CN106596779B - The detection method of two octodrines in leather, textile - Google Patents
The detection method of two octodrines in leather, textile Download PDFInfo
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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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- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The invention discloses a kind of detection methods of two octodrines in leather, textile, comprising the following steps: sample treatment: taking sample to be tested, organic solvent extraction is added and obtains extract liquor；Gas chromatography-mass spectrography detection.Detection method of the invention is easy quickly, and preferably methanol is as extractant, by the way that under the testing conditions of optimization, two octodrines can complete a chromatography in 11min, and can obtain good separating effect after methanol extraction.This method is linear good in the two octodrine concentration ranges of 0.1~10mg/L, linearly dependent coefficient reaches 0.9998, and detection limit reaches 0.1mg/L, repeated relative standard deviation < 3%, sample recovery of standard addition is 95%~110%, is had a good application prospect.
Description
Technical field
The present invention relates to chemical analysis fields, more particularly to a kind of detection method of two octodrines in leather, textile.
Background technique
Two octodrines are used in leather textile mainly as the intermediate of surfactant, it may also be used for ore floating washing,
Extractant, emulsifier of rare metal etc..Research shows that two octodrines are toxic to fish, there is irritation to eyes, skin,
With potential persistence, bioconcentration and toxicity, seriously jeopardize human health.On March 17th, 2015, Europe chemistry quality control
The community, European Union that reason administration ECHA has formally issued 2015-2017 rolls action plan (CoRAP) list of substances, altogether includes 134
A, two octodrines are put into wherein.As it can be seen that the harmfulness of two octodrines has caused the great attention of society, therefore, establish
Detection method appropriate is necessary to detect the content of two octodrines.
And the detection method of two octodrines in product yet there are no at present all in report, Europe is entered to China's Related product
Allied city field forms certain obstruction.
Summary of the invention
Based on this, it is necessary to provide a kind of fast and effectively leather, in textile two octodrines detection method.
Specific technical solution is as follows:
The detection method of two octodrines in a kind of leather, textile, comprising the following steps:
Sample treatment: taking sample to be tested, and organic solvent extraction is added and obtains extract liquor；
Gas chromatography-mass spectrography detection:
Carry out gas chromatography-mass spectrography detection to the extract liquor, GC conditions are as follows: chromatographic column: stationary phase is
The phenyl modified dimethyl polysiloxane of cyanogen propyl, length 25-35m, 1.3-1.5 μm of film thickness, internal diameter 0.23-0.27mm；Using
Temperature programming；Injector temperature: 230-250 DEG C；Sample introduction mode: it does not shunt；Flow: 0.8-1.5ml/min；Quantified by external standard method；
Mass Spectrometry Conditions are as follows: ion source temperature: 225-235 DEG C；Chromatography-mass spectroscopy interface temperature: 220-250 DEG C；Ionization mode:
Electron impact ionization；The solvent delay time: 3-6min；Acquisition mode: full scan mode and selection ion scan mode.
The GC conditions in one of the embodiments, are as follows: chromatographic column: DB-624, length 30m, 1.4 μ of film thickness
M, internal diameter 0.25mm；Using temperature programming；Injector temperature: 250 DEG C；Sample introduction mode: it does not shunt；Flow: 1.5ml/min；Outside
Mark standard measure.
The Mass Spectrometry Conditions in one of the embodiments, are as follows: 230 DEG C of ion source temperature, chromatography-mass spectroscopy interface temperature:
240℃；Ionization mode: electron impact ionization, ionizing energy 70eV；The solvent delay time: 4min；Acquisition mode: full scan
Mode and selection ion scan mode.
Described program heats up in one of the embodiments, specifically: 80-120 DEG C of initial temperature, 0.5-2min is kept,
230-250 DEG C is risen to the rate of 5-20 DEG C/min, keeps 2-10min.
In one of the embodiments, described program heat up specifically: 120 DEG C of initial temperature, keep 1min, with 20 DEG C/
The rate of min rises to 250 DEG C, keeps 3.5min.
The scanning range of the full scan mode is 35-300m/z in one of the embodiments,.
