CN106770826A - A kind of micro-extracting method for detecting triclosan and methyl triclosan - Google Patents
A kind of micro-extracting method for detecting triclosan and methyl triclosan Download PDFInfo
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- CN106770826A CN106770826A CN201611201108.2A CN201611201108A CN106770826A CN 106770826 A CN106770826 A CN 106770826A CN 201611201108 A CN201611201108 A CN 201611201108A CN 106770826 A CN106770826 A CN 106770826A
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a kind of micro-extracting method for detecting triclosan and methyl triclosan, ionic liquid is imidazoles naphthoic acid salt, the features such as with highly acid, slightly water-soluble and have Fluorescence Sensitizing Effect to hypofluorescence compound, can and conventional ionic liquid [C4MIM]BF4Mixing is used as the dispersant in micro-extraction program.Its synthesis step includes：1 chloromethane is reacted with N methylimidazoles, and the mol ratio of the two is 1.1~1.5, and product is obtained final product with the reaction of 1 naphthoic acid again.Present invention facilitates the nonpolar environment of extractant, the volume of precipitated phase is increased, improve the rate of recovery of TCS and MTCS up to 10 20%；Avoid the procedure of pH adjustment in micro-extraction program；Under the conditions of factor optimizing, the rate of recovery in the matrix such as blood plasma, urine sample, egg and milk is up to 98.6 106.1%；Minimum detectability as little as 0.12 0.66 μ g/L.
Description
Technical field
The invention belongs to bactericide detection technique field, more particularly to a kind of micro- extraction for detecting triclosan and methyl triclosan
Take method.
Background technology
At present, 2,4,4'- tri- chloro- 2'- dihydroxy diphenyl ethers (triclosan, TCS) are a kind of broad-spectrum germicides, can be answered extensively
For such as toothpaste, shampoo, hand cleanser in personal care product and household cleaning agent.Due to excessive abuse, TCS into
It is a kind of ubiquitous pollutant in many matrix, these matrix include water sample, biological fluid and varieties of food items.Largely grind
Study carefully and show：TCS can be changed under illumination condition 2,8- dichloros simultaneously-p- dioxin (2,8-DCDD), this compound quilt
The toxicity carcinogen being known as in the world.Methyl triclosan (MTCS) is the methylate of TCS, compared with TCS, it
logKowIt is 5.4 to be worth, and the log of TCSKowIt is 4.8 to be worth, therefore there is MTCS lipophilicity higher to cause to enable it to easily, also more
Lasting accumulation in vivo.TCS and MTCS belongs to incretion interferent, can be detected in fish, algae and human body
To the presence of which, while detection is carried out to TCS and MTCS can more really react the pollution condition of TCS.Have at present
Close the extensive concern that TCS and MTCS has caused environmental science circle to the potential threat that human health is present.
So far, several sample pretreating methods are applied to detect the TCS and MTCS in sample, these sides
Method includes SPE (SPE), SPME (SPME), doughnut combination liquid-phase micro-extraction (HF-LPME), stirring rod extraction
Take (SBSE), liquid-liquid extraction (LLE), dispersion liquid micro-extraction (DLLME).In addition to DLLME, other sample pretreating methods have aobvious
The shortcoming of work such as takes, high cost, not environmentally.Although DLLME has many significant advantages compared with other method, such as in reality
, in micro updating, extraction time is short etc. for the extractant and dispersion dosage needed during testing.But the main of it has the disadvantage to use
To environment and the harmful organic solvent of human body as extractant and dispersant.Therefore, more environmentally-friendly dividing based on ionic liquid
Scattered micro-extraction technique is increasingly paid close attention to and welcome by people.
In sum, existing sample pretreating method have that time-consuming, high cost, not environmentally.
The content of the invention
It is an object of the invention to provide a kind of micro-extracting method of detection triclosan TCS and methyl triclosan MTCS, purport
Solve the problems, such as existing sample pretreating method have that time-consuming, high cost, not environmentally.
Ionic liquid of the present invention is [C4MIM][NPA]；
The ionic liquid synthesis includes：N- methylimidazoles are in single-necked flask and 1- chloromethanes；1- chloromethanes are
1.1~1.5 times of N- methylimidazole moles.
