotus leaves aquatic products according to claim 2
It is：The disabling coumarin kind compound includes cumarin, 7- methylcoumarins, ayapanin and 7- ethyls -4-
Methylcoumarin.
4. the quick determination method of coumarin kind compound, its feature are disabled in liquid distilled from honeysuckle flowers or lotus leaves aquatic products according to claim 3
It is：
The Information in Mass Spectra of the test substance of table 1
The Information in Mass Spectra of test substance is as shown in table 1.
5. the quick determination method of coumarin kind compound, its feature are disabled in liquid distilled from honeysuckle flowers or lotus leaves aquatic products according to claim 4
It is：First three-way pipe (1) and second three-way pipe (2) include horizontal tube and VERTICAL TUBE, first three-way pipe
(1) left end of horizontal tube is closed using stator (10), the left end phase of right-hand member and the horizontal tube of second three-way pipe (2)
Even, through hole being provided with the stator (10), the rear end of the capillary pipe spray pipe (3) passes from the through hole, with
The isocon (4) is connected.
6. the quick determination method of coumarin kind compound, its feature are disabled in liquid distilled from honeysuckle flowers or lotus leaves aquatic products according to claim 5
It is：The VERTICAL TUBE of first three-way pipe (1) provides device (7) with the gas by pipeline and is connected, second threeway
The VERTICAL TUBE of pipe (2) is connected by pipeline with the syringe pump (8).
7. the quick determination method of coumarin kind compound, its feature are disabled in liquid distilled from honeysuckle flowers or lotus leaves aquatic products according to claim 6
It is：The interface of first three-way pipe (1) and second three-way pipe (2) is 1/8 inch or 1/16 inch；The capillary
The internal diameter of injection spray pipe (3) is 10~200 μm.
8. the quick determination method of coumarin kind compound, its feature are disabled in liquid distilled from honeysuckle flowers or lotus leaves aquatic products according to claim 7
It is：The front end of the capillary pipe spray pipe (3) is arranged in second three-way pipe (2), with second three-way pipe (2)
The distance between right-hand member of horizontal tube is 1~3cm.
9. the quick determination method of coumarin kind compound, its feature are disabled in liquid distilled from honeysuckle flowers or lotus leaves aquatic products according to claim 8
It is：Flow control valve is provided with the isocon (4).
10. the quick determination method of coumarin kind compound, its feature are disabled in liquid distilled from honeysuckle flowers or lotus leaves aquatic products according to claim 9
It is：The liquid that the syringe pump (8) introduces is formic acid solution.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710883224.5A CN107655963B (en) | 2017-09-26 | 2017-09-26 | Rapid detection method for forbidden coumarin compounds in floral water product |
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| CN201710883224.5A CN107655963B (en) | 2017-09-26 | 2017-09-26 | Rapid detection method for forbidden coumarin compounds in floral water product |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110044978A (en) * | 2019-04-17 | 2019-07-23 | 安徽大学 | A method of distinguishing 4 hydroxy coumarin (4-HC) and its isomer umbelliferone (7-HC) |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110044978A (en) * | 2019-04-17 | 2019-07-23 | 安徽大学 | A method of distinguishing 4 hydroxy coumarin (4-HC) and its isomer umbelliferone (7-HC) |
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