CN110398549A - The method of plasticiser is extracted in a kind of carclazyte - Google Patents

The method of plasticiser is extracted in a kind of carclazyte Download PDF

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Publication number
CN110398549A
CN110398549A CN201910618786.6A CN201910618786A CN110398549A CN 110398549 A CN110398549 A CN 110398549A CN 201910618786 A CN201910618786 A CN 201910618786A CN 110398549 A CN110398549 A CN 110398549A
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hexane
plasticiser
carclazyte
extracting
added
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宋立里
高冠勇
陈宁
崔韵升
谢惠
贾召鹏
费晓伟
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Shandong Jinsheng Cereals Oils And Foodstuffs Co Ltd
Jinsheng Grain And Oil Group Co Ltd
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Shandong Jinsheng Cereals Oils And Foodstuffs Co Ltd
Jinsheng Grain And Oil Group Co Ltd
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Priority to CN201910618786.6A priority Critical patent/CN110398549A/en
Publication of CN110398549A publication Critical patent/CN110398549A/en
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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
    • 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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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention discloses a kind of methods that plasticiser is extracted in carclazyte, belong to peanut oil extractive technique field, the method for plasticiser are extracted in a kind of carclazyte, comprising the following steps: 1) weigh 1g carclazyte in glass centrifuge tube；2) extractant extracting method is used, the n-hexane extractant of 5-20mL methanol saturation, extraction time 1-5min are added into glass centrifuge tube, Extracting temperature is 0-30 DEG C, obtains extracting solution；3) by obtained extracting solution in vortex mixed 2min, 2min is centrifuged with the revolving speed not less than 4000r/min；4) after being centrifuged, Aspirate supernatant is blown to using nitrogen under conditions of 40 DEG C close dry, obtains extract.The extracting method of plasticiser in a kind of carclazyte provided by the invention, recovery rate is high, residual is few, influence of the reduction of maximum possible because of reagent to extraction effect, the n-hexane extractant being saturated using methanol, is dissolved into the plasticiser in carclazyte sufficiently in extracting solution, extraction process is simple, it is easy to operate, efficient low-consume.

Description

The method of plasticiser is extracted in a kind of carclazyte
Technical field
The present invention relates to peanut oil extractive technique field, the method for plasticiser is extracted in specially a kind of carclazyte.
Background technique
Vegetable oil is our daily life indispensable requisites, but crude oil contains many impurity, such as colloid, dirt Angstrom, free fatty acid, pigment, slime etc., these impurity will cause damages to human health, while influence storage property, also Difficulty is brought to grease deep processing, it is necessary to is removed.In conventional refining processes, it is most important that degumming, decoloration and depickling work Sequence, wherein only atlapulgite adsorption bleaching process is simple, easy to operate, and the advantages that do not need water-oil separating.Atlapulgite is It is raw material with clay (mainly bentonite), is handled through inorganic acidifying or salt or other methods, then through made of water rinsing, drying Adsorbent, appearance is off-white powder, odorless, tasteless, nontoxic, and absorption property is very strong, can adsorb coloring matter, organic substance.
Atlapulgite has preferable de- as the decolorising agent in oil and fat refining process, and impurity plain to the dark color in crude oil Except effect, grease color after decolorizing purification is shallow, clarification, glossy, and stability is good, acid value is low, but due to atlapulgite itself Containing plasticiser, grease is polluted, so that increasing consumption refining in deodorising process behind, it is therefore desirable to by the modeling in carclazyte Agent extracts, however existing plasticiser extracting method not only complex steps, and time-consuming, laborious, and recovery rate is low.
Summary of the invention
(1) the technical issues of solving
1. technical problems to be solved
Aiming at the problems existing in the prior art, the purpose of the present invention is to provide in a kind of carclazyte extract plasticiser method, Have that recovery rate is high, advantage easy to operate, solve existing plasticiser extracting method not only complex steps, and it is time-consuming, take Power, the low problem of recovery rate.