Another object of the present invention is to provide a kind of preparation method of the ionic liquid, the preparation of the ionic liquid
Method is comprised the following steps：
(1) N- methylimidazoles are weighed in single-necked flask, then weighs 1- chloromethanes, be added dropwise in single-necked flask, be added dropwise
After finishing, in after back flow reaction 24h at 80 DEG C, reaction completely, liquid in cooling system boils off unnecessary 1- chloromethanes, obtains
Faint yellow solid；
(2) weigh NaOH in beaker, with water dissolves, then weigh 1- naphthoic acids in single-necked flask, will dissolving it is complete
In NaOH addition systems, in 80 DEG C react 24h, react yellow solution, after completion of the reaction, boil off part water, surplus solution
It is used as the next step.
(3) faint yellow solid is weighed, is added in yellow solution, 24h, after completion of the reaction, vacuum distillation are reacted at 60 DEG C
The water gone in system, adds absolute ethyl alcohol, has NaCl to separate out, and is put into refrigerator freezing 3h, leaches out NaCl solids in system, hangs and steams
Dry solvent obtains final product product [C4MIM][NPA]。
It is a kind of using the ionic liquid detection triclosan TCS and methyl triclosan another object of the present invention is to provide
The micro-extracting method of MTCS, the described method comprises the following steps：
(1) the sample 1mL that will be handled well is added in the centrifuge tube of 15mL, is diluted with water to 5mL, adds 20-120 μ L miaows
Azoles hexafluorophosphoric acid salt ionic liquid [CnMIM][PF6] (n=4-8), 45-135 μ L tetrafluoroborate class ionic liquids
[CnMIM][BF4] (n=2-4) and 45-135 μ L 1- butyl -3- methyl-imidazoles naphthoic acid class ionic liquids [C4MIM][NPA]
Mixture be added in centrifuge tube, milk shape uniform liquid, subsequent ultrasound 0-10min are formed after vibration, and add 0-0.17g
NH4PF6Salt, is put into ice bath after vortex and cools down 1-11min；
(2) centrifuge tube is put into centrifuge and 0-10min is centrifuged with 3000rpm, the water on upper strata is removed after realizing being separated
Phase, then with liquid-transfering gun take out lower floor precipitated phase be put into the centrifuge tube of 1mL, with flowing phase dilution after use membrane filtration again
Afterwards, enter High Performance Liquid Chromatography/Photodiode Array Detection to be analyzed object.
Further, the High Performance Liquid Chromatography/Photodiode Array Detection analysis condition is：Mobile phase is acetonitrile A, methyl alcohol
B and ultra-pure water C carry out binary gradient elutes with 1.5mL/min flow velocitys；Gradient elution program is as follows：0min, 75%A；3min,
65%A；5min, 50%A；7min 80%A and 8-14min 70%A；Total run time is 8min, and sample size is 20 μ L,
Detection wavelength is 280nm, 30 DEG C of column temperature.
Further, the dispersant [C4MIM][BF4]+[C4MIM] [NPA] cumulative volume is 150 μ L, the volume ratio of the two is
4:1。
Side another object of the present invention is to provide TCS and MTCS in a kind of detection blood sample using the ionic liquid
Method.
Side another object of the present invention is to provide TCS and MTCS in a kind of detection urine sample using the ionic liquid
Method.
Side another object of the present invention is to provide TCS and MTCS in a kind of detection milk using the ionic liquid
Method.
Side another object of the present invention is to provide TCS and MTCS in a kind of detection egg using the ionic liquid
Method.
The present invention provide detection triclosan TCS and methyl triclosan MTCS micro-extracting method, pretreatment technology with it is normal
The dispersive liquid-liquid microextraction technology of rule is compared, and 1- naphthoic acids is introduced into imidazole ring and has synthesized a kind of new ionic liquid 1- fourths
Base -3- methylimidazole naphthoates ([C4MIM][NPA]).During micro-extraction, by new ionic liquid and 1- butyl-
3- methyl imidazolium tetrafluoroborates ([C4MIM][BF4]) mix by a certain percentage as a kind of mixed type dispersant, novel ion
Application have：Improve the rate of recovery 10-20% of TCS and MTCS；New naphthoate ionic liquid tool highly acid, therefore its
Itself can be as pH adjusting agent, it is to avoid the procedure of pH adjustment in micro-extraction program, makes the micro-extraction technique more simple to operate
Change；It is a kind of simple, quick and environmentally friendly detection method.