In one of the embodiments, it is described selection ion scan mode ion be selected from 44m/z, 142m/z, 143m/z,
241m/z and 242m/z.
In one of the embodiments, before the gas chromatography-mass spectrography detecting step, the extract liquor is with 0.45
μm filtering with microporous membrane.
In one of the embodiments, in the sample handling procedure, extraction time 50-120min, extraction temperature
It is 58-62 DEG C.
The organic solvent is methanol, the matter of the sample to be tested and the organic solvent in one of the embodiments,
Amount volume ratio is 0.1-2g:5-20ml.
The principle of the present invention and the utility model has the advantages that
The present invention through a large number of experiments and has been determined using methanol as extractant, and two in extraction sample are different
Octylame, it is qualitative with appearance time by the optimization of selection and extraction conditions, gas-chromatography and Mass Spectrometry Conditions to chromatographic column,
Response is quantitative, establishes a kind of detection method of quickly and effectively two octodrines.Detection method of the invention has wider
The range of linearity, two octodrines are linear good in the range of 0.1mg/L-10mg/L, and linearly dependent coefficient reaches 0.9998, detection
Limit is down to 0.1mg/L, and recovery of standard addition 95%-110%, relative standard deviation < 3%, sensitivity and accuracy are higher, because
This has a good application prospect.
Detailed description of the invention
Fig. 1 is the gas chromatogram of embodiment 1, and wherein A is full scan mode, and B is selection ion scan mode；
Fig. 2 is the mass spectrogram of embodiment 1；
Fig. 3 is the gas chromatogram of embodiment 2；
Fig. 4 is the gas chromatogram of comparative example 1；
Fig. 5 is the extraction efficiency result figure of different extractants；
Fig. 6 is the extraction efficiency result figure of different extraction temperatures；
Fig. 7 is the extraction efficiency result figure of different extraction times；
Fig. 8 is the standard curve of two octodrines；
Fig. 9 is the gas chromatogram of the two octodrine standard solution of 0.1mg/L.
Specific embodiment
To facilitate the understanding of the present invention, a more comprehensive description of the invention is given in the following sections with reference to the relevant attached drawings.In attached drawing
Give presently preferred embodiments of the present invention.But the invention can be realized in many different forms, however it is not limited to this paper institute
The embodiment of description.On the contrary, purpose of providing these embodiments is keeps the understanding to the disclosure more thorough
Comprehensively.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein "and/or" includes one or more phases
Any and all combinations of the listed item of pass.
Related equipment used in the present embodiment are as follows: gas chromatograph-mass spectrometer (GC-MS) 7890A-5975C, the U.S.
Agilent company；Ultrasonic cleaner 2300HT, Shanghai ANPEL Scientific Instrument Co., Ltd.；Table model high speed centrifuge H1650,
Changsha Xiang Yi centrifuge Instrument Ltd.；Rotary Evaporators V-850, BUCHI company, Switzerland；Eddy mixer XW-80A, on
Industrial Co., Ltd., Nereid section；100000 hierarchical analysis balance X205BDU, METTLER TOLEDO company, Switzerland；Ten thousand hierarchical analysis
Balance AL204, METTLER TOLEDO company, Switzerland.Related reagent used in the present embodiment are as follows: methanol, ethyl alcohol, acetone
It is UPLC grades, Shanghai ANPEL Scientific Instrument Co., Ltd.；Two octodrine standard items, purity 99%, U.S. Aldrich
Chemistry company.It is appreciated that instrument model and brand are without being limited thereto, specification is similar.
The preparation of two octodrine standard solution: two octodrine sterling 10mg (tool is accurately weighed with 100,000 hierarchical analysis balances
Body sample weighting amount need to convert according to purity), it is added in 10mL volumetric flask, dissolves constant volume with methanol, be configured to the standard of 1000mg/L
Stock solution, the standard for being then diluted to 0.1mg/L, 0.2mg/L, 0.5mg/L, 1mg/L, 2mg/L, 5mg/L, 10mg/L step by step are molten
Liquid.
The detection method of two octodrines, includes the following steps: in the leather of an embodiment of the present invention, textile
S10, sample treatment: taking sample to be tested, and organic solvent extraction is added and obtains extract liquor.