(2) technical solution
To realize said extracted rate height, purpose easy to operate, the invention provides the following technical scheme: extracting plasticizing in a kind of carclazyte The method of agent, comprising the following steps:
1) 1g carclazyte is weighed in glass centrifuge tube；
2) extractant extracting method is used, the n-hexane extractant of 5-20mL methanol saturation is added into glass centrifuge tube, is extracted Time is 1-5min, and Extracting temperature is 0-30 DEG C, obtains extracting solution；
3) by obtained extracting solution in vortex mixed 2min, 2min is centrifuged with the revolving speed not less than 4000r/min；
4) after being centrifuged, Aspirate supernatant is blown to using nitrogen under conditions of 40 DEG C close dry, obtains extract；
5) to obtaining in extract, 2mL n-hexane is added, concussion mixes, and is purified liquid；
6) SPE(Solid Phase Extraction is taken) purification pillar, 5mL acetone is successively used, 5mL n-hexane crosses column purification, and efflux discards；
7) loading: liquid to be clean is added in purified SPE purification pillar；
8) it elutes: successively being eluted with 5mL n-hexane, 5mL4% acetone-hexane solution, collect efflux, it then will outflow Liquid drying, is then added 1mL n-hexane, obtains liquid to be determined；
9) GC-MS(gas chromatograph-mass spectrometer (GC-MS) is used) component and content of plasticiser in detection liquid to be determined.
Preferably, the loading flow velocity is 1mL/min, and the efflux dries concrete operations are as follows: in 40 DEG C of temperature, is delayed Under the conditions of slow nitrogen stream, volatilized after blowing close do.
Preferably, the GC-MS detection includes gas phase condition and Mass Spectrometry Conditions.
Preferably, the gas phase condition includes: 1. chromatographic column: HP-5MS capillary chromatographic column；2. injector temperature 280 ℃；3. shunt mode: Splitless injecting samples；4. carrier gas: helium (purity >=99.99%)；5. flow velocity 1mL/min；Sample volume 1ul.
Preferably, the Mass Spectrometry Conditions include: 1. mass spectrum transmission line temperature (Aux-2): 300 DEG C；2. the mode of ionization is electricity Sub- bombardment source (EI)；3. monitoring mode selects ion scan mode (SIM) ionizing energy 70eV；4. solvent delay 5min.
(3) beneficial effect
Compared with prior art, the present invention provides in a kind of carclazyte extract plasticiser method, have it is following the utility model has the advantages that
(1) in a kind of carclazyte provided by the invention plasticiser extracting method, recovery rate is high, and residual is few, the reduction of maximum possible Influence because of reagent to extraction effect.
(2) in a kind of carclazyte provided by the invention plasticiser extracting method, extraction process is simple, easy to operate, efficiently Low consumption.
(3) in a kind of carclazyte provided by the invention plasticiser extracting method, the whole process used time of extraction is short, improves Extraction efficiency is suitble to batch extracting.
(4) in a kind of carclazyte provided by the invention plasticiser extracting method, using methanol be saturated n-hexane extractant, It is dissolved into the plasticiser in carclazyte sufficiently in extracting solution.
(5) in a kind of carclazyte provided by the invention plasticiser extracting method, using methanol saturation n-hexane, just oneself A small amount of reagent such as alkane, acetone reduces the type that drug uses, as far as possible harm of the reduction drug to human body and environment.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution in the embodiment of the present invention is clearly and completely retouched It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention In embodiment, every other implementation obtained by those of ordinary skill in the art without making creative efforts Example, shall fall within the protection scope of the present invention.
Embodiment one:
The method of plasticiser is extracted in a kind of carclazyte, comprising the following steps:
1) 1g carclazyte is weighed in glass centrifuge tube；
2) extractant extracting method is used, the n-hexane extractant of 5mL methanol saturation, extraction time are added into glass centrifuge tube For 1min, Extracting temperature is 10 DEG C, obtains extracting solution；
3) by obtained extracting solution in vortex mixed 2min, 2min is centrifuged with the revolving speed not less than 4000r/min；
4) after being centrifuged, Aspirate supernatant is blown to using nitrogen under conditions of 40 DEG C close dry, obtains extract；
5) to obtaining in extract, 2mL n-hexane is added, concussion mixes, and is purified liquid；
6) SPE(Solid Phase Extraction is taken) purification pillar, 5mL acetone is successively used, 5mL n-hexane crosses column purification, and efflux discards；
7) loading: liquid to be clean is added in purified SPE purification pillar；
8) it elutes: successively being eluted with 5mL n-hexane, 5mL4% acetone-hexane solution, collect efflux, it then will outflow Liquid drying, is then added 1mL n-hexane, obtains liquid to be determined；
9) GC-MS(gas chromatograph-mass spectrometer (GC-MS) is used) component and content of plasticiser in detection liquid to be determined.