TCS and MTCS analyses that the present invention can be used in human body fluid (such as blood sample, urine sample) and food；In the invention I
Synthesized ionic liquid (1- butyl -3- methyl-imidazoles naphthoates, [C4MIM] [NPA]) and be applied to " entirely from
In sub- liquid micro-extraction ".The synthesis condition of the ionic liquid is ripe, reproducible；New ionic liquid and conventional ionic liquid
It is used in mixed way as dispersant, the rate of recovery that can improve TCS and MTCS reaches 10-20%；Additionally, its strong acid sexual function can be used as pH
Conditioning agent is used, it is to avoid the procedure of pH adjustment in micro-extraction program, makes micro-extraction technique more simple operation；It is a kind of letter
Single, quick and environmentally friendly pre-treating method, the TCS that can be used in human body fluid (such as blood sample, urine sample) and food and
MTCS is analyzed, and belongs to " Green Analytical Chemistry " research field.
New naphthoate ionic liquid used in the present invention has relatively low water solubility, promotes the non-of extractant
Polar environment, and then increased the volume of precipitated phase, therefore improve the rate of recovery of TCS and MTCS and reach 10-20%；Pre-treatment skill
Art has highly acid in itself due to new naphthoate ionic liquid, so its own as pH adjusting agent, therefore can be kept away
The procedure of pH adjustment in micro-extraction program is exempted from；Under the conditions of factor optimizing, in the matrix such as blood plasma, urine sample, egg and milk
TCS the and MTCS rate of recovery up to 98.6-106.1%；Minimum detectability as little as 0.12-0.66 μ g/L.Based on this, the present invention has
Have the advantages that test limit is low, extraction yield is high, the operating time is short, no using any organic solvent.
Brief description of the drawings
Fig. 1 is the micro-extracting method flow of detection triclosan TCS and methyl triclosan MTCS provided in an embodiment of the present invention
Figure.
Fig. 2 is [C provided in an embodiment of the present invention4MIM] [NPA] nuclear-magnetism spectrum schematic diagram.
Fig. 3 is " full ionic liquid micro-extraction " operation sequence schematic diagram provided in an embodiment of the present invention.
Fig. 4 is TCS the and MTCS chromatographic peak schematic diagrames in blood sample provided in an embodiment of the present invention and urine sample.
Fig. 5 is TCS the and MTCS chromatographic peaks in milk provided in an embodiment of the present invention and egg.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Application principle of the invention is explained in detail below in conjunction with the accompanying drawings.
As shown in figure 1, the method for detection TCS and MTCS provided in an embodiment of the present invention is comprised the following steps：
S101：The actual sample 1mL that will be handled well first is added in the centrifuge tube of 15mL, is diluted with water to 5mL, is added
20-120 μ L limidazolium hexafluorophosphate class ionic liquids [CnMIM][PF6] (n=4-8), 45-135 μ L tetrafluoroborate classes
Ionic liquid [CnMIM][BF4] (n=2-4) and 45-135 μ L 1- butyl -3- methylimidazole naphthoic acid salt ionic liquids
[C4MIM] mixture of [NPA] is quickly adding into centrifuge tube, and milk shape uniform liquid, subsequent ultrasound 0- are formed after vibration
10min, and add the NH of 0-0.17g4PF6Salt, is put into ice bath after vortex and cools down 1-11min；
S102：Centrifuge tube is put into centrifuge 0-10min is centrifuged with 3000rpm, upper strata is removed after realizing being separated
Water phase；
S103：The precipitated phase for taking out lower floor with liquid-transfering gun is put into the centrifuge tube of 5mL, with filter membrane after flowing phase dilution
(0.22um), High Performance Liquid Chromatography/Photodiode Array Detection (HPLC-DAD) is analyzed to object.
The micro-extracting method of detection triclosan TCS and methyl triclosan MTCS provided in an embodiment of the present invention specifically include with
Lower step：
Full ionic liquid dispersion micro-extraction technique of the invention contains come the TCS and MTCS in detecting human body fluid and various food
Amount, in turn includes the following steps：
The first step：The preparation of naphthoate ionic liquid：
With N- methylimidazoles and 1- chloro-normal butanes as raw material, 40 DEG C of reactions introduce naphthoic acid sodium, finally after the completion of reaction
Form target product.Reaction needs three steps, gross production rate to be about 62.64% altogether.
