CN105758963B - It is a kind of to be used for the magnetic control dispersion solid-phase extraction method of aniline and benzidine residues detecton in textile - Google Patents
It is a kind of to be used for the magnetic control dispersion solid-phase extraction method of aniline and benzidine residues detecton in textile Download PDFInfo
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- CN105758963B CN105758963B CN201610127227.1A CN201610127227A CN105758963B CN 105758963 B CN105758963 B CN 105758963B CN 201610127227 A CN201610127227 A CN 201610127227A CN 105758963 B CN105758963 B CN 105758963B
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- amido
- acetic acid
- molecular engram
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- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 title claims abstract description 78
- HFACYLZERDEVSX-UHFFFAOYSA-N benzidine Chemical group C1=CC(N)=CC=C1C1=CC=C(N)C=C1 HFACYLZERDEVSX-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 239000004753 textile Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000006185 dispersion Substances 0.000 title claims abstract description 13
- 238000002414 normal-phase solid-phase extraction Methods 0.000 title claims abstract description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 96
- 239000002245 particle Substances 0.000 claims abstract description 52
- 125000003368 amide group Chemical group 0.000 claims abstract description 45
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 239000004743 Polypropylene Substances 0.000 claims abstract description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 11
- -1 polypropylene Polymers 0.000 claims abstract description 11
- 229920001155 polypropylene Polymers 0.000 claims abstract description 11
- 238000000746 purification Methods 0.000 claims abstract description 11
- 238000002137 ultrasound extraction Methods 0.000 claims abstract description 11
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000006228 supernatant Substances 0.000 claims description 26
- 239000003480 eluent Substances 0.000 claims description 12
- 239000004744 fabric Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000002604 ultrasonography Methods 0.000 claims description 9
- 150000001412 amines Chemical class 0.000 claims description 7
- 229920000742 Cotton Polymers 0.000 claims description 4
- 229920002873 Polyethylenimine Polymers 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 210000002268 wool Anatomy 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 2
- 239000000178 monomer Substances 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 150000002825 nitriles Chemical class 0.000 claims 1
- 229920002994 synthetic fiber Polymers 0.000 claims 1
- 238000000605 extraction Methods 0.000 abstract description 6
- 238000000926 separation method Methods 0.000 abstract description 6
- 238000004458 analytical method Methods 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract description 2
- 238000011017 operating method Methods 0.000 abstract description 2
- 230000005526 G1 to G0 transition Effects 0.000 abstract 1
- 230000033228 biological regulation Effects 0.000 abstract 1
- 238000002955 isolation Methods 0.000 abstract 1
- 230000014759 maintenance of location Effects 0.000 abstract 1
- 230000035945 sensitivity Effects 0.000 abstract 1
- 239000007787 solid Substances 0.000 abstract 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 12
- 238000011084 recovery Methods 0.000 description 11
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 8
- 238000010828 elution Methods 0.000 description 7
- 239000004305 biphenyl Substances 0.000 description 6
- 235000010290 biphenyl Nutrition 0.000 description 6
- 239000000523 sample Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 229920002972 Acrylic fiber Polymers 0.000 description 3
- 239000000987 azo dye Substances 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 1
- 239000005695 Ammonium acetate Substances 0.000 description 1
- 206010010219 Compulsions Diseases 0.000 description 1
- 206010011793 Cystitis haemorrhagic Diseases 0.000 description 1
- 201000004624 Dermatitis Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 235000019257 ammonium acetate Nutrition 0.000 description 1
- 229940043376 ammonium acetate Drugs 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 231100000693 bioaccumulation Toxicity 0.000 description 1
- 201000001531 bladder carcinoma Diseases 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 201000002802 hemorrhagic cystitis Diseases 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 208000019423 liver disease Diseases 0.000 description 1
- 208000005135 methemoglobinemia Diseases 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 208000010570 urinary bladder carcinoma Diseases 0.000 description 1
Classifications
-
- 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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
Abstract
It is used for the magnetic control dispersion solid-phase extraction method of aniline and benzidine residues detecton in textile the invention discloses a kind of.It is characterized in that：Take representative homogeneous sample, it is some to be cut into blockage, 0.40~0.6g is weighed after fully mixing in 10mL polypropylene centrifuge tubes using after 0.01~0.05 (v/v) % acetic acid solutions/ethanol solution ultrasonic extraction, add appropriate ammoniacal liquor regulation pH to 8.5~9.5, again using the more amido sub-micron molecular engram particle enrichment purifications of appropriate Magnetic Spherical, separation of solid and liquid is carried out using magnetic control isolation technics, then after being eluted using 0.4~0.6mL methanol, detected using stationary phases for HPLC.The present invention carries out being enriched with purification and separation using the extraction of acetic acid solution alcohol mixeding liquid, using the more amido sub-micron molecular engram particles of Magnetic Spherical to extract solution, eliminate the operating procedure of cumbersome Liquid liquid Separation, matrix interference is few, it is simple to operate, cheap, speed is fast, with good detection sensitivity and precision, it is suitable for the sample pretreatment of aniline and benzidine retention analysis in textile.