Further, loading flow velocity is 1mL/min, and efflux dries concrete operations are as follows: in 40 DEG C of temperature, slow nitrogen Under the conditions of stream, volatilized after blowing close do.
Further, GC-MS detection includes gas phase condition and Mass Spectrometry Conditions, and gas phase condition includes: 1. chromatographic column: HP-5MS Capillary chromatographic column；2. 280 DEG C of injector temperature；3. shunt mode: Splitless injecting samples；4. carrier gas: helium (purity >= 99.99%)；5. flow velocity 1mL/min；Sample volume 1ul；Mass Spectrometry Conditions include: 1. mass spectrum transmission line temperature (Aux-2): 300 DEG C；② Ionization mode is electron bombardment ionization source (EI)；3. monitoring mode selects ion scan mode (SIM) ionizing energy 70eV；4. solvent prolongs Slow 5min.
Embodiment two:
The method of plasticiser is extracted in a kind of carclazyte, comprising the following steps:
1) 1g carclazyte is weighed in glass centrifuge tube；
2) extractant extracting method is used, the n-hexane extractant of 10mL methanol saturation is added into glass centrifuge tube, when extraction Between be 1min, Extracting temperature be 10 DEG C, obtain extracting solution；
3) by obtained extracting solution in vortex mixed 2min, 2min is centrifuged with the revolving speed not less than 4000r/min；
4) after being centrifuged, Aspirate supernatant is blown to using nitrogen under conditions of 40 DEG C close dry, obtains extract；
5) to obtaining in extract, 2mL n-hexane is added, concussion mixes, and is purified liquid；
6) SPE(Solid Phase Extraction is taken) purification pillar, 5mL acetone is successively used, 5mL n-hexane crosses column purification, and efflux discards；
7) loading: liquid to be clean is added in purified SPE purification pillar；
8) it elutes: successively being eluted with 5mL n-hexane, 5mL4% acetone-hexane solution, collect efflux, it then will outflow Liquid drying, is then added 1mL n-hexane, obtains liquid to be determined；
9) GC-MS(gas chromatograph-mass spectrometer (GC-MS) is used) component and content of plasticiser in detection liquid to be determined.
Further, loading flow velocity is 1mL/min, and efflux dries concrete operations are as follows: in 40 DEG C of temperature, slow nitrogen Under the conditions of stream, volatilized after blowing close do.
Further, GC-MS detection includes gas phase condition and Mass Spectrometry Conditions, and gas phase condition includes: 1. chromatographic column: HP-5MS Capillary chromatographic column；2. 280 DEG C of injector temperature；3. shunt mode: Splitless injecting samples；4. carrier gas: helium (purity >= 99.99%)；5. flow velocity 1mL/min；Sample volume 1ul；Mass Spectrometry Conditions include: 1. mass spectrum transmission line temperature (Aux-2): 300 DEG C；② Ionization mode is electron bombardment ionization source (EI)；3. monitoring mode selects ion scan mode (SIM) ionizing energy 70eV；4. solvent prolongs Slow 5min.
Embodiment three:
The method of plasticiser is extracted in a kind of carclazyte, comprising the following steps:
1) 1g carclazyte is weighed in glass centrifuge tube；
2) extractant extracting method is used, the n-hexane extractant of 20mL methanol saturation is added into glass centrifuge tube, when extraction Between be 1min, Extracting temperature be 10 DEG C, obtain extracting solution；
3) by obtained extracting solution in vortex mixed 2min, 2min is centrifuged with the revolving speed not less than 4000r/min；
4) after being centrifuged, Aspirate supernatant is blown to using nitrogen under conditions of 40 DEG C close dry, obtains extract；
5) to obtaining in extract, 2mL n-hexane is added, concussion mixes, and is purified liquid；
6) SPE(Solid Phase Extraction is taken) purification pillar, 5mL acetone is successively used, 5mL n-hexane crosses column purification, and efflux discards；
7) loading: liquid to be clean is added in purified SPE purification pillar；
8) it elutes: successively being eluted with 5mL n-hexane, 5mL4% acetone-hexane solution, collect efflux, it then will outflow Liquid drying, is then added 1mL n-hexane, obtains liquid to be determined；
9) GC-MS(gas chromatograph-mass spectrometer (GC-MS) is used) component and content of plasticiser in detection liquid to be determined.
Further, loading flow velocity is 1mL/min, and efflux dries concrete operations are as follows: in 40 DEG C of temperature, slow nitrogen Under the conditions of stream, volatilized after blowing close do.