Synthesis chemical equation such as equation is as follows：
Second step：The actual sample 1mL that will be handled well first is added in the centrifuge tube of 15mL, is diluted with water to 5mL, plus
Enter 20-120 μ L limidazolium hexafluorophosphate class ionic liquids [CnMIM][PF6] (n=4-8), 45-135 μ L tetrafluoroborates
Class ionic liquid [CnMIM][BF4] (n=2-4) and 45-135 μ L 1- butyl -3- methyl-imidazoles naphthoic acid class ionic liquids
[C4MIM] mixture of [NPA] is quickly adding into centrifuge tube, and milk shape uniform liquid, subsequent ultrasound 0- are formed after vibration
10min, and add the NH of 0-0.17g4PF6Salt, is put into ice bath after vortex and cools down 1-11min, and centrifuge tube finally is put into centrifugation
0-10min is centrifuged with 3000rpm in machine, the water phase on upper strata is removed after realizing being separated, then take out the heavy of lower floor with liquid-transfering gun
Shallow lake is mutually put into the centrifuge tube of 5mL, and with filter membrane (0.22um) after flowing phase dilution, HPLC-DAD is analyzed to object,
Gradient elution, sample size is 20 μ L, and Detection wavelength is 280nm, 30 DEG C of column temperature.
Application principle of the invention is further described with reference to specific embodiment.
Embodiment 1：[C4MIM] [NPA] synthesis
Step 1：N- methylimidazoles 4g (48.7mmol) are weighed in single-necked flask, then weighs 1- chloromethanes 6.68g
(72.2mmol) (about 1.1~1.5 times of N- methylimidazoles mole), are slowly added dropwise in single-necked flask, after completion of dropping,
In back flow reaction 24h at 80 DEG C, thin-layered chromatography monitoring reaction, after reaction completely, liquid in cooling system boils off unnecessary 1-
Chloromethane, obtains white solid, and yield is 90%.Step 2：Weigh 1.8g NaOH (45mmol) (NaOH slightly mistakes in beaker
Amount), dissolved with little water, then 1- naphthoic acids 7.53g (43.8mmol) are weighed in single-necked flask, complete NaOH will be dissolved
In addition system, 24h are reacted in 80 DEG C, react yellow solution, point plate monitoring after completion of the reaction, boils off part water, remaining
Solution is used as the next step.Step 3：Solid 7.67g (43.8mmol) in step 1 is weighed, the yellow that step 2 obtains is added to molten
In liquid, 24h is reacted at 60 DEG C, high-efficient liquid phase chromatogram technique monitoring reacts, after completion of the reaction, the water that vacuum distillation is gone in system, plus
Enter absolute ethyl alcohol, there is NaCl is separated out, and is put into refrigerator freezing 3h, leaches out NaCl solids in system, and outstanding solvent evaporated obtains final product product,
Product is brown crystalline, and yield is 62%.[C4MIM] [NPA]1H NMR are characterized as below Fig. 2.
Embodiment 2：The detection of TCS and MTCS in blood sample
Blood pre-treatment：1mL healthy premenopausal volunteers serum is added in 10mL centrifuge tubes, the vibration of 4mL acetonitriles is subsequently adding
2min, is placed in 85 DEG C of water-bath and heats 15min afterwards, and 15min is centrifuged with 5000rpm rotating speeds after cooling, is taken after centrifugation
Clear liquid filters (0.45 μm of filter membrane), then 5min is centrifuged with 10000rpm rotating speeds, takes supernatant liquor for actual sample.Follow-up is " complete
Ionic liquid micro-extraction " operation sequence See Figure 3.
HPLC testing conditions：Mobile phase carries out two for acetonitrile (A), methyl alcohol (B) and ultra-pure water (C) with 1.5mL/min flow velocitys
First gradient elution.Gradient elution program is as follows：0min, 75% acetonitrile；3min, 65% acetonitrile；5min, 50% acetonitrile；7min,
80% acetonitrile and 8-14min, 70% acetonitrile, total run time is 8min.Sample size is 20 μ L, and Detection wavelength is 280nm column temperatures
30℃.The μ L of sample size 20.TCS and MTCS detections chromatographic peak is shown in Fig. 4 in blood sample.
Embodiment 3：TCS and MTCS detection in urine sample
Urine pre-treatment：3mL healthy premenopausal volunteers urines are added in 10mL centrifuge tubes, is then centrifuged with 4000rpm
10min, then supernatant liquid filtering (0.22 μm of filter membrane) is taken, it is the actual sample handled well to take supernatant liquor.
