CN109507306A - The measuring method of tributyl 2-acetylcitrate in a kind of water base adhesive - Google Patents
The measuring method of tributyl 2-acetylcitrate in a kind of water base adhesive Download PDFInfo
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- CN109507306A CN109507306A CN201811119680.3A CN201811119680A CN109507306A CN 109507306 A CN109507306 A CN 109507306A CN 201811119680 A CN201811119680 A CN 201811119680A CN 109507306 A CN109507306 A CN 109507306A
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- tributyl
- acetylcitrate
- water base
- base adhesive
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Pathology (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a kind of measuring methods of tributyl 2-acetylcitrate content in water base adhesive, and first with the tributyl 2-acetylcitrate in acetonitrile extraction water base adhesive sample, C is added later18Dispersive solid-phase extraction agent is centrifugated after vortex oscillation, supernatant liquid filtering film is taken to be analyzed with Ultra Performance Liquid Chromatography instrument, and quantified by external standard method measures the content of tributyl 2-acetylcitrate in solution.The present invention provides a kind of measuring methods of tributyl 2-acetylcitrate in simple, fast and efficient water base adhesive, specific advantage is: 1) the characteristics of being directed to small UPLC instrument pipeline dead volume, high sensitivity, sample-pretreating method is targetedly developed, by the way that C is added18Bonded silica gel significantly reduces the interference of non-targeted object in matrix as dispersive solid-phase extraction agent；2) quick analyzing novel methods are established by the optimization to UPLC chromatographic condition according to target compound feature, minute is less than 20min.
Description
Technical field
The invention belongs to analysis technical fields, and in particular to the measurement of tributyl 2-acetylcitrate content in a kind of water base adhesive
Method.
Background technique
Plasticizer be it is a kind of can reduce high-molecular compound glass transition temperature and melting temperature, improve glue-line brittleness, promote
The substance of melt fluidity.Appropriate plasticizer is added in adhesive components, shear strength can be improved and unevenly avulses strong
Degree, increases the flexibility of glue film.Tributyl 2-acetylcitrate is a kind of novel green, nontoxic plasticizer, LD50=4000mg/
Kg can be used as the plasticising of polyvinyl chloride, celluosic resin and synthetic rubber.It is granulated for nontoxic PVC, food container, youngster
Virgin toy product, medical product, the products such as film, plate, cellulose paint can also add in the production of same water base adhesive product
Substance of this kind.
Currently, the national standard or professional standard of tributyl 2-acetylcitrate in adhesive detect not yet in China, therefore
Establish quality monitoring and buying side of the measuring method of tributyl 2-acetylcitrate in water base adhesive for water base adhesive manufacturing enterprise
Raw material monitoring have important meaning.
Summary of the invention
The purpose of the present invention is intended to establish the measurement side of tributyl 2-acetylcitrate in simple, the quick water base adhesive of one kind
Method, using UPLC as instrument analysis means, and it is mating establish corresponding sample-pretreating method, to obtain clean upper machine
Solution reduces interference of the matrix to measurement object.
The purpose of the present invention is achieved through the following technical solutions:
The measuring method of tributyl 2-acetylcitrate content, includes the following steps: in a kind of water base adhesive
Step 1) with the tributyl 2-acetylcitrate in acetonitrile extraction water base adhesive sample, C18 dispersive solid-phase extraction is added
Agent is centrifugated after vortex oscillation, takes supernatant liquid filtering film, obtain the sample solution to be tested；
Step 2) prepare tributyl 2-acetylcitrate calibration curve solution；
Step 3) with Ultra Performance Liquid Chromatography instrument using acetonitrile and water as eluent gradient elution analysis the sample solution to be tested and standard
Curve solution, quantified by external standard method measure tributyl 2-acetylcitrate；Acetyl tributyl citrate three in water base adhesive is calculated according to measurement result
The content of butyl ester.
Further to improve, the step 3) in chromatographic condition are as follows: chromatographic column is Atlantis T33mm×
100mm；Gradient elution program: 0~15min, acetonitrile and water ratio are linearly risen to 100% acetonitrile by 20:80；15~20min,
100% acetonitrile；
Column temperature: 20~40 DEG C；Flow velocity: 0.3~0.6mL/min；Sample volume: 1~5 μ L；Detector is diode array inspection
Survey device, Detection wavelength 212nm.
Further to improve, the column temperature is 30 DEG C, flow velocity 0.6mL/min, and sample volume is 2 μ L.
Further to improve, the step 1) in weigh 0.5~1g water base adhesive sample and be placed in conical flask, 5~20mL is added
Acetonitrile solution, vortex oscillation 5min obtains water base adhesive with 0.22 μm of organic membrane filtration after taking a small amount of extract liquor to be centrifugated
Testing sample solution.
Further to improve, the step 1) in centrifuge separation temperature be 20~25 DEG C, revolving speed is 10000~
15000rpm, time are 5~10min.
Further to improve, when quantified by external standard method, can make standard curve in the usual way, but preferably press following process systems
Make: being formulated as follows tributyl 2-acetylcitrate standard working solution (0.01mg/mL, 0.05mg/mL, 0.1mg/ of 5 concentration
ML, 0.5mg/mL and 1mg/mL), using peak area as ordinate, the concentration with tributyl 2-acetylcitrate standard working solution is
Abscissa draws standard curve.Test should make standard curve every time, and an intermediate concentration should be added after every 20 samples measurement
Standard solution should re-start the drafting of standard curve if the value measured and initial value differ by more than 5%.
In the present invention, tributyl 2-acetylcitrate content is calculated by formula (1) in water base adhesive sample:
In formula:
The concentration of tributyl 2-acetylcitrate in the water base adhesive sample that C-is obtained by standard curve, unit are the every milli of microgram
It rises (μ g/mL)；
C0Tributyl 2-acetylcitrate concentration in the-blank sample obtained by standard curve, unit is micrograms per millilitre
(μg/mL)；
V-extract liquor volume, unit are milliliter (mL)；
K- extension rate；
M- sample quality, unit are gram (g).
Average value to be measured in parallel twice is accurate to 0.1mg/kg for final measurement result.
Being measured in parallel its relative average debiation of result should be less than 10%.
If the concentration of sample to be tested solution exceeds the concentration range of standard working curve, change the extension rate of extract liquor
After redeterminate.
The present invention provides a kind of measuring method of tributyl 2-acetylcitrate in simple, fast and efficient water base adhesive, tools
There is following advantage: 1) the characteristics of being directed to small UPLC instrument pipeline dead volume, high sensitivity, before targetedly developing sample
Reason method, by the way that C is added18Bonded silica gel is diluted as dispersive solid-phase extraction agent and a certain proportion of solvent, is greatly reduced
The interference of non-targeted object in matrix；2) it according to target compound feature, by the optimization to UPLC chromatographic condition, establishes fast
Fast analyzing novel methods, minute are less than 20min.
1. the detection of inventive method limits
It selects the standard solution (0.01mg/mL) of minimum concentration to be measured in parallel 10 times, calculates its standard deviation, marked with 3 times
Quasi- deviation is the detection limit of measurement.Research shows that method detection is limited to 0.005mg/mL.
2. the rate of recovery and repeatability of inventive method
Using the rate of recovery of Standard Addition Method for Determination method.It weighs 0.5g sample, is added and its content is comparable mixes mark
Quasi- solution is extracted according to the Pretreatment of this method, is repeated 6 times, and measures its recovery of standard addition and repeatability, as a result such as
Shown in table 1.Average recovery rate is 101.5%, and repeated experiment RSD is 4.8%, can satisfy quantitative analysis needs.
1 rate of recovery of table and repeatability
Detailed description of the invention
Fig. 1: 0.1mg/mL standard working solution chromatogram under 1 chromatographic condition of present example；
Fig. 2: water base adhesive sample chromatogram figure under 1 chromatographic condition of present example.
Specific embodiment
The present invention is described further below in conjunction with example, but is not the limitation present invention.
Embodiment 1:
1. instrument and reagent:
Tributyl 2-acetylcitrate [purity is greater than 97%, uncommon love (Shanghai) the chemical conversion industry Development Co., Ltd of ladder], chromatography
Pure grade acetonitrile.
(waters is public for ACQUITY UPLC I-Class Ultra Performance Liquid Chromatography instrument (waters company), PDA detector
Department), 3 chromatographic work station of Empower (waters company)；BP221S electronic balance (sensibility reciprocal 0.0001g, German Sartorius
Company)；VX-2500 type turbula shaker (HENRY TROEMNER LLC company, the U.S.)；Milli-Q ultrapure water machine (the U.S.
Millipore company)；The organic filter membrane of micropore (0.22 μm, Shanghai ANPEL Scientific Instrument Co., Ltd.).
2. sample treatment:
It weighs 0.5g water base adhesive sample and is placed in conical flask, 10mL acetonitrile solution is added, it is rear that 150mg C is added18Dispersed solid phase
It is molten to obtain sample to be tested with 0.22 μm of organic membrane filtration after taking a small amount of extract liquor to be centrifugated by extractant, vortex oscillation 5min
Liquid.
3. standard working solution:
Be formulated as follows 5 concentration tributyl 2-acetylcitrate standard working solution (0.01mg/mL, 0.05mg/mL,
0.1mg/mL, 0.5mg/mL and 1mg/mL).
4. sample measures:
Measure the chromatographic condition used are as follows: chromatographic column: Atlantis T33mm×100mm；Column temperature: 30 DEG C；Column
Flow velocity: 0.6mL/min；Sample volume: 2 μ L；Detection wavelength: 212nm.Mobile phase A: water；Mobile phase B: acetonitrile；Gradient elution journey
Sequence: 0~15min, acetonitrile and water ratio are linearly risen to 100% acetonitrile by 20:80；15~20min, 100% acetonitrile.Gradient elution
20min。
The standard working solution for respectively taking 0.5mL various concentration carries out UPLC-UV according to the sequence of concentration from low to high respectively
The mass concentration (x, mg/L) of the UV peak area (y) measured and standard solution is carried out linear regression analysis, obtains target by measurement
The calibration curve equation of compound are as follows: y=752.93x+8365.3, coefficient R2It is 0.9995.
Sample after extraction is measured, it is qualitative with retention time, to measure object peak area value, it is bent to substitute into standard
Line equation acquires the content of tributyl 2-acetylcitrate in sample.(sample measures chromatogram referring to fig. 2)
The testing result of object in 2 sample A of table
Embodiment 2:
Specific detecting step is as described in Example 1, selects another water base adhesive sample B, as a result table 3.
The testing result of object in 3 sample B of table
Embodiment 3:
Specific detecting step is as described in Example 1, selects another water base adhesive sample C, as a result table 4.
The testing result of object in 4 sample C of table
Claims (6)
1. the measuring method of tributyl 2-acetylcitrate content in a kind of water base adhesive, which comprises the steps of:
Step 1) with the tributyl 2-acetylcitrate in acetonitrile extraction water base adhesive sample, the agent of C18 dispersive solid-phase extraction, whirlpool is added
It is centrifugated after rotation oscillation, takes supernatant liquid filtering film, obtain the sample solution to be tested；
Step 2) prepare tributyl 2-acetylcitrate calibration curve solution；
Step 3) with Ultra Performance Liquid Chromatography instrument using acetonitrile and water as eluent gradient elution analysis the sample solution to be tested and standard curve
Solution, quantified by external standard method measure tributyl 2-acetylcitrate；Three fourth of acetyl tributyl citrate in raw water base rubber is calculated according to measurement result
The content of ester.
2. the measuring method of tributyl 2-acetylcitrate content in water base adhesive as described in claim 1, it is characterised in that: described
Step 3) in chromatographic condition are as follows: chromatographic column isGradient elution program: 0~
15min, acetonitrile and water ratio are linearly risen to 100% acetonitrile by 20:80；15~20min, 100% acetonitrile；
Column temperature: 20~40 DEG C；Flow velocity: 0.3~0.6mL/min；Sample volume: 1~5 μ L；Detector is diode array detector,
Detection wavelength is 212nm.
3. the measuring method of tributyl 2-acetylcitrate content in water base adhesive as claimed in claim 2, it is characterised in that: described
Column temperature is 30 DEG C, flow velocity 0.6mL/min, and sample volume is 2 μ L.
4. the measuring method of tributyl 2-acetylcitrate content in water base adhesive as described in claim 1, it is characterised in that: described
Step 1) in weigh 0.5~1g water base adhesive sample and be placed in conical flask, be added the acetonitrile solution of 5~20mL, vortex oscillation 5min,
After taking a small amount of extract liquor to be centrifugated, water base adhesive testing sample solution is obtained with 0.22 μm of organic membrane filtration.
5. the measuring method of tributyl 2-acetylcitrate content in water base adhesive as described in claim 1, it is characterised in that: described
Step 1) in centrifuge separation temperature be 20~25 DEG C, revolving speed be 10000~15000rpm, the time be 5~10min.
6. the measuring method of tributyl 2-acetylcitrate content in water base adhesive as described in claim 1, it is characterised in that: described
Step 2) in the concentration of tributyl 2-acetylcitrate calibration curve solution be followed successively by 0.01mg/mL, 0.05mg/mL, 0.1mg/
ML, 0.5mg/mL and 1mg/mL.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811119680.3A CN109507306B (en) | 2018-09-25 | 2018-09-25 | Method for determining acetyl tributyl citrate in water-based adhesive |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811119680.3A CN109507306B (en) | 2018-09-25 | 2018-09-25 | Method for determining acetyl tributyl citrate in water-based adhesive |
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| CN109507306A true CN109507306A (en) | 2019-03-22 |
| CN109507306B CN109507306B (en) | 2021-09-07 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111307980A (en) * | 2020-03-16 | 2020-06-19 | 河南中烟工业有限责任公司 | Pretreatment method and detection method for detecting water-based adhesive for cigarettes |
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| CN108152424A (en) * | 2018-02-08 | 2018-06-12 | 河南中烟工业有限责任公司 | The detection method of citric acid ester plasticizer content in a kind of cigarette paper wrapper |
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| CN103487542A (en) * | 2013-09-11 | 2014-01-01 | 湖南中烟工业有限责任公司 | Method for concurrently detecting 23 ester compounds in cigarette water-base adhesive |
| CN108152424A (en) * | 2018-02-08 | 2018-06-12 | 河南中烟工业有限责任公司 | The detection method of citric acid ester plasticizer content in a kind of cigarette paper wrapper |
| CN108426952A (en) * | 2018-02-08 | 2018-08-21 | 河南中烟工业有限责任公司 | The detection method of citric acid ester plasticizer content in a kind of essence spice for cigarette |
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Cited By (1)
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| CN111307980A (en) * | 2020-03-16 | 2020-06-19 | 河南中烟工业有限责任公司 | Pretreatment method and detection method for detecting water-based adhesive for cigarettes |
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