Preferably, extraction time 50-120min, extraction temperature are 58-62 DEG C.
Preferably, organic solvent is methanol, and the mass volume ratio of sample to be tested and organic solvent is 0.1-2g:5-20ml.
It is appreciated that can according to need repetition extraction repeatedly to further increase extraction yield, merge multiple extraction
Liquid.
S20, gas chromatography-mass spectrography detection:
Carry out gas chromatography-mass spectrography detection to extract liquor, GC conditions are as follows: chromatographic column: stationary phase is cyanogen third
The phenyl modified dimethyl polysiloxane of base, length 25-35m, 1.3-1.5 μm of film thickness, internal diameter 0.23-0.27mm；Using program
Heating；Injector temperature: 230-250 DEG C；Sample introduction mode: it does not shunt；Flow: 0.8-1.5ml/min；Quantified by external standard method；Mass spectrum
Condition are as follows: ion source temperature: 225-235 DEG C；Chromatography-mass spectroscopy interface temperature: 220-250 DEG C；Ionization mode: electron bombardment electricity
From；The solvent delay time: 3-6min；Acquisition mode: full scan mode and selection ion scan mode.
Preferably, GC conditions are as follows: chromatographic column: DB-624, length 30m, 1.4 μm of film thickness, internal diameter 0.25mm；Using
Temperature programming；Injector temperature: 250 DEG C；Sample introduction mode: it does not shunt；Flow: 1.5ml/min；Quantified by external standard method.
Preferably, Mass Spectrometry Conditions are as follows: 230 DEG C of ion source temperature, chromatography-mass spectroscopy interface temperature: 240 DEG C；Ionization mode: electricity
Son bombardment ionization, ionizing energy 70eV；The solvent delay time: 4min；Acquisition mode: full scan mode and selection ion scan
Mode.
Preferably, temperature programming specifically: 80-120 DEG C of initial temperature, 0.5-2min is kept, with the speed of 5-20 DEG C/min
Rate rises to 230-250 DEG C, keeps 2-10min.It is highly preferred that temperature programming specifically: 120 DEG C of initial temperature, 1min is kept, with
The rate of 20 DEG C/min rises to 250 DEG C, keeps 3.5min.
Preferably, the scanning range of full scan mode is 35-300m/z.
Preferably, the ion of ion scan mode is selected to be selected from 44m/z, 142m/z, 143m/z, 241m/z and 242m/z.
Preferably, before step S20,0.45 μm of filtering with microporous membrane of extract liquor avoids instrument stifled to reduce interference
Fill in the lost of life.
The present invention through a large number of experiments and has been determined using methanol as extractant, and two in extraction sample are different
Octylame, it is qualitative with appearance time by the optimization of selection and extraction conditions, gas-chromatography and Mass Spectrometry Conditions to chromatographic column,
Response is quantitative, establishes a kind of detection method of quickly and effectively two octodrines.Detection method of the invention has wider
The range of linearity, two octodrines are linear good in the range of 0.1mg/L-10mg/L, and linearly dependent coefficient reaches 0.9998, detection
Limit is down to 0.1mg/L, and recovery of standard addition 95%-110%, relative standard deviation < 3%, sensitivity and accuracy are higher, because
This has a good application prospect.
The application is further elaborated below by way of specific embodiment.
Embodiment 1
Leather or textile sample are cut to 2mm × 2mm × 2mm size, weigh 1g ± 0.1g (being accurate to 0.1mg) in
In 60ml glass reaction bottle, the methanol of 10ml is added, in 60 DEG C of ultrasonic extraction 60min ± 5min, repeats to extract primary, merging two
Secondary extract liquor mixes, and is concentrated into about 2ml with Rotary Evaporators, and slowly nitrogen is blown to close dry, with methanol constant volume to 1ml, then passes through
Then 0.45 μm of filtering with microporous membrane carries out gas chromatography-mass spectrography detection.
GC conditions: chromatographic column: DB-624, length 30m, 1.4 μm of film thickness, internal diameter 0.25mm；Temperature program: initial
Temperature is 120 DEG C, keeps 1min, rises to 250 DEG C with the rate of 20 DEG C/min, keeps 3.5min；Injector temperature: 250 DEG C；Into
Original mold formula: it does not shunt；Sample volume: 1 μ L；Carrier gas: helium, purity >=99.999%；Flow: 1.5ml/min；Quantified by external standard method.
Mass Spectrometry Conditions: 230 DEG C of ion source temperature, chromatography-mass spectroscopy interface temperature: 240 DEG C；Ionization mode: electron impact ionization, ionization energy
Amount is 70eV；The solvent delay time: 4min；Acquisition mode: full scan Mode S CAN, scanning range 35-300m/z, select from
Sub- scan pattern SIM, selects quota ion for 142m/z, and qualitative ion is 241m/z, 44m/z.Chromatographic results as shown in Figure 1,
It can be seen that two octodrines are totally separated from, retention time 7.92min, and peak shape is symmetrical, response is very high, separation
Effect is fine, and analysis time is short.For mass spectral results as shown in Fig. 2, visible response value is high, miscellaneous peak is few, interferes small.
Embodiment 2
Detection method is substantially the same manner as Example 1, and difference is only that temperature program: initial temperature is 100 DEG C, is kept
1min rises to 250 DEG C with the rate of 30 DEG C/min, keeps 7min, and chromatographic results are as shown in Figure 3, it can be seen that, two octodrine energy
It is enough to be separated, but response is lower compared with Example 1, appearance time is more early, and analysis time is longer.
Comparative example 1
Detection method is substantially the same manner as Example 1, and difference is only that the chromatographic column used is HP-5MS, and stationary phase is hexichol
The modified dimethyl arlydene siloxanes of base, length 30m, 0.25 μm of film thickness, internal diameter 0.25mm, chromatographic results are as shown in figure 4, can
It is unable to get obvious independent two octodrines chromatographic peak to see, separation purpose cannot be reached.
The Optimum Experiment of extractant
Four kinds of methanol, water, ethyl alcohol and acetone solvents are chosen as extractant and carry out extraction yield comparative test, as a result as schemed
Shown in 5, under such as 1 the same terms of embodiment, the extraction yield highest of methanol, therefore, methanol are most preferred extractant.
The Optimum Experiment of extraction temperature
15 DEG C, 35 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C and 80 DEG C are chosen as extraction temperatures and carries out extraction yields to having a competition
It tests, as a result as shown in fig. 6, under such as 1 the same terms of embodiment, 60 DEG C of whens can achieve maximum extraction yield, therefore 60 DEG C are
Most preferred extraction temperature.
The Optimum Experiment of extraction time
15min, 35min, 40min, 50min, 60min, 70min and 80min are chosen as extraction time and carries out extraction yield
Comparative test, as a result as shown in fig. 7,60min can achieve maximum extraction yield, therefore under such as 1 the same terms of embodiment
60min is most preferred extraction time.
The standard curve of two octodrines
According to the testing conditions of embodiment 1, to two octodrine 0.1mg/L, 0.2mg/L, 0.5mg/L, 1mg/L, 2mg/L,
The standard solution of 5mg/L, 10mg/L are tested and analyzed, and then using concentration as abscissa, are drawn and are marked as ordinate using response
Directrix curve, as a result as shown in Figure 8, it can be seen that the detection method is linear in the range of two octodrine concentration 0.1-10mg/L
Well, linearly dependent coefficient reaches 0.9998, meets quantitative calculate and requires, linear equation Y=690010X+47570.According to
It, can be different pungent according in formula A=X × V × f/m calculating sample to be tested two after linear equation calculates the value of concentration X (mg/L)
The content of amine, wherein A is the content (mg/kg) of two octodrines in sample to be tested, and V is final constant volume (ml), and m is weighed
Sample to be tested quality (g), f are dilution gfactor.
Detection limit measurement
According to the testing conditions of embodiment 1, two octodrine standard samples of various concentration are tested and analyzed, with 3 times
Signal-to-noise ratio (S/N >=3) determines the detection limit (LOD) of method, and the detection for measuring two octodrines is limited to 0.1mg/L, is illustrated in figure 9
The response of the gas chromatogram of the two octodrine standard solution of 0.1mg/L, blank test result is less than detection limit, can satisfy
The testing requirements of two octodrines.