HPLC testing conditions：Mobile phase carries out two for acetonitrile (A), methyl alcohol (B) and ultra-pure water (C) with 1.5mL/min flow velocitys
First gradient elution.Gradient elution program is as follows：0min, 75% acetonitrile；3min, 65% acetonitrile；5min, 50% acetonitrile；7min
80% acetonitrile and the acetonitrile total run times of 8-14min 70% are 8min.Sample size is 20 μ L, and Detection wavelength is 280nm, column temperature
30 DEG C, the μ L of sample size 20.TCS and MTCS detections chromatographic peak is shown in Fig. 4 in urine sample.
Embodiment 4：TCS and MTCS detection in egg
Egg pre-treatment：The egg that will be bought takes out 1mL (about 1g) egg white, adds the ultra-pure water of 2mL, the 20% of 0.5mL
Glacial acetic acid, then the acetonitrile of 4mL is put into centrifuge tube, is put into after vortex instrument vibrates 5min on 80 DEG C of water-bath and steamed
Mixeding liquid volume about 3mL is sent to, then by the low speed of 4800rpm, supernatant 1mL is taken and is added in the centrifuge tube of 10mL, used
Water is diluted to 5mL.Following step is similar with DLLME.The extractant of 30-110 μ L, 40-120 are added after being vibrated with vortex instrument
The dispersant of μ L, after oscillating ultrasonic 3-11min, adds 0-0.2g salt, after ultrasonic 3min, 20min is cooled down, then in 3000rpm
Centrifugation 8min, takes out the organic phase of lower floor with liquid-transfering gun after the water phase on removal upper strata, add 60 μ L methyl alcohol, HPLC-DAD detections.
HPLC testing conditions：Mobile phase is acetonitrile (A) and ultra-pure water (B) with 1.5mL min-1Flow velocity carries out binary gradient and washes
It is de-.Wash-out 75% (A) and 25% (B), total run time is 11min.Sample size 20 μ L, Detection wavelength 280nm, column temperature 30
℃.TCS and MTCS chromatographic peaks in egg are shown in Fig. 5.
Embodiment 5：TCS and MTCS detection in milk
Milk pre-treatment：Milk 1.00mL accurately is measured, the ultra-pure water of the acetic acid of 200 μ L 20% and 2.80mL is added into
In, 1min is shaken, 15min is preserved at 4 DEG C, 15min then is centrifuged in 3000rpm, take out the filter that supernatant crosses 0.22 μm
Film, adds the n-hexane of 5mL, vortex 1min that 10min is centrifuged in 4500rpm, and removal n-hexane layer is crossed 0.22 μm of filter membrane, obtained
Milk supernatant.The supernatant for taking 1mL adds 4mL acetonitriles, shakes 2min, and 15min is heated under the conditions of 95 DEG C, is evaporated to 2mL,
15min is centrifuged under the conditions of 5000rpm using centrifuge, finally takes supernatant and is preserved with 0.45 μm of membrane filtration, its filtering
Liquid is analyzed for HPLC.
HPLC testing conditions：Mobile phase carries out binary gradient elutes for acetonitrile (A) ultra-pure water (B) with 1.5mL/min flow velocitys.
Gradient elution program is as follows：0min, 75% acetonitrile；3min, 65% acetonitrile；5min, 50% acetonitrile；The acetonitriles of 7min 80% and 8-
The acetonitriles of 14min 70%, total run time is 8min, and sample size is 20 μ L, and Detection wavelength is 280nm, 30 DEG C of column temperature, sample size
20μL.TCS and MTCS chromatographic peaks in milk are shown in Fig. 5.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, it is all in essence of the invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (9)
1. a kind of ionic liquid, it is characterised in that the ionic liquid is imidazoles naphthoic acid salt；
The preparation of the ionic liquid is reacted in single-necked flask using N- methylimidazoles with 1- chloromethanes；1- chloromethanes are
1.1~1.5 times of N- methylimidazole moles.
2. a kind of preparation method of ionic liquid as claimed in claim 1, it is characterised in that the preparation method of the ionic liquid
Comprise the following steps：
(1) N- methylimidazoles are weighed in single-necked flask, then weighs 1- chloromethanes, be added dropwise in single-necked flask, completion of dropping
Afterwards, in back flow reaction 24h at 80 DEG C, after reaction completely, liquid in cooling system boils off unnecessary 1- chloromethanes, obtains yellowish
Color solid；
(2) weigh NaOH in beaker, with water dissolves, then weigh 1- naphthoic acids in single-necked flask, will the complete NaOH of dissolving
In addition system, 24h are reacted in 80 DEG C, react yellow solution, after completion of the reaction, part water is boiled off, under surplus solution is made
Step reaction is used；
(3) faint yellow solid is weighed, is added in yellow solution, 24h is reacted at 60 DEG C, after completion of the reaction, body is removed in vacuum distillation
Water in system, adds absolute ethyl alcohol, has NaCl to separate out, and is put into refrigerator freezing 3h, leaches out NaCl solids in system, it is outstanding be evaporated it is molten
Agent obtains final product product [C4MIM][NPA]。
3. ionic liquid described in a kind of utilization claim 1 detects the micro-extracting method of triclosan TCS and methyl triclosan MTCS,
Characterized in that, the detection method is comprised the following steps：
(1) the sample 1mL that will be handled well is added in the centrifuge tube of 15mL, is diluted with water to 5mL, adds 20-120 μ L imidazoles six
Fluorophosphoric acid salt ionic liquid [CnMIM][PF6] (n=4-8), 45-135 μ L tetrafluoroborate class ionic liquids [CnMIM]
[BF4] (n=2-4) and 45-135 μ L 1- butyl -3- methylimidazole naphthoic acid salt ionic liquids [C4MIM] [NPA] mixing
Thing is added in centrifuge tube, milk shape uniform liquid, subsequent ultrasound 0-10min is formed after vibration, and add 0-0.17g's
NH4PF6Salt, is put into ice bath after vortex and cools down 1-11min；
(2) centrifuge tube is put into centrifuge and 0-10min is centrifuged with 3000rpm, the water phase on upper strata is removed after realizing being separated, so
The precipitated phase for taking out lower floor with liquid-transfering gun afterwards is put into the centrifuge tube of 5mL, with filter membrane, high-efficient liquid phase color after flowing phase dilution
Spectrum-PDAD is analyzed to object.
4. the micro-extracting method of triclosan TCS and methyl triclosan MTCS is detected as claimed in claim 3, it is characterised in that
The High Performance Liquid Chromatography/Photodiode Array Detection analysis condition is：Mobile phase be acetonitrile A, methyl alcohol B and ultra-pure water C with
1.5mL/min flow velocitys carry out binary gradient elutes；Gradient elution program is as follows：0min, 75%A；3min, 65%A；5min,
50%A；7min 80%A and 8-14min70%A；Total run time is 8min, and sample size is 20 μ L, and Detection wavelength is
280nm, 30 DEG C of column temperature.
5. the micro-extracting method of triclosan TCS and methyl triclosan MTCS is detected as claimed in claim 3, it is characterised in that
Dispersant [the C4MIM][BF4]+[C4MIM] [NPA] cumulative volume be 150 μ L, the volume ratio of the two be 4:1.
6. the blood sample that ionic liquid described in a kind of utilization claim 1 is detected.
7. the urine sample that ionic liquid described in a kind of utilization claim 1 is detected.
8. the milk that ionic liquid described in a kind of utilization claim 1 is detected.
9. the egg that ionic liquid described in a kind of utilization claim 1 is detected.
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| CN108918713A (en) * | 2018-07-18 | 2018-11-30 | 香港浸会大学深圳研究院 | A kind of triclosan ichthyodin and the preparation method and application thereof |
| CN109612819A (en) * | 2018-11-28 | 2019-04-12 | 温州医科大学 | Based on pretreatment technology and its application associated with enzymatic hydrolysis auxiliary and solidification floating drop micro-extraction |
| CN109738561A (en) * | 2018-12-13 | 2019-05-10 | 温州医科大学 | Triclosan and methyl triclosan detection method in a kind of body fluid based on reaction in-situ micro-extraction technique |
| CN111443136A (en) * | 2020-03-03 | 2020-07-24 | 温州医科大学 | Double-positive ionic liquid as extractant and application thereof in enrichment and detection of polycyclic aromatic hydrocarbon in meat products |
| CN113252815A (en) * | 2021-06-16 | 2021-08-13 | 中国科学院地理科学与资源研究所 | Method for detecting triclosan and triclocarban in sludge compost |
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| CN108918713B (en) * | 2018-07-18 | 2021-03-16 | 香港浸会大学深圳研究院 | Ammonium triclosan sulfonate and preparation method and application thereof |
| CN109612819A (en) * | 2018-11-28 | 2019-04-12 | 温州医科大学 | Based on pretreatment technology and its application associated with enzymatic hydrolysis auxiliary and solidification floating drop micro-extraction |
| CN109738561A (en) * | 2018-12-13 | 2019-05-10 | 温州医科大学 | Triclosan and methyl triclosan detection method in a kind of body fluid based on reaction in-situ micro-extraction technique |
| CN111443136A (en) * | 2020-03-03 | 2020-07-24 | 温州医科大学 | Double-positive ionic liquid as extractant and application thereof in enrichment and detection of polycyclic aromatