CN108196020A - The separation method of persistence organic pollutant in a kind of aquatic products - Google Patents
The separation method of persistence organic pollutant in a kind of aquatic products Download PDFInfo
- Publication number
- CN108196020A CN108196020A CN201711369931.9A CN201711369931A CN108196020A CN 108196020 A CN108196020 A CN 108196020A CN 201711369931 A CN201711369931 A CN 201711369931A CN 108196020 A CN108196020 A CN 108196020A
- Authority
- CN
- China
- Prior art keywords
- aquatic products
- weight
- parts
- separation method
- hydrogel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000002957 persistent organic pollutant Substances 0.000 title claims abstract description 40
- 230000002688 persistence Effects 0.000 title claims abstract description 25
- 238000000926 separation method Methods 0.000 title claims abstract description 25
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000000047 product Substances 0.000 claims abstract description 47
- 238000005119 centrifugation Methods 0.000 claims abstract description 32
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000003960 organic solvent Substances 0.000 claims abstract description 23
- 239000000284 extract Substances 0.000 claims abstract description 17
- 239000006228 supernatant Substances 0.000 claims abstract description 16
- 239000003463 adsorbent Substances 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 230000010355 oscillation Effects 0.000 claims abstract description 12
- 230000009514 concussion Effects 0.000 claims abstract description 8
- 238000002390 rotary evaporation Methods 0.000 claims abstract description 8
- 239000000017 hydrogel Substances 0.000 claims description 51
- 238000001035 drying Methods 0.000 claims description 41
- 238000005406 washing Methods 0.000 claims description 38
- 238000000034 method Methods 0.000 claims description 35
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 24
- 230000008569 process Effects 0.000 claims description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 21
- 239000000741 silica gel Substances 0.000 claims description 21
- 229910002027 silica gel Inorganic materials 0.000 claims description 21
- 238000007654 immersion Methods 0.000 claims description 14
- 238000010298 pulverizing process Methods 0.000 claims description 14
- 238000002414 normal-phase solid-phase extraction Methods 0.000 claims description 9
- 238000004891 communication Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 239000012046 mixed solvent Substances 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- 238000000638 solvent extraction Methods 0.000 claims description 8
- 239000000499 gel Substances 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- 210000003205 muscle Anatomy 0.000 claims description 7
- 230000003534 oscillatory effect Effects 0.000 claims description 7
- 235000019353 potassium silicate Nutrition 0.000 claims description 7
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 238000012544 monitoring process Methods 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 230000000694 effects Effects 0.000 description 7
- 239000003921 oil Substances 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 4
- 230000006378 damage Effects 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 238000005227 gel permeation chromatography Methods 0.000 description 3
- 230000036541 health Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 241001465754 Metazoa Species 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001727 in vivo Methods 0.000 description 2
- 210000005036 nerve Anatomy 0.000 description 2
- 239000003993 organochlorine pesticide Substances 0.000 description 2
- 230000002085 persistent effect Effects 0.000 description 2
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 2
- 238000000899 pressurised-fluid extraction Methods 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- MVWHGTYKUMDIHL-UHFFFAOYSA-N 2,2',4,4',5,5'-hexachlorobiphenyl Chemical compound C1=C(Cl)C(Cl)=CC(Cl)=C1C1=CC(Cl)=C(Cl)C=C1Cl MVWHGTYKUMDIHL-UHFFFAOYSA-N 0.000 description 1
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- 241001635206 Conger conger Species 0.000 description 1
- 102000002322 Egg Proteins Human genes 0.000 description 1
- 108010000912 Egg Proteins Proteins 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 238000000944 Soxhlet extraction Methods 0.000 description 1
- 208000031320 Teratogenesis Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 230000035558 fertility Effects 0.000 description 1
- 210000003754 fetus Anatomy 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000003102 growth factor Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229940088597 hormone Drugs 0.000 description 1
- 239000005556 hormone Substances 0.000 description 1
- 235000020256 human milk Nutrition 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000000622 liquid--liquid extraction Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000007886 mutagenicity Effects 0.000 description 1
- 231100000299 mutagenicity Toxicity 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 210000004681 ovum Anatomy 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- PANBYUAFMMOFOV-UHFFFAOYSA-N sodium;sulfuric acid Chemical compound [Na].OS(O)(=O)=O PANBYUAFMMOFOV-UHFFFAOYSA-N 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006277 sulfonation reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
- G01N33/1826—Organic contamination in water
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
- G01N2001/4061—Solvent extraction
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Silicon Compounds (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The present invention relates to pollutant monitoring field, in particular to a kind of separation method of persistence organic pollutant in aquatic products.The separation method of persistence organic pollutant, includes the following steps in a kind of aquatic products：By the extractant of middle addition 15 ~ 17 parts by weight of the sample after the concentrated sulfuric acid is cleared up, after 1 ~ 5min of vortex oscillation, supernatant upper strata organic solvent is transferred to another centrifuge tube after centrifugation；Again to the extractant by adding in 15 ~ 17 parts by weight in treated sample, be vortexed 1 ~ 5min of concussion, upper strata organic solvent is taken after centrifugation, organic solvent twice is merged into simultaneously mixing, obtains extract liquor, adsorbent is added in into extract liquor, after 2 ~ 4min of vortex oscillation, supernatant is transferred in revolving bottle after centrifugation, 40 ~ 50 DEG C of water-bath rotary evaporations are done near, 1 ~ 2 parts by weight n-hexane is rejoined, is re-dissolved.The present invention has the advantages of separative efficiency is high, at low cost.
Description
Technical field
The present invention relates to pollutant monitoring field, in particular to a kind of point of persistence organic pollutant in aquatic products
From method.
Background technology
Persistence organic pollutant is mankind's synthesis, is difficult to degrade in the environment, is fat-soluble high and can be in food chain
A kind of compound of middle enrichment amplification.These substances have half volatile, can in the world be carried out by different approaches
Transport And Transformation, it will usually bring larger harm to environment and human health.Since 20th century, POPs to the harm of environment and its
The problems such as cutting down control also gradually becomes people and pays close attention to after conventional atmosphere and water pollution is administered and heavy metal pollution controls
Hot spot.The production history of typical POPs such as organo-chlorine pesticides, Polychlorinated biphenyls and polycyclic aromatic hydrocarbon etc. is long, and use scope is wide,
Retention time is long in environment.The half-life period of PCBs in Soil was in 10 ~ 20 years, and the Polychlorinated biphenyls that molecular weight is bigger, held
Long property is stronger, and half-life period of the PCB 153 in sea eel and human body is all at 10 years or more.Therefore, though the POPs disabled still
It can so detect in the environment, and persistence be caused to destroy environment.
And POPs has stronger toxicity (carcinogenicity, teratogenesis and mutagenicity) more, mass production and discharge are also right
Ecological environment and health produce threat.The toxicity of POPs can be to the reproduction of organism, immune, nerve and internal system
Etc. distortion and canceration for interfering and destroying and cause organism etc..POPs can cause bad shadow to the fecundity of organism
Ring, upset biological hormone in vivo, enzyme, growth factor normal function, damage hereditary material DNA and cause nerve problems
Deng.And POPs longer-term persistences in vivo, neonatal constitutional index and intellectual development etc. can be influenced.In addition many researchs
Be found that POPs has residual in some animal ovum and human breast milk, may make new born animal and fetus, newborn etc. be in compared with
High POPs load, and influence its production, growth and development.
The source of POPs is numerous in human body, and the intake by polluted water product is one of main source, therefore right
The monitoring of POPs in aquatic products body, it is all particularly significant to ecological environment and health.
The research of any pollutant be unable to do without accurate detection method, to the research of POPs always along with correlation before
The optimization of reason technology and instrument analytical method.The extraction of POPs is mainly extracted using Soxhlet extraction, liquid-liquid extraction, solid phase at present
It takes, modes, the purification style such as ultrasonic wave/microwave auxiliary extraction, accelerated solvent extraction mainly have gel permeation chromatography（GPC）Only
Change, solid phase chromatography column purification, sulfuric acid sulfonation etc..These methods need to expend a large amount of organic solvent more and the plenty of time carries out sample
The pre-treatment work (such as soxhlet type and GPC purifications) of product needs higher instrument and equipment (such as accelerated solvent extraction
Deng).In addition, a variety of POPs considerably increase pre-treatment and Instrumental Analysis mainly using the method for individually handling and analyzing at present
Time.
Therefore in order to meet the persistent organism in detection aquatic products, a kind of efficient, at low cost water is needed at present
The separation method of persistence organic pollutant in product.
Invention content
A kind of separation method of persistence organic pollutant in aquatic products is provided to solve the above-mentioned problems, and the present invention uses
Following technical scheme:
The separation method of persistence organic pollutant, includes the following steps in a kind of aquatic products：
（1）The concentrated sulfuric acid is cleared up：The aquatic products muscle samples after the homogenate of 10 ~ 15 parts by weight are weighed to add in centrifuge tube, addition 15 ~
The concentrated sulfuric acid of 17 parts by weight, slight oscillatory simultaneously react 30 ~ 40 min；
（2）Vortex solvent extraction：The extractant of 15 ~ 17 parts by weight is added in sample after being cleared up by the concentrated sulfuric acid, vortex shakes
After swinging 1 ~ 5min, supernatant upper strata organic solvent is transferred to another centrifuge tube after centrifugation；Again to by treated sample
The extractant of 15 ~ 17 parts by weight is added in product, be vortexed 1 ~ 5min of concussion, and upper strata organic solvent is taken after centrifugation, organic by twice
Solvent merges and mixing, obtains extract liquor；
（3）Dispersive solid phase extraction：Adsorbent is added in into extract liquor, after 2 ~ 4min of vortex oscillation, by supernatant after centrifugation
It is transferred in revolving bottle, 40 ~ 50 DEG C of water-bath rotary evaporations are done near, are rejoined 1 ~ 2 parts by weight n-hexane, are re-dissolved.
The present invention effectively shortens the time needed for resolution using concentrated sulfuric acid resolution sample, simultaneously because in aquatic products
POPs such as organo-chlorine pesticides, Polychlorinated biphenyls and polycyclic aromatic hydrocarbon etc. are in the digestion process of the present invention not by concentrated sulfuric acid dehydration
It influences, therefore separating effect of the present invention will not be had an impact using the concentrated sulfuric acid, and present invention employs be vortexed to extract aquatic products
POPs in product, then impurity is removed by way of Dispersive solid phase extraction, it does not need to, into processes such as luggage columns, shorten place
Manage the time, reduce human cost, have take it is shorter, effect of extracting is good, it is easy to operate the advantages of.
Preferably, the extractant is n-hexane and dichloromethane mixed solvent, the volume ratio of mixing is 1：1~
1：1.5.
Present invention employs n-hexane and dichloromethane mixed solvent as extractant, while the difference in aquatic products is held
Long property organic pollution has good effect of extracting, improves the efficiency of extraction, also improves for persistent organism
Separation rate.
Preferably, the adsorbent includes the component of following parts by weight：2 ~ 3 parts of silica gel and polysulfonamides 0.2 ~ 0.3
Part.
By the present invention in that the scheme being used cooperatively with silica gel and polysulfonamides, can improve for impurity in extractant
Adsorption efficiency improves the purity of separation, is conducive to the accurate of testing result.
Preferably, in the centrifugally operated, centrifugal rotational speed is 5000 ~ 6000 r/min, centrifugation time for 5 ~
10min。
The present invention can improve the efficiency of separation using the centrifugation time, contribute to the solid and liquid in quick separating system
Body reduces the time cost of separation.
Preferably, the silica gel is prepared by following steps：
A, gel is generated：The aqueous sulfuric acid for being 10 ~ 25% with weight concentration by the waterglass that mass fraction is 10 ~ 25%
It is mixed, the pH of mixed liquor is made to be 8 ~ 10 by the ratio for adjusting two kinds of materials, then instill the mixed liquor
Hydrogel is made in drips ball forming in forming oil column device；
B, process is impregnated：Hydrogel after molding is impregnated with dilute sulfuric acid；
C, washing step：Hydrogel after immersion is sent into washing pool and is washed；
D, work process is dried：Hydrogel after washing is being dried；
E, pulverizing process：Crushing obtains final products.
The present invention is micronised state by using silica gel prepared by above-mentioned steps, has better adsorption capacity, contributes to
Improve separative efficiency.
Preferably, soaking time is 14 ~ 18 hours in the step b impregnates process, the temperature of liquid during immersion
65℃ ~95℃。
The present invention contributes to the formation of the upper micropore of hydrogel using the temperature and soaking time, so as to increase silica gel
The specific surface area of grain helps to improve the adsorption capacity for the silica gel powder prepared, and helps to improve the function and effect of the present invention.
Preferably, the temperature washed in the step c washing steps be 40 DEG C ~ 100 DEG C, washing step continue to
Hydrogel pH value is more than 6.
Help to remove acid and sulfuric acid sodium impurity that may be present in hydrogel using 40 ~ 100 DEG C of washing temperature,
And can ensure that flow rinses the surface of hydrogel and hydrogel is maintained at relatively stable position using washing pool, it avoids
Hydrogel is mutually collided in water-washing process and is ruptured, and so as to influence the specific surface area for preparing silica gel, is unfavorable for adding
The separative efficiency of strong silica gel.
Preferably, the baking operation includes drying for the first time and second dries the first time drying temperature
It it is 80 ~ 120 DEG C, drying time is 15 ~ 20min, and second of drying, described second baking are carried out after removing damaged hydrogel
Dry temperature is 140 DEG C ~ 700 DEG C, and the drying time is 30 ~ 50min.
Present invention employs the operations dried twice, dry for the first time, reducing the water content in hydrogel helps to remove
Damaged hydrogel is removed, prevents from destroying other hydrogels during carrying out removing damaged hydrogel, helps to ensure that silicon
The adsorption capacity of glue improves the function and effect of the present invention.
Preferably, superfine communication technique is used in the step e pulverizing process.
The present invention can further improve the adsorption capacity of silica gel using superfine communication technique, improve separative efficiency.
The present invention has separating effect strong, and separative efficiency is high, advantage at low cost.
Specific embodiment
The present invention is further explained with reference to specific implementation case：
Embodiment 1
The separation method of persistence organic pollutant, includes the following steps in a kind of aquatic products：
（1）The concentrated sulfuric acid is cleared up：It weighs the aquatic products muscle samples after the homogenate of 10 parts by weight to add in centrifuge tube, adds in 15 ~ 17 weights
The concentrated sulfuric acid of part is measured, slight oscillatory simultaneously reacts 30 min；
（2）Vortex solvent extraction：The extractant of 15 ~ 17 parts by weight is added in sample after being cleared up by the concentrated sulfuric acid, vortex shakes
After swinging 1min, supernatant upper strata organic solvent is transferred to another centrifuge tube after centrifugation；Again to by treated sample
The middle extractant for adding in 15 ~ 17 parts by weight, be vortexed concussion 1min, upper strata organic solvent is taken after centrifugation, by organic solvent twice
Merge simultaneously mixing, obtain extract liquor；
（3）Dispersive solid phase extraction：It adds in adsorbent into extract liquor, after 2 min of vortex oscillation, turns supernatant after centrifugation
It moves in revolving bottle, 40 DEG C of water-bath rotary evaporations are done near, are rejoined 1 parts by weight n-hexane, are re-dissolved.
Wherein, the extractant is n-hexane and dichloromethane mixed solvent, and the volume ratio of mixing is 1：1.
Wherein, the adsorbent includes the component of following parts by weight：0.2 part of 2 parts of silica gel and polysulfonamides.
Wherein, in the centrifugally operated, centrifugal rotational speed is 5000 r/min, centrifugation time 5min.
Wherein, the silica gel is prepared by following steps：
A, gel is generated：The waterglass that mass fraction is 10% is mixed with aqueous sulfuric acid that weight concentration is 10 %
It closes, the pH of mixed liquor is made to be 8 by the ratio for adjusting two kinds of materials, the mixed liquor is then instilled into forming oil column dress
It puts middle drips ball forming and hydrogel is made
B, process is impregnated：Hydrogel after molding is impregnated with dilute sulfuric acid；
C, washing step：Hydrogel after immersion is sent into washing pool and is washed；
D, work process is dried：Hydrogel after washing is being dried；
E, pulverizing process：Crushing obtains final products.
Wherein, soaking time is 14 hours in the step b impregnates process, 65 DEG C of the temperature of liquid during immersion.
Wherein, the temperature washed in the step c washing steps is 100 DEG C, and washing step continues to hydrogel pH
Be worth is 6.
Wherein, it is 80 that the baking operation, which includes drying for the first time and dries the first time drying temperature for second,
DEG C, drying time 15min carries out second of drying after removing damaged hydrogel, and second of drying temperature is 140
DEG C, the drying time is 30min.
Wherein, superfine communication technique is used in the step e pulverizing process.
Embodiment 2
The separation method of persistence organic pollutant, includes the following steps in a kind of aquatic products：
（1）The concentrated sulfuric acid is cleared up：It weighs the aquatic products muscle samples after the homogenate of 15 parts by weight to add in centrifuge tube, adds in 15 ~ 17
The concentrated sulfuric acid of parts by weight, slight oscillatory simultaneously react 40 min；
（2）Vortex solvent extraction：The extractant of 17 parts by weight, vortex oscillation are added in sample after being cleared up by the concentrated sulfuric acid
After 5min, supernatant upper strata organic solvent is transferred to another centrifuge tube after centrifugation；Again to by treated sample
The extractant of 17 parts by weight is added in, be vortexed concussion 5min, and upper strata organic solvent is taken after centrifugation, organic solvent twice is merged
And mixing, obtain extract liquor；
（3）Dispersive solid phase extraction：It adds in adsorbent into extract liquor, after vortex oscillation 4min, turns supernatant after centrifugation
It moves in revolving bottle, 40 DEG C of water-bath rotary evaporations are done near, are rejoined 2 parts by weight n-hexanes, are re-dissolved.
Wherein, the extractant is n-hexane and dichloromethane mixed solvent, and the volume ratio of mixing is 1：1.
Wherein, the adsorbent includes the component of following parts by weight：0.2 part of 2 parts of silica gel and polysulfonamides.
Wherein, in the centrifugally operated, centrifugal rotational speed is 5000 r/min, centrifugation time 5min.
Wherein, the silica gel is prepared by following steps：
A, gel is generated：The waterglass that mass fraction is 10% is mixed with aqueous sulfuric acid that weight concentration is 10 %
It closes, the pH of mixed liquor is made to be 8 by the ratio for adjusting two kinds of materials, the mixed liquor is then instilled into forming oil column dress
It puts middle drips ball forming and hydrogel is made
B, process is impregnated：Hydrogel after molding is impregnated with dilute sulfuric acid；
C, washing step：Hydrogel after immersion is sent into washing pool and is washed；
D, work process is dried：Hydrogel after washing is being dried；
E, pulverizing process：Crushing obtains final products.
Wherein, soaking time is 14 hours in the step b impregnates process, 65 DEG C of the temperature of liquid during immersion.
Wherein, the temperature washed in the step c washing steps is 100 DEG C, and washing step continues to hydrogel pH
Be worth is 6.
Wherein, it is 80 that the baking operation, which includes drying for the first time and dries the first time drying temperature for second,
DEG C, drying time 15min carries out second of drying after removing damaged hydrogel, and second of drying temperature is 140
DEG C, the drying time is 30min.
Wherein, superfine communication technique is used in the step e pulverizing process.
Embodiment 3
The separation method of persistence organic pollutant, includes the following steps in a kind of aquatic products：
（1）The concentrated sulfuric acid is cleared up：It weighs the aquatic products muscle samples after the homogenate of 15 parts by weight to add in centrifuge tube, adds in 17 weight
The concentrated sulfuric acid of part, slight oscillatory simultaneously react 30 min；
（2）Vortex solvent extraction：The extractant of 17 parts by weight, vortex oscillation are added in sample after being cleared up by the concentrated sulfuric acid
After 3min, supernatant upper strata organic solvent is transferred to another centrifuge tube after centrifugation；Again to by treated sample
The extractant of 15 parts by weight is added in, be vortexed 1 ~ 5min of concussion, and upper strata organic solvent is taken after centrifugation, organic solvent twice is closed
And simultaneously mixing, obtain extract liquor；
（3）Dispersive solid phase extraction：It adds in adsorbent into extract liquor, after vortex oscillation 4min, turns supernatant after centrifugation
It moves in revolving bottle, 40 DEG C of water-bath rotary evaporations are done near, are rejoined 2 parts by weight n-hexanes, are re-dissolved.
Wherein, the extractant is n-hexane and dichloromethane mixed solvent, and the volume ratio of mixing is 1：1.
Wherein, the adsorbent includes the component of following parts by weight：0.2 part of 2 parts of silica gel and polysulfonamides.
Wherein, in the centrifugally operated, centrifugal rotational speed is 5000 r/min, centrifugation time 5min.
Wherein, the silica gel is prepared by following steps：
A, gel is generated：The waterglass that mass fraction is 10% is mixed with aqueous sulfuric acid that weight concentration is 10 %
It closes, the pH of mixed liquor is made to be 8 by the ratio for adjusting two kinds of materials, the mixed liquor is then instilled into forming oil column dress
It puts middle drips ball forming and hydrogel is made
B, process is impregnated：Hydrogel after molding is impregnated with dilute sulfuric acid；
C, washing step：Hydrogel after immersion is sent into washing pool and is washed；
D, work process is dried：Hydrogel after washing is being dried；
E, pulverizing process：Crushing obtains final products.
Wherein, soaking time is 14 hours in the step b impregnates process, 65 DEG C of the temperature of liquid during immersion.
Wherein, the temperature washed in the step c washing steps is 100 DEG C, and washing step continues to hydrogel pH
Be worth is 6.
Wherein, it is 80 that the baking operation, which includes drying for the first time and dries the first time drying temperature for second,
DEG C, drying time 15min carries out second of drying after removing damaged hydrogel, and second of drying temperature is 140
DEG C, the drying time is 30min.
Wherein, superfine communication technique is used in the step e pulverizing process.
Embodiment 4
The separation method of persistence organic pollutant, includes the following steps in a kind of aquatic products：
（1）The concentrated sulfuric acid is cleared up：It weighs the aquatic products muscle samples after the homogenate of 10 parts by weight to add in centrifuge tube, adds in 15 ~ 17
The concentrated sulfuric acid of parts by weight, slight oscillatory simultaneously react 35 min；
（2）Vortex solvent extraction：The extractant of 15 ~ 17 parts by weight is added in sample after being cleared up by the concentrated sulfuric acid, vortex shakes
After swinging 3min, supernatant upper strata organic solvent is transferred to another centrifuge tube after centrifugation；Again to by treated sample
The middle extractant for adding in 16 parts by weight, be vortexed concussion 3min, and upper strata organic solvent is taken after centrifugation, organic solvent twice is merged
And mixing, obtain extract liquor；
（3）Dispersive solid phase extraction：It adds in adsorbent into extract liquor, after vortex oscillation 3min, turns supernatant after centrifugation
It moves in revolving bottle, 40 DEG C of water-bath rotary evaporations are done near, are rejoined 1 parts by weight n-hexane, are re-dissolved.
Wherein, the extractant is n-hexane and dichloromethane mixed solvent, and the volume ratio of mixing is 1：1.
Wherein, the adsorbent includes the component of following parts by weight：0.2 part of 2 parts of silica gel and polysulfonamides.
Wherein, in the centrifugally operated, centrifugal rotational speed is 5000 r/min, centrifugation time 5min.
Wherein, the silica gel is prepared by following steps：
A, gel is generated：The waterglass that mass fraction is 10% is mixed with aqueous sulfuric acid that weight concentration is 10 %
It closes, the pH of mixed liquor is made to be 8 by the ratio for adjusting two kinds of materials, the mixed liquor is then instilled into forming oil column dress
It puts middle drips ball forming and hydrogel is made
B, process is impregnated：Hydrogel after molding is impregnated with dilute sulfuric acid；
C, washing step：Hydrogel after immersion is sent into washing pool and is washed；
D, work process is dried：Hydrogel after washing is being dried；
E, pulverizing process：Crushing obtains final products.
Wherein, soaking time is 14 hours in the step b impregnates process, 65 DEG C of the temperature of liquid during immersion.
Wherein, the temperature washed in the step c washing steps is 100 DEG C, and washing step continues to hydrogel pH
Be worth is 6.
Wherein, it is 80 that the baking operation, which includes drying for the first time and dries the first time drying temperature for second,
DEG C, drying time 15min carries out second of drying after removing damaged hydrogel, and second of drying temperature is 140
DEG C, the drying time is 30min.
Wherein, superfine communication technique is used in the step e pulverizing process.
Embodiment 5
The separation method of persistence organic pollutant, includes the following steps in a kind of aquatic products：
（1）The concentrated sulfuric acid is cleared up：It weighs the aquatic products muscle samples after the homogenate of 12 parts by weight to add in centrifuge tube, adds in 15 ~ 17
The concentrated sulfuric acid of parts by weight, slight oscillatory simultaneously react 36min；
（2）Vortex solvent extraction：The extractant of 16 parts by weight, vortex oscillation are added in sample after being cleared up by the concentrated sulfuric acid
After 5min, supernatant upper strata organic solvent is transferred to another centrifuge tube after centrifugation；Again to by treated sample
The extractant of 17 parts by weight is added in, be vortexed concussion 4min, and upper strata organic solvent is taken after centrifugation, organic solvent twice is merged
And mixing, obtain extract liquor；
（3）Dispersive solid phase extraction：It adds in adsorbent into extract liquor, after vortex oscillation 3min, turns supernatant after centrifugation
It moves in revolving bottle, 40 DEG C of water-bath rotary evaporations are done near, are rejoined 1 parts by weight n-hexane, are re-dissolved.
Wherein, the extractant is n-hexane and dichloromethane mixed solvent, and the volume ratio of mixing is 1：1.
Wherein, the adsorbent includes the component of following parts by weight：0.2 part of 2 parts of silica gel and polysulfonamides.
Wherein, in the centrifugally operated, centrifugal rotational speed is 5000 r/min, centrifugation time 5min.
Wherein, the silica gel is prepared by following steps：
A, gel is generated：The waterglass that mass fraction is 10% is mixed with aqueous sulfuric acid that weight concentration is 10 %
It closes, the pH of mixed liquor is made to be 8 by the ratio for adjusting two kinds of materials, the mixed liquor is then instilled into forming oil column dress
It puts middle drips ball forming and hydrogel is made
B, process is impregnated：Hydrogel after molding is impregnated with dilute sulfuric acid；
C, washing step：Hydrogel after immersion is sent into washing pool and is washed；
D, work process is dried：Hydrogel after washing is being dried；
E, pulverizing process：Crushing obtains final products.
Wherein, soaking time is 14 hours in the step b impregnates process, 65 DEG C of the temperature of liquid during immersion.
Wherein, the temperature washed in the step c washing steps is 100 DEG C, and washing step continues to hydrogel pH
Be worth is 6.
Wherein, it is 80 that the baking operation, which includes drying for the first time and dries the first time drying temperature for second,
DEG C, drying time 15min carries out second of drying after removing damaged hydrogel, and second of drying temperature is 140
DEG C, the drying time is 30min.
Wherein, superfine communication technique is used in the step e pulverizing process.
The present invention effectively shortens the time needed for resolution using concentrated sulfuric acid resolution sample, then extracts aquatic products by vortex
POPs in product, then impurity is removed by way of Dispersive solid phase extraction, it does not need to, into processes such as luggage columns, shorten place
Manage the time, reduce human cost, have take it is shorter, effect of extracting is good, it is easy to operate the advantages of.
Claims (9)
1. the separation method of persistence organic pollutant in a kind of aquatic products, which is characterized in that include the following steps：
（1）The concentrated sulfuric acid is cleared up：The aquatic products muscle samples after the homogenate of 10 ~ 15 parts by weight are weighed to add in centrifuge tube, addition 15 ~
The concentrated sulfuric acid of 17 parts by weight, slight oscillatory simultaneously react 30 ~ 40 min；
（2）Vortex solvent extraction：The extractant of 15 ~ 17 parts by weight is added in sample after being cleared up by the concentrated sulfuric acid, vortex shakes
After swinging 1 ~ 5min, supernatant upper strata organic solvent is transferred to another centrifuge tube after centrifugation；Again to by treated sample
The extractant of 15 ~ 17 parts by weight is added in product, be vortexed 1 ~ 5min of concussion, and upper strata organic solvent is taken after centrifugation, organic by twice
Solvent merges and mixing, obtains extract liquor；
（3）Dispersive solid phase extraction：Adsorbent is added in into extract liquor, after 2 ~ 4min of vortex oscillation, by supernatant after centrifugation
It is transferred in revolving bottle, 40 ~ 50 DEG C of water-bath rotary evaporations are done near, are rejoined 1 ~ 2 parts by weight n-hexane, are re-dissolved.
2. the separation method of persistence organic pollutant in a kind of aquatic products according to claim 1, it is characterised in that：Institute
The extractant stated is n-hexane and dichloromethane mixed solvent, and the volume ratio of mixing is 1：1~1：1.5.
3. the separation method of persistence organic pollutant in a kind of aquatic products according to claim 1, it is characterised in that：Institute
The adsorbent stated includes the component of following parts by weight：0.2 ~ 0.3 part of 2 ~ 3 parts of silica gel and polysulfonamides.
4. the separation method of persistence organic pollutant in a kind of aquatic products according to claim 1, it is characterised in that：Institute
In the centrifugally operated stated, centrifugal rotational speed is 5000 ~ 6000 r/min, and centrifugation time is 5 ~ 10min.
5. the separation method of persistence organic pollutant in a kind of aquatic products according to claim 1, which is characterized in that institute
The silica gel stated is prepared by following steps：
A, gel is generated：The aqueous sulfuric acid for being 10 ~ 25% with weight concentration by the waterglass that mass fraction is 10 ~ 25%
It is mixed, the pH of mixed liquor is made to be 8 ~ 10 by the ratio for adjusting two kinds of materials, then instill the mixed liquor
Hydrogel is made in drips ball forming in forming oil column device；
B, process is impregnated：Hydrogel after molding is impregnated with dilute sulfuric acid；
C, washing step：Hydrogel after immersion is sent into washing pool and is washed；
D, work process is dried：Hydrogel after washing is being dried；
E, pulverizing process：Crushing obtains final products.
6. the separation method of persistence organic pollutant in a kind of aquatic products according to claim 5, it is characterised in that：
It is 14 ~ 18 hours that the step b, which impregnates soaking time in process, 65 DEG C ~ 95 DEG C of the temperature of liquid during immersion.
7. the separation method of persistence organic pollutant in a kind of aquatic products according to claim 5, it is characterised in that：Institute
The temperature washed in the step c washing steps stated is 40 DEG C ~ 100 DEG C, and washing step continues to hydrogel pH value more than 6.
8. the separation method of persistence organic pollutant in a kind of aquatic products according to claim 5, it is characterised in that：Institute
It is 80 ~ 120 DEG C that the baking operation stated, which includes drying for the first time and dries the first time drying temperature for second, drying time
For 15 ~ 20min, second of drying is carried out after removing damaged hydrogel, second of drying temperature is 140 DEG C ~ 700
DEG C, the drying time is 30 ~ 50min.
9. the separation method of persistence organic pollutant in a kind of aquatic products according to claim 5, it is characterised in that：Institute
Superfine communication technique is used in the step e pulverizing process stated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711369931.9A CN108196020A (en) | 2017-12-19 | 2017-12-19 | The separation method of persistence organic pollutant in a kind of aquatic products |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711369931.9A CN108196020A (en) | 2017-12-19 | 2017-12-19 | The separation method of persistence organic pollutant in a kind of aquatic products |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108196020A true CN108196020A (en) | 2018-06-22 |
Family
ID=62574611
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711369931.9A Pending CN108196020A (en) | 2017-12-19 | 2017-12-19 | The separation method of persistence organic pollutant in a kind of aquatic products |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108196020A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111504740A (en) * | 2020-04-22 | 2020-08-07 | 中国科学院生态环境研究中心 | Sample solidification pretreatment method for analyzing heavy metals in waste water and waste liquid by rapid detection technology |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101224409A (en) * | 2007-10-18 | 2008-07-23 | 烟台博瑞特精细化工有限公司 | Production method of superfine silica powder with high adsorption value |
| CN101813677A (en) * | 2010-04-29 | 2010-08-25 | 同济大学 | Method for analyzing and determining organics persistently containing chlorine in aquatic product |
| CN105044249A (en) * | 2015-06-25 | 2015-11-11 | 中华人民共和国福清出入境检验检疫局 | Rapid-detection pretreatment kit for 28 polychlorinated biphenyls in aquatic product and application of kit |
-
2017
- 2017-12-19 CN CN201711369931.9A patent/CN108196020A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101224409A (en) * | 2007-10-18 | 2008-07-23 | 烟台博瑞特精细化工有限公司 | Production method of superfine silica powder with high adsorption value |
| CN101813677A (en) * | 2010-04-29 | 2010-08-25 | 同济大学 | Method for analyzing and determining organics persistently containing chlorine in aquatic product |
| CN105044249A (en) * | 2015-06-25 | 2015-11-11 | 中华人民共和国福清出入境检验检疫局 | Rapid-detection pretreatment kit for 28 polychlorinated biphenyls in aquatic product and application of kit |
Non-Patent Citations (6)
| Title |
|---|
| 丁立平等: "双重净化/气相色谱法测定水产品中指示性多氯联苯", 《分析测试学报》 * |
| 吴益春等: "酸消化-气相色谱法测定鱼肉中指示性多氯联苯研究", 《食品安全质量检测学报》 * |
| 孙秀梅等: "气相色谱法测定贻贝中的多氯联苯和有机氯农药", 《广州化工》 * |
| 朱洪法: "《催化剂载体》", 30 April 1980, 化学工业出版社 * |
| 胡礼渊等: "分散固相萃取-气相色谱法测定水产品中多氯联苯", 《食品科学》 * |
| 许仁杰等: "气相色谱法测定水产品有机氯农药和多氯联苯", 《食品工业》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111504740A (en) * | 2020-04-22 | 2020-08-07 | 中国科学院生态环境研究中心 | Sample solidification pretreatment method for analyzing heavy metals in waste water and waste liquid by rapid detection technology |
| CN111504740B (en) * | 2020-04-22 | 2021-02-19 | 中国科学院生态环境研究中心 | Sample solidification pretreatment method for analyzing heavy metals in waste water and waste liquid |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| X Liu et al. | Extraction and characterization of proanthocyanidins from grape seeds | |
| CN109632427B (en) | Pretreatment method for rapid detection of nitrofuran metabolites and detection method thereof | |
| WO2000064883A1 (en) | Methods for purifying proanthocyanidin oligomers | |
| CN108195982A (en) | The detection method of persistence organic pollutant in a kind of aquatic products | |
| CN1555728A (en) | Method of combined preparing garlic essential oil and garlic polysaccharide | |
| Liu et al. | A novel approach for the simultaneous extraction of dihydroquercetin and arabinogalactan from Larix gmelinii by homogenate-ultrasound-synergistic technique using the ionic liquid | |
| CN108196020A (en) | The separation method of persistence organic pollutant in a kind of aquatic products | |
| RU2435766C1 (en) | Method of producing dihydroquercetin | |
| CN103920470B (en) | A kind of magnetic humic acid and its preparation method and application | |
| CN108459112B (en) | Method for detecting content of organochlorine pesticide in crab cream of Eriocheir sinensis | |
| CN104256640B (en) | Method for extracting natural antioxidant substances from naseberry leaves | |
| CN108675917A (en) | The chelated calcium isolation and purification method of sugar alcohol in a kind of organic fertilizer | |
| CN107121507A (en) | A kind of bamboo shoot shell polyphenol substance assay method | |
| CN107033017B (en) | A kind of method of quick preparation high-purity hydroxyl-γ-sanshool | |
| CN105254692A (en) | Method for extracting aucubin and geniposide from eucommia ulmoides peel at same time | |
| CN108732260A (en) | The extraction and purification methods of aflatoxin B1 in one vegetable oil | |
| CN106187975B (en) | A kind of preparation for improving rice bran aldehydes matter bioactivity and purification process | |
| CN104622757B (en) | A kind of extracting method of Apple cell extract and its application | |
| CN105037311B (en) | A kind of compound liquid phase method for extraction and purification of the online two dimension of apiolin | |
| CN107468746A (en) | A kind of method that middle extraction polyphenol and flavones are spent from Zhu Ying | |
| CN107474150A (en) | A kind of ultrasonic extracting method of Zhegucai polysaccharide and application | |
| CN1334267A (en) | Process for preparing total sanchinoside | |
| CN109142571B (en) | Method for measuring content of anthraquinone components | |
| CN101607981A (en) | The method of steroid saponin in the integrated column chromatography isolation and purification yellow ginger | |
| CN101148658A (en) | Double aqueous phase method for extracting superoxide dismutase from animal blood |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180622 |
|
| RJ01 | Rejection of invention patent application after publication |