Description
Technical field
It is used for the magnetic control dispersion solid-phase extraction method of aniline and benzidine residues detecton in textile the present invention relates to a kind of,
The more amido sub-micron molecular engram particle absorption enrichments of magnetic remained more particularly to aniline in textile and benzidine
And its magnetic control separation method.
Background technology
Aniline and benzidine are the important intermediates for synthesizing azo dyes, can be by sucking, eating or inhaled through skin
Receive and cause urgency/slow poisoning, wherein aniline can cause methemoglobinemia, toxic hepatic disease etc., and benzidine, which can cause, to be connect
Touch property dermatitis, hemorrhagic cystitis and carcinoma of urinary bladder.It is state compulsion that the forbidding azo dyes such as aniline and biphenyl are remained in textile
Standard GB 18401-2010《National general safety technical code for textile products》Defined ecological safety index, it is that textile is normal
Advise detection project.At present, the extraction of aniline and benzidine mainly uses ether as extractant in textile, but ether is easy
Peroxide is generated with the oxygen reaction in air, and peroxide easily makes aniline and benzidine that oxidation reaction occur so as to change
The property of aniline and benzidine and cause extraction efficiency to decline.It is cumbersome and time-consuming to there is pre-treatment step using extracted by ether simultaneously
The problems such as long.Therefore a kind of simple, practical, quick extracting method is developed, for aniline in control textile and benzidine
Pollution, ensure human-body safety and health of human body, have great importance.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of bioaccumulation efficiency height, technique is simple and convenient to operate efficiently
Magnetic dispersion solid-phase extraction method for aniline in textile and benzidine residues detecton.
Technical scheme is used by the present invention solves above-mentioned technical problem：One kind is used for aniline and benzidine in textile
The magnetic dispersion solid-phase extraction method of residues detecton, it is characterised in that comprise the following steps：
1) extract：Representative homogeneous sample is taken, it is some to be cut into 0.4cm~0.6cm square, claims after fully mixing
0.40~0.60g is taken in 10mL polypropylene centrifuge tubes, adds 0.01%~0.05 (v/v) % acetic acid solutions-alcohol mixeding liquid 4
After~6mL, 4~6min of ultrasonic extraction, supernatant is poured out in another centrifuge tube, is at least repeated 1 time, merges supernatant
Liquid, pH to 8.5~9.5 is adjusted with ammoniacal liquor.
2) it is enriched with, purification separates with magnetic control：Then the more amido sub-micron molecular engrams of appropriate magnetic are added in centrifuge tube
Particle, ultrasound fully mix 1~3min, the more amido sub-micron molecular engram particle buildups of magnetic are made in the presence of externally-applied magnetic field
In centrifugation tube wall, solution is discarded, with the more amido sub-micron molecular engram particles of 1.5~2.5mL water wash magnetic, discards elution
Liquid, finally eluted with 0.4~0.6mL methanol, collect eluent, analyzed and detect for HPLC.
Preferably, the textile is one kind in cotton, acrylic fiber fabric or wool fabric.
Preferably, the acetic acid solution in the step 1) is 0.04% acetic acid solution, 0.01% acetic acid solution and 0.5%
One kind in acetic acid solution, the volume ratio of acetic acid solution and ethanol is 1-6 in acetic acid solution-alcohol mixeding liquid:1.
Further preferably, the acetic acid solution is 0.04% acetic acid solution, acetic acid solution in acetic acid solution-alcohol mixeding liquid
Volume ratio with ethanol is 5:1.
Preferably, the square that the sample is cut into 0.5cm is some, 0.50g is weighed in 10mL polypropylene after fully mixing
In centrifuge tube, add 0.04% acetic acid solution-alcohol mixeding liquid 5mL, after ultrasonic extraction 5min, pour out supernatant in it is another from
In heart pipe, repeat 1 time, merge supernatant, pH to 9 is adjusted with ammoniacal liquor.
As an improvement, the more amido sub-micron molecular engram particles of magnetic in the step 2) refer in polyethyleneimine
(PEI) coexisted down with TEPA (TEPA) amine-containing monomers and aniline and benzidine template molecule in coated silica
Magnetic ferroferric oxide surface it is aggregated reaction and obtain a kind of molecular imprinting composite material, for magnetic sub-micron molecule print
One kind in mark particle.The sub-micron molecular engram particle is spherical, and the particle diameter of particle is 150~300nm, and magnetic sub-micron is divided
The addition of sub- trace particle and the weight/volume score ratio of extract solution are 1-20mg/10mL.
Further preferably, the addition of the more amido sub-micron molecular engram particles of the magnetic and the weight/volume of extract solution point
Number ratio is 3.0mg/10mL.
Ultrasound fully mixes 2min after the step 2) adds the more amido sub-micron molecular engram particles of magnetic, in additional magnetic
The more amido sub-micron molecular engram particle buildups of magnetic is being centrifuged tube wall in the presence of, solution is discarded, with 2mL water wash magnetic
Property more amido sub-micron molecular engram particles, discard leacheate, finally with 0.5mL methanol elute.
Finally, the HPLC analyses are on a cl 8 column flowing with acetonitrile/50mmol/L ammonium acetate solutions (V/V=25/75)
Phase, fluoroscopic examination wavelength aniline λ ex/ λ em=232nm/329nm, benzidine λ ex/ λ em=292nm/383nm.
Compared with prior art, the advantage of the invention is that：Spun in the present invention using acetic acid solution-alcohol mixeding liquid extraction
The trace aniline and benzidine remained in fabric, it is low to overcome aniline and benzidine extraction recovery in existing extracting method
Problem, at the same also overcome in the prior art by the use of ether as aniline during extract solution and benzidine is oxidizable, service speed is slow and
The problem of being not easy to realize effective quick separating；The present invention uses the more amido sub-micron molecular engram particles pair of Magnetic Spherical simultaneously
Extract solution carries out being enriched with purification and separation, eliminates the operating procedure of cumbersome liquid-liquid separation, matrix effect is lower, to target
The selectivity of thing aniline and benzidine is stronger, also make it that operation is more convenient.
Brief description of the drawings
Fig. 1 be in the embodiment of the present invention 1 sample solution difference pH value to aniline and the influence curve figure of benzidine adsorption rate；
Fig. 2 is the more amido sub-micron molecular engram particle dosages of magnetic in embodiment 1 to aniline and benzidine adsorption efficiency
Influence curve figure；
Fig. 3 is eluant, eluent volume in embodiment 1 to aniline and the influence curve figure of the benzidine rate of recovery；
Embodiment
The present invention is described in further detail below in conjunction with accompanying drawing embodiment.
Embodiment 1：
1.1 take representative uniform cotton swatch, and it is some to be cut into 0.5cm × 0.5cm square, claim after fully mixing
0.50g is taken in 10mL polypropylene centrifuge tubes, adds 0.04% acetic acid/ethanol (5：1, V/V) solution 5mL, ultrasonic extraction 5min
Afterwards, supernatant is poured out in another centrifuge tube, is repeated 1 time, merges supernatant, adjusts pH to 9.0 with ammoniacal liquor respectively.
1.2 enrichments, purification separate with magnetic control, then accurately weigh the more amido sub-micron molecular engram particle 3.0mg of magnetic,
It is dispersed in supernatant, ultrasound fully mixes 2min, and the more amido sub-micron molecular engrams of magnetic are made in the presence of externally-applied magnetic field
Particle buildup is centrifuging tube wall, discards solution, with the more amido sub-micron molecular engram particles of 2mL water wash magnetic, discards elution
Liquid, finally eluted with 0.5mL methanol, collect eluent, analyzed and detect for HPLC.As a result aniline and biphenyl in textile are measured
The recovery of standard addition of amine is 90.6~98.7%.
The parameter of the present embodiment is changed to illustrate optimal processing parameter below：
Above-mentioned other conditions are constant, change pH to 1.0,2.0,3.0,4.0,5.0,6.0,7.0,8.0,9.0,10.0 and distinguish
Tested, as a result measure in different pH value that the adsorption rate of aniline and benzidine is as shown in Figure 1 in textile, it can be seen that when
When pH is 9.0, the recovery of standard addition highest of aniline and benzidine in textile,
Above-mentioned other conditions are constant, change the addition of the more amido sub-micron molecular engram particles of magnetic, weigh magnetic respectively
The more amido sub-micron molecular engram particle 1.0mg, 2.0mg of property, 3.0mg, 4.0mg, 5.0mg, 6.0mg, 7.0mg, 8.0mg,
9.0mg, 10.0mg, tested respectively, as a result measure and spun in the more amido sub-micron molecular engram particle dosages of different magnetic
The adsorption rate of aniline and benzidine is as shown in Figure 2 in fabric, it can be seen that when the more amido sub-micron molecular engram particles of magnetic
The recovery of standard addition highest of aniline and benzidine in textile, it is 90.6~98.7% during 3.0mg.
Above-mentioned other conditions are constant, change eluant, eluent methanol volume, respectively 0.1mL, 0.2mL, 0.3mL, 0.4mL,
0.5mL, 0.6mL, 0.7mL, 0.8mL, 0.9mL, 1.0mL, tested respectively, as a result measure and spun in different eluant, eluent volumes
The adsorption rate of aniline and benzidine is as shown in Figure 3 in fabric, it can be seen that when eluant, eluent is 0.5mL, in textile aniline and
The recovery of standard addition highest of benzidine.
Embodiment 2：
2.1 take representative uniform acrylic fiber fabric sample, and it is some to be cut into 0.5cm × 0.5cm square, fully mix
After weigh 0.50g in 10mL polypropylene centrifuge tubes, add 0.01% acetic acid/ethanol (5：1, V/V) solution 5mL, ultrasonic extraction
After 5min, supernatant is poured out in another centrifuge tube, is repeated 1 time, merges supernatant, and pH to 9.0 is adjusted with ammoniacal liquor.
2.2 enrichments, purification separate with magnetic control, then accurately weigh the more amido sub-micron molecular engram particle 3.0mg of magnetic,
It is dispersed in supernatant, ultrasound fully mixes 2min, and the more amido sub-micron molecular engrams of magnetic are made in the presence of externally-applied magnetic field
Particle buildup is centrifuging tube wall, discards solution, with the more amido sub-micron molecular engram particles of 2mL water wash magnetic, discards elution
Liquid, finally eluted with 0.5mL methanol, collect eluent, analyzed and detect for HPLC.As a result aniline and biphenyl in textile are measured
The recovery of standard addition of amine is 87.3~95.6%.
Embodiment 3：
3.1 take representative uniform wool fabric sample, and it is some to be cut into 0.5cm × 0.5cm square, fully mix
After weigh 0.50g in 10mL polypropylene centrifuge tubes, add 0.04% acetic acid/ethanol (5：1, V/V) solution 5mL, ultrasonic extraction
After 5min, supernatant is poured out in another centrifuge tube, is repeated 1 time, merges supernatant, and pH to 9.0 is adjusted with ammoniacal liquor.