Further, GC-MS detection includes gas phase condition and Mass Spectrometry Conditions, and gas phase condition includes: 1. chromatographic column: HP-5MS Capillary chromatographic column；2. 280 DEG C of injector temperature；3. shunt mode: Splitless injecting samples；4. carrier gas: helium (purity >= 99.99%)；5. flow velocity 1mL/min；Sample volume 1ul；Mass Spectrometry Conditions include: 1. mass spectrum transmission line temperature (Aux-2): 300 DEG C；② Ionization mode is electron bombardment ionization source (EI)；3. monitoring mode selects ion scan mode (SIM) ionizing energy 70eV；4. solvent prolongs Slow 5min.
Experimental example one:
Difference, which extracts reagent, influences atlapulgite plasticiser extraction effect
Extractant type DBP(mg/kg) DEHP(mg/kg) DINP(mg/kg) Extract total amount
N-hexane 0.0202 1.5772 0.0008 1.5982
Second eyeball 0.0456 0.2536 0.0054 0.3046
Methanol 0.0861 0.8856 0.0044 0.9761
The n-hexane of methanol saturation 0.066 3.5544 0.0018 3.6222
According to the experimental results:
It tests and the different extraction effects for extracting reagent is compared, the n-hexane extraction effect being saturated using methanol is best, energy The nonpolarity of n-hexane and the polarity of methanol are comprehensively utilized, the polar group of plasticiser and non-polar group are all effectively extracted Come.
Experimental example two:
The extractant of different amounts is taken by embodiment one to three, carries out experimental data comparison, the result is as follows:
Methanol, which is saturated n-hexane extractant dosage, influences atlapulgite content of plasticizing agent
Solid-liquid ratio (carclazyte: methanol is saturated n-hexane) DBP(mg/kg) DEHP(mg/kg) DINP(mg/kg) Extract total amount
1:5 0.0524 1.3312 0.0006 1.3842
1:10 0.066 3.5544 0.0018 3.6222
1:20 0.0078 3.1972 0.0054 3.2104
According to the experimental results:
Test to the dosage for extracting reagent probed into the result shows that, be optimised process with 10mL extractant effect, therefore real It tests and primarily determines the n-hexane for using 10mL methanol to be saturated as optimum extraction agent dosage.
Example IV:
The method of plasticiser is extracted in a kind of carclazyte, comprising the following steps:
1) 1g carclazyte is weighed in glass centrifuge tube；
2) extractant extracting method is used, the n-hexane extractant of 10mL methanol saturation is added into glass centrifuge tube, when extraction Between be 1min, Extracting temperature be 10 DEG C, obtain extracting solution；
3) by obtained extracting solution in vortex mixed 2min, 2min is centrifuged with the revolving speed not less than 4000r/min；
4) after being centrifuged, Aspirate supernatant is blown to using nitrogen under conditions of 40 DEG C close dry, obtains extract；
5) to obtaining in extract, 2mL n-hexane is added, concussion mixes, and is purified liquid；
6) SPE(Solid Phase Extraction is taken) purification pillar, 5mL acetone is successively used, 5mL n-hexane crosses column purification, and efflux discards；
7) loading: liquid to be clean is added in purified SPE purification pillar；
8) it elutes: successively being eluted with 5mL n-hexane, 5mL4% acetone-hexane solution, collect efflux, it then will outflow Liquid drying, is then added 1mL n-hexane, obtains liquid to be determined；
9) GC-MS(gas chromatograph-mass spectrometer (GC-MS) is used) component and content of plasticiser in detection liquid to be determined.
Further, loading flow velocity is 1mL/min, and efflux dries concrete operations are as follows: in 40 DEG C of temperature, slow nitrogen Under the conditions of stream, volatilized after blowing close do.
Further, GC-MS detection includes gas phase condition and Mass Spectrometry Conditions, and gas phase condition includes: 1. chromatographic column: HP-5MS Capillary chromatographic column；2. 280 DEG C of injector temperature；3. shunt mode: Splitless injecting samples；4. carrier gas: helium (purity >= 99.99%)；5. flow velocity 1mL/min；Sample volume 1ul；Mass Spectrometry Conditions include: 1. mass spectrum transmission line temperature (Aux-2): 300 DEG C；② Ionization mode is electron bombardment ionization source (EI)；3. monitoring mode selects ion scan mode (SIM) ionizing energy 70eV；4. solvent prolongs Slow 5min.
Embodiment five:
The method of plasticiser is extracted in a kind of carclazyte, comprising the following steps:
1) 1g carclazyte is weighed in glass centrifuge tube；
2) extractant extracting method is used, the n-hexane extractant of 10mL methanol saturation is added into glass centrifuge tube, when extraction Between be 3min, Extracting temperature be 10 DEG C, obtain extracting solution；
3) by obtained extracting solution in vortex mixed 2min, 2min is centrifuged with the revolving speed not less than 4000r/min；
4) after being centrifuged, Aspirate supernatant is blown to using nitrogen under conditions of 40 DEG C close dry, obtains extract；
5) to obtaining in extract, 2mL n-hexane is added, concussion mixes, and is purified liquid；
6) SPE(Solid Phase Extraction is taken) purification pillar, 5mL acetone is successively used, 5mL n-hexane crosses column purification, and efflux discards；
7) loading: liquid to be clean is added in purified SPE purification pillar；
8) it elutes: successively being eluted with 5mL n-hexane, 5mL4% acetone-hexane solution, collect efflux, it then will outflow Liquid drying, is then added 1mL n-hexane, obtains liquid to be determined；
9) GC-MS(gas chromatograph-mass spectrometer (GC-MS) is used) component and content of plasticiser in detection liquid to be determined.
Further, loading flow velocity is 1mL/min, and efflux dries concrete operations are as follows: in 40 DEG C of temperature, slow nitrogen Under the conditions of stream, volatilized after blowing close do.
Further, GC-MS detection includes gas phase condition and Mass Spectrometry Conditions, and gas phase condition includes: 1. chromatographic column: HP-5MS Capillary chromatographic column；2. 280 DEG C of injector temperature；3. shunt mode: Splitless injecting samples；4. carrier gas: helium (purity >= 99.99%)；5. flow velocity 1mL/min；Sample volume 1ul；Mass Spectrometry Conditions include: 1. mass spectrum transmission line temperature (Aux-2): 300 DEG C；② Ionization mode is electron bombardment ionization source (EI)；3. monitoring mode selects ion scan mode (SIM) ionizing energy 70eV；4. solvent prolongs Slow 5min.
Embodiment six:
The method of plasticiser is extracted in a kind of carclazyte, comprising the following steps:
1) 1g carclazyte is weighed in glass centrifuge tube；
2) extractant extracting method is used, the n-hexane extractant of 10mL methanol saturation is added into glass centrifuge tube, when extraction Between be 5min, Extracting temperature be 10 DEG C, obtain extracting solution；
3) by obtained extracting solution in vortex mixed 2min, 2min is centrifuged with the revolving speed not less than 4000r/min；
4) after being centrifuged, Aspirate supernatant is blown to using nitrogen under conditions of 40 DEG C close dry, obtains extract；
5) to obtaining in extract, 2mL n-hexane is added, concussion mixes, and is purified liquid；
6) SPE(Solid Phase Extraction is taken) purification pillar, 5mL acetone is successively used, 5mL n-hexane crosses column purification, and efflux discards；
7) loading: liquid to be clean is added in purified SPE purification pillar；
8) it elutes: successively being eluted with 5mL n-hexane, 5mL4% acetone-hexane solution, collect efflux, it then will outflow Liquid drying, is then added 1mL n-hexane, obtains liquid to be determined；
9) GC-MS(gas chromatograph-mass spectrometer (GC-MS) is used) component and content of plasticiser in detection liquid to be determined.
Further, loading flow velocity is 1mL/min, and efflux dries concrete operations are as follows: in 40 DEG C of temperature, slow nitrogen Under the conditions of stream, volatilized after blowing close do.
Further, GC-MS detection includes gas phase condition and Mass Spectrometry Conditions, and gas phase condition includes: 1. chromatographic column: HP-5MS Capillary chromatographic column；2. 280 DEG C of injector temperature；3. shunt mode: Splitless injecting samples；4. carrier gas: helium (purity >= 99.99%)；5. flow velocity 1mL/min；Sample volume 1ul；Mass Spectrometry Conditions include: 1. mass spectrum transmission line temperature (Aux-2): 300 DEG C；② Ionization mode is electron bombardment ionization source (EI)；3. monitoring mode selects ion scan mode (SIM) ionizing energy 70eV；4. solvent prolongs Slow 5min.
Experimental example three:
Atlapulgite content of plasticizing agent is influenced by being probed into different extraction times by example IV to six, carries out experimental data Comparison, the result is as follows:
Extraction time influences atlapulgite content of plasticizing agent
Extraction time (min) DBP(mg/kg) DEHP(mg/kg) DINP(mg/kg) Extract total amount
1 0.035 1.7852 0.0009 1.8211
3 0.066 3.5544 0.0018 3.6222
5 0.069 3.5042 0.002 3.5752
From upper table experimental result:
Test to extraction time probed into the result shows that, extraction time be 3min extractant effect it is best, therefore test just It walks and determines that extraction time is 3min.
Embodiment seven:
The method of plasticiser is extracted in a kind of carclazyte, comprising the following steps:
1) 1g carclazyte is weighed in glass centrifuge tube；
2) extractant extracting method is used, the n-hexane extractant of 10mL methanol saturation is added into glass centrifuge tube, when extraction Between be 3min, Extracting temperature be 0 DEG C, obtain extracting solution；
3) by obtained extracting solution in vortex mixed 2min, 2min is centrifuged with the revolving speed not less than 4000r/min；
4) after being centrifuged, Aspirate supernatant is blown to using nitrogen under conditions of 40 DEG C close dry, obtains extract；
5) to obtaining in extract, 2mL n-hexane is added, concussion mixes, and is purified liquid；
6) SPE(Solid Phase Extraction is taken) purification pillar, 5mL acetone is successively used, 5mL n-hexane crosses column purification, and efflux discards；
7) loading: liquid to be clean is added in purified SPE purification pillar；
8) it elutes: successively being eluted with 5mL n-hexane, 5mL4% acetone-hexane solution, collect efflux, it then will outflow Liquid drying, is then added 1mL n-hexane, obtains liquid to be determined；
9) GC-MS(gas chromatograph-mass spectrometer (GC-MS) is used) component and content of plasticiser in detection liquid to be determined.
Further, loading flow velocity is 1mL/min, and efflux dries concrete operations are as follows: in 40 DEG C of temperature, slow nitrogen Under the conditions of stream, volatilized after blowing close do.
Further, GC-MS detection includes gas phase condition and Mass Spectrometry Conditions, and gas phase condition includes: 1. chromatographic column: HP-5MS Capillary chromatographic column；2. 280 DEG C of injector temperature；3. shunt mode: Splitless injecting samples；4. carrier gas: helium (purity >= 99.99%)；5. flow velocity 1mL/min；Sample volume 1ul；Mass Spectrometry Conditions include: 1. mass spectrum transmission line temperature (Aux-2): 300 DEG C；② Ionization mode is electron bombardment ionization source (EI)；3. monitoring mode selects ion scan mode (SIM) ionizing energy 70eV；4. solvent prolongs Slow 5min.
Embodiment eight:
The method of plasticiser is extracted in a kind of carclazyte, comprising the following steps:
1) 1g carclazyte is weighed in glass centrifuge tube；
2) extractant extracting method is used, the n-hexane extractant of 10mL methanol saturation is added into glass centrifuge tube, when extraction Between be 3min, Extracting temperature be 10 DEG C, obtain extracting solution；
3) by obtained extracting solution in vortex mixed 2min, 2min is centrifuged with the revolving speed not less than 4000r/min；
4) after being centrifuged, Aspirate supernatant is blown to using nitrogen under conditions of 40 DEG C close dry, obtains extract；
5) to obtaining in extract, 2mL n-hexane is added, concussion mixes, and is purified liquid；
6) SPE(Solid Phase Extraction is taken) purification pillar, 5mL acetone is successively used, 5mL n-hexane crosses column purification, and efflux discards；
7) loading: liquid to be clean is added in purified SPE purification pillar；
8) it elutes: successively being eluted with 5mL n-hexane, 5mL4% acetone-hexane solution, collect efflux, it then will outflow Liquid drying, is then added 1mL n-hexane, obtains liquid to be determined；
9) GC-MS(gas chromatograph-mass spectrometer (GC-MS) is used) component and content of plasticiser in detection liquid to be determined.
Further, loading flow velocity is 1mL/min, and efflux dries concrete operations are as follows: in 40 DEG C of temperature, slow nitrogen Under the conditions of stream, volatilized after blowing close do.
Further, GC-MS detection includes gas phase condition and Mass Spectrometry Conditions, and gas phase condition includes: 1. chromatographic column: HP-5MS Capillary chromatographic column；2. 280 DEG C of injector temperature；3. shunt mode: Splitless injecting samples；4. carrier gas: helium (purity >= 99.99%)；5. flow velocity 1mL/min；Sample volume 1ul；Mass Spectrometry Conditions include: 1. mass spectrum transmission line temperature (Aux-2): 300 DEG C；② Ionization mode is electron bombardment ionization source (EI)；3. monitoring mode selects ion scan mode (SIM) ionizing energy 70eV；4. solvent prolongs Slow 5min.
Embodiment nine:
The method of plasticiser is extracted in a kind of carclazyte, comprising the following steps:
1) 1g carclazyte is weighed in glass centrifuge tube；
2) extractant extracting method is used, the n-hexane extractant of 10mL methanol saturation is added into glass centrifuge tube, when extraction Between be 3min, Extracting temperature be 20 DEG C, obtain extracting solution；
3) by obtained extracting solution in vortex mixed 2min, 2min is centrifuged with the revolving speed not less than 4000r/min；
4) after being centrifuged, Aspirate supernatant is blown to using nitrogen under conditions of 40 DEG C close dry, obtains extract；
5) to obtaining in extract, 2mL n-hexane is added, concussion mixes, and is purified liquid；
6) SPE(Solid Phase Extraction is taken) purification pillar, 5mL acetone is successively used, 5mL n-hexane crosses column purification, and efflux discards；
7) loading: liquid to be clean is added in purified SPE purification pillar；
8) it elutes: successively being eluted with 5mL n-hexane, 5mL4% acetone-hexane solution, collect efflux, it then will outflow Liquid drying, is then added 1mL n-hexane, obtains liquid to be determined；
9) GC-MS(gas chromatograph-mass spectrometer (GC-MS) is used) component and content of plasticiser in detection liquid to be determined.
Further, loading flow velocity is 1mL/min, and efflux dries concrete operations are as follows: in 40 DEG C of temperature, slow nitrogen Under the conditions of stream, volatilized after blowing close do.
Further, GC-MS detection includes gas phase condition and Mass Spectrometry Conditions, and gas phase condition includes: 1. chromatographic column: HP-5MS Capillary chromatographic column；2. 280 DEG C of injector temperature；3. shunt mode: Splitless injecting samples；4. carrier gas: helium (purity >= 99.99%)；5. flow velocity 1mL/min；Sample volume 1ul；Mass Spectrometry Conditions include: 1. mass spectrum transmission line temperature (Aux-2): 300 DEG C；② Ionization mode is electron bombardment ionization source (EI)；3. monitoring mode selects ion scan mode (SIM) ionizing energy 70eV；4. solvent prolongs Slow 5min.
Embodiment ten:
The method of plasticiser is extracted in a kind of carclazyte, comprising the following steps:
1) 1g carclazyte is weighed in glass centrifuge tube；
2) extractant extracting method is used, the n-hexane extractant of 10mL methanol saturation is added into glass centrifuge tube, when extraction Between be 3min, Extracting temperature be 30 DEG C, obtain extracting solution；
3) by obtained extracting solution in vortex mixed 2min, 2min is centrifuged with the revolving speed not less than 4000r/min；
4) after being centrifuged, Aspirate supernatant is blown to using nitrogen under conditions of 40 DEG C close dry, obtains extract；
5) to obtaining in extract, 2mL n-hexane is added, concussion mixes, and is purified liquid；
6) SPE(Solid Phase Extraction is taken) purification pillar, 5mL acetone is successively used, 5mL n-hexane crosses column purification, and efflux discards；
7) loading: liquid to be clean is added in purified SPE purification pillar；
8) it elutes: successively being eluted with 5mL n-hexane, 5mL4% acetone-hexane solution, collect efflux, it then will outflow Liquid drying, is then added 1mL n-hexane, obtains liquid to be determined；
9) GC-MS(gas chromatograph-mass spectrometer (GC-MS) is used) component and content of plasticiser in detection liquid to be determined.
Further, loading flow velocity is 1mL/min, and efflux dries concrete operations are as follows: in 40 DEG C of temperature, slow nitrogen Under the conditions of stream, volatilized after blowing close do.
Further, GC-MS detection includes gas phase condition and Mass Spectrometry Conditions, and gas phase condition includes: 1. chromatographic column: HP-5MS Capillary chromatographic column；2. 280 DEG C of injector temperature；3. shunt mode: Splitless injecting samples；4. carrier gas: helium (purity >= 99.99%)；5. flow velocity 1mL/min；Sample volume 1ul；Mass Spectrometry Conditions include: 1. mass spectrum transmission line temperature (Aux-2): 300 DEG C；② Ionization mode is electron bombardment ionization source (EI)；3. monitoring mode selects ion scan mode (SIM) ionizing energy 70eV；4. solvent prolongs Slow 5min.
Experimental example four:
Atlapulgite content of plasticizing agent is influenced by being probed into different Extracting temperatures by embodiment seven to ten, carries out experimental data Comparison, the result is as follows:
Extracting temperature influences atlapulgite content of plasticizing agent
Extracting temperature (DEG C) DBP(mg/kg) DEHP(mg/kg) DINP(mg/kg) Extract total amount
0 0.0427 1.1212 0.0012 1.1651
10 0.058 2.8792 0.0016 2.9388
20 0.066 3.5544 0.0018 3.6222
30 0.071 3.5322 0.0017 3.6049
From upper table experimental result:
Test to Extracting temperature probed into the result shows that, its extractant effect is best when Extracting temperature is 20 DEG C, therefore real It tests and primarily determines that Extracting temperature is 20 DEG C.
Therefore, the optimal extraction process of plasticiser in atlapulgite is tentatively obtained by the experiment of experimental example one to four are as follows: For the n-hexane for using methanol to be saturated as extractant, atlapulgite amount is 1g, and extracting solution dosage is 10mL, and extraction time is 3min, Extracting temperature are 20 DEG C.
(2) the foregoing is intended to be a preferred embodiment of the present invention；But protection scope of the present invention is not limited to In this.Anyone skilled in the art in the technical scope disclosed by the present invention, technical side according to the present invention Case and its improvement design are subject to equivalent substitution or change, should be covered by the scope of protection of the present invention.

Claims (5)

1. extracting the method for plasticiser in a kind of carclazyte, it is characterised in that: the following steps are included:
1) 1g carclazyte is weighed in glass centrifuge tube；
2) extractant extracting method is used, the n-hexane extractant of 5-20mL methanol saturation is added into glass centrifuge tube, is extracted Time is 1-5min, and Extracting temperature is 0-30 DEG C, obtains extracting solution；
3) by obtained extracting solution in vortex mixed 2min, 2min is centrifuged with the revolving speed not less than 4000r/min；
4) after being centrifuged, Aspirate supernatant is blown to using nitrogen under conditions of 40 DEG C close dry, obtains extract；
5) to obtaining in extract, 2mL n-hexane is added, concussion mixes, and is purified liquid；
6) SPE(Solid Phase Extraction is taken) purification pillar, 5mL acetone is successively used, 5mL n-hexane crosses column purification, and efflux discards；
7) loading: liquid to be clean is added in purified SPE purification pillar；
8) it elutes: successively being eluted with 5mL n-hexane, 5mL4% acetone-hexane solution, collect efflux, it then will outflow Liquid drying, is then added 1mL n-hexane, obtains liquid to be determined；
9) GC-MS(gas chromatograph-mass spectrometer (GC-MS) is used) component and content of plasticiser in detection liquid to be determined.
2. extracting the method for plasticiser in a kind of carclazyte according to claim 1, it is characterised in that: the loading flow velocity is 1mL/min, the efflux dry concrete operations are as follows: under the conditions of 40 DEG C of temperature, slow nitrogen stream, volatilize after blowing close do.
3. extracting the method for plasticiser in a kind of carclazyte according to claim 1, it is characterised in that: the GC-MS detection Including gas phase condition and Mass Spectrometry Conditions.
4. extracting the method for plasticiser in a kind of carclazyte according to claim 3, it is characterised in that: the gas phase condition packet It includes: 1. chromatographic column: HP-5MS capillary chromatographic column；2. 280 DEG C of injector temperature；3. shunt mode: Splitless injecting samples；4. carrying Gas: helium (purity >=99.99%)；5. flow velocity 1mL/min；Sample volume 1ul.
5. extracting the method for plasticiser in a kind of carclazyte according to claim 3, it is characterised in that: the Mass Spectrometry Conditions packet It includes: 1. mass spectrum transmission line temperature (Aux-2): 300 DEG C；2. ionization mode is electron bombardment ionization source (EI)；3. monitoring mode select from Sub- scan pattern (SIM) ionizing energy 70eV；4. solvent delay 5min.
CN201910618786.6A 2019-07-10 2019-07-10 The method of plasticiser is extracted in a kind of carclazyte Pending CN110398549A (en)

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Application publication date: 20191101