Precision test
According to the testing conditions of embodiment 1, the standard solution of two octodrines of 1mg/L is continuously detected 6 times, as a result such as table
Shown in 1, relative standard deviation < 3% can be obtained according to testing result, illustrate that the detection method precision is high, it is reproducible.
Table 1
Accuracy test
It is molten that the standard that ultimate density is 0.1mg/L, 0.5mg/L, 2mg/L and 10mg/L is separately added into blank sample
Liquid, according to the testing conditions of embodiment 1, each concentration point does parallel test three times, calculates recovery of standard addition.From the result of table 2
It is found that the rate of recovery of two octodrines is between 95%-110%, it is seen that the detection method accuracy is higher.
Table 2
In summary, the present invention by constantly test and exploration establish a kind of detection of gas chromatography-mass spectrometry to
The analysis test method of two octodrines in sample, this method is easy quickly, and preferably methanol passes through methanol ultrasound as extractant
After extraction under the testing conditions of optimization, two octodrines can complete a chromatography in 11min, and can obtain well
Separating effect.This method is linear good in the two octodrine concentration ranges of 0.1~10mg/L, and linearly dependent coefficient reaches
0.9998, detection limit reaches 0.1mg/L, repeated relative standard deviation < 3%, and sample recovery of standard addition is 95%~110%,
It has a good application prospect.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (7)
1. the detection method of two octodrines in a kind of leather, textile, which comprises the following steps:
Sample treatment: taking sample to be tested, and organic solvent extraction is added and obtains extract liquor；The organic solvent be methanol, it is described to
The mass volume ratio of sample and the organic solvent is (0.1-2g): (5-20) ml, extraction time 50min-120min, extraction
Taking temperature is 58-62 DEG C；
Gas chromatography-mass spectrography detection:
Gas chromatography-mass spectrography detection, GC conditions are as follows: chromatographic column: DB-624, length are carried out to the extract liquor
30m, 1.4 μm of film thickness, internal diameter 0.25mm；Using temperature programming；Injector temperature: 230-250 DEG C；Sample introduction mode: it does not shunt；Stream
Amount: 0.8-1.5ml/min；Quantified by external standard method；Described program heating specifically: 80-120 DEG C of initial temperature, 0.5-2min is kept,
230-250 DEG C is risen to the rate of 5-20 DEG C/min, keeps 2-10min；
Mass Spectrometry Conditions are as follows: ion source temperature: 225-235 DEG C；Chromatography-mass spectroscopy interface temperature: 220-250 DEG C；Ionization mode: electronics
Bombardment ionization；The solvent delay time: 3-6min；Acquisition mode: full scan mode and selection ion scan mode.
2. detection method according to claim 1, which is characterized in that the GC conditions are as follows: chromatographic column: DB-
624, length 30m, 1.4 μm of film thickness, internal diameter 0.25mm；Using temperature programming；Injector temperature: 250 DEG C；Sample introduction mode: regardless of
Stream；Flow: 1.5ml/min；Quantified by external standard method.
3. detection method according to claim 1, which is characterized in that the Mass Spectrometry Conditions are as follows: 230 DEG C of ion source temperature,
Chromatography-mass spectroscopy interface temperature: 240 DEG C；Ionization mode: electron impact ionization, ionizing energy 70eV；The solvent delay time:
4min；Acquisition mode: full scan mode and selection ion scan mode.
4. detection method according to claim 1, which is characterized in that described program heating specifically: initial temperature 120
DEG C, 1min is kept, 250 DEG C is risen to the rate of 20 DEG C/min, keeps 3.5min.
5. detection method according to claim 1, which is characterized in that the scanning range of the full scan mode is 35-
300m/z。
6. detection method according to claim 1, which is characterized in that the ion of the selection ion scan mode is selected from 44
M/z, 142 m/z, 143 m/z, 241 m/z and 242 m/z.
7. detection method according to claim 1, which is characterized in that in the gas chromatography-mass spectrography detecting step
Before, 0.45 μm of filtering with microporous membrane of the extract liquor.
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