3.2 enrichments, purification separate with magnetic control, then accurately weigh the more amido sub-micron molecular engram particle 3.0mg of magnetic,
It is dispersed in supernatant, ultrasound fully mixes 2min, and the more amido sub-micron molecular engrams of magnetic are made in the presence of externally-applied magnetic field
Particle buildup is centrifuging tube wall, discards solution, with the more amido sub-micron molecular engram particles of 2mL water wash magnetic, discards elution
Liquid, finally eluted with 0.5mL methanol, collect eluent, analyzed and detect for HPLC.As a result aniline and biphenyl in textile are measured
The recovery of standard addition of amine is 88.6~94.5%.
Embodiment 4：
4.1 take representative uniform wool fabric sample, and it is some to be cut into 0.5cm × 0.5cm square, fully mix
After weigh 0.50g in 10mL polypropylene centrifuge tubes, add 0.01% acetic acid/ethanol (5：1, V/V) solution 5mL, ultrasonic extraction
After 5min, supernatant is poured out in another centrifuge tube, is repeated 1 time, merges supernatant, and pH to 9.0 is adjusted with ammoniacal liquor.
4.2 enrichments, purification separate with magnetic control, then accurately weigh the more amido sub-micron molecular engram particle 3.0mg of magnetic,
It is dispersed in supernatant, ultrasound fully mixes 2min, and the more amido sub-micron molecular engrams of magnetic are made in the presence of externally-applied magnetic field
Particle buildup is centrifuging tube wall, discards solution, with the more amido sub-micron molecular engram particles of 2mL water wash magnetic, discards elution
Liquid, finally eluted with 0.5mL methanol, collect eluent, analyze and detect for HPLC.As a result aniline and connection in textile are measured
The recovery of standard addition of aniline is 67.3~78.4%.
Embodiment 5：
5.1 take representative uniform cotton swatch, and it is some to be cut into 0.5cm × 0.5cm square, claim after fully mixing
0.50g is taken in 10mL polypropylene centrifuge tubes, adds 0.5% acetic acid/ethanol (5：1, V/V) solution 5mL, ultrasonic extraction 5min
Afterwards, supernatant is poured out in another centrifuge tube, is repeated 1 time, merges supernatant, and pH to 9.0 is adjusted with ammoniacal liquor.
5.2 enrichments, purification separate with magnetic control, then accurately weigh the more amido sub-micron molecular engram particle 3.0mg of magnetic,
It is dispersed in supernatant, ultrasound fully mixes 2min, and the more amido sub-micron molecular engrams of magnetic are made in the presence of externally-applied magnetic field
Particle buildup is centrifuging tube wall, discards solution, with the more amido sub-micron molecular engram particles of 2mL water wash magnetic, discards elution
Liquid, finally eluted with 0.5mL methanol, collect eluent, analyzed and detect for HPLC.As a result aniline and biphenyl in textile are measured
The recovery of standard addition of amine is 83.6~92.8%.
Embodiment 6：
2.1 take representative uniform acrylic fiber fabric sample, and it is some to be cut into 0.5cm × 0.5cm square, fully mix
After weigh 0.50g in 10mL polypropylene centrifuge tubes, add 0.5% acetic acid/ethanol (5：1, V/V) solution 5mL, ultrasonic extraction
After 5min, supernatant is poured out in another centrifuge tube, is repeated 1 time, merges supernatant, and pH to 9.0 is adjusted with ammoniacal liquor.
2.2 enrichments, purification separate with magnetic control, then accurately weigh the more amido sub-micron molecular engram particle 3.0mg of magnetic,
It is dispersed in supernatant, ultrasound fully mixes 2min, and the more amido sub-micron molecular engrams of magnetic are made in the presence of externally-applied magnetic field
Particle buildup is centrifuging tube wall, discards solution, with the more amido sub-micron molecular engram particles of 2mL water wash magnetic, discards elution
Liquid, finally eluted with 0.5mL methanol, collect eluent, analyzed and detect for HPLC.As a result aniline and biphenyl in textile are measured
The recovery of standard addition of amine is 83.3~91.2%.
Claims (8)
1. a kind of be used for the magnetic control dispersion solid-phase extraction method of aniline and benzidine residues detecton in textile, it is characterised in that bag
Include following steps：
1) extract：Representative homogeneous sample is taken, it is some to be cut into 0.4cm~0.6cm square, is weighed after fully mixing
0.40~0.60g in 10mL polypropylene centrifuge tubes, add 0.01%~0.05 (v/v) % acetic acid solutions-alcohol mixeding liquid 4~
After 6mL, 4~6min of ultrasonic extraction, supernatant is poured out in another centrifuge tube, is at least repeated 1 time, merges supernatant,
PH to 8.5~9.5 is adjusted with ammoniacal liquor；
2) it is enriched with, purification separates with magnetic control：Then the more amido sub-micron molecular engram particles of appropriate magnetic are added in centrifuge tube,
It is ultrasonic fully to mix 1~3min, make in the presence of externally-applied magnetic field the more amido sub-micron molecular engram particle buildups of magnetic from
Heart tube wall, discards solution, with the more amido sub-micron molecular engram particles of 1.5~2.5mL water wash magnetic, discards leacheate, most
Eluted afterwards with 0.4~0.6mL methanol, collect eluent, analyzed and detect for HPLC；
The more amido sub-micron molecular engram particles of magnetic refer in polyethyleneimine (PEI) and TEPA (TEPA) amine
Base monomer and aniline and benzidine template molecule are coexisted down on the magnetic ferroferric oxide surface of coated silica through poly-
A kind of molecular imprinting composite material for closing reaction and obtaining, it is one kind in magnetic sub-micron molecular engram particle.
2. magnetic control dispersion solid-phase extraction method according to claim 1, it is characterised in that：The textile is cotton, nitrile
One kind in synthetic fibre cloth or wool fabric.
3. magnetic control dispersion solid-phase extraction method according to claim 1, it is characterised in that：Acetic acid in the step 1) is molten
Liquid is 0.04% acetic acid solution, one kind in 0.01% acetic acid solution, acetic acid solution and ethanol in acetic acid solution-alcohol mixeding liquid
Volume ratio be 1-6:1.
4. magnetic control dispersion solid-phase extraction method according to claim 3, it is characterised in that：The acetic acid solution is 0.04%
Acetic acid solution, the volume ratio of acetic acid solution and ethanol is 5 in acetic acid solution-alcohol mixeding liquid:1.
5. magnetic control dispersion solid-phase extraction method according to claim 1, it is characterised in that：The sample is cut into 0.5cm's
Square is some, and 0.50g is weighed in 10mL polypropylene centrifuge tubes after fully mixing, and adds 0.04% acetic acid solution-ethanol mixing
After liquid 5mL, ultrasonic extraction 5min, supernatant is poured out in another centrifuge tube, is repeated 1 time, is merged supernatant, is used ammoniacal liquor
Adjust pH to 9.
6. magnetic control dispersion solid-phase extraction method according to claim 1, it is characterised in that：The more amido sub-micron of magnetic
Being shaped as molecular engram particle is spherical, and particle diameter is 150~300nm, the addition of the more amido sub-micron molecular engram particles of magnetic
Amount and the weight/volume of extract solution are 1-20mg/10mL.
7. magnetic control dispersion solid-phase extraction method according to claim 6, it is characterised in that：The more amido sub-micron of magnetic
The addition of molecular engram particle and the weight/volume of extract solution are 3.0mg/10mL.
8. magnetic control dispersion solid-phase extraction method according to claim 1, it is characterised in that：It is more that the step 2) adds magnetic
Ultrasound fully mixes 2min after amido sub-micron molecular engram particle, and the more amido sub-micron of magnetic are made in the presence of externally-applied magnetic field
Molecular engram particle buildup discards solution in centrifugation tube wall, with the more amido sub-micron molecular engram particles of 2mL water wash magnetic,
Leacheate is discarded, is finally eluted with 0.5mL methanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610127227.1A CN105758963B (en) | 2016-03-07 | 2016-03-07 | It is a kind of to be used for the magnetic control dispersion solid-phase extraction method of aniline and benzidine residues detecton in textile |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610127227.1A CN105758963B (en) | 2016-03-07 | 2016-03-07 | It is a kind of to be used for the magnetic control dispersion solid-phase extraction method of aniline and benzidine residues detecton in textile |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105758963A CN105758963A (en) | 2016-07-13 |
| CN105758963B true CN105758963B (en) | 2018-01-16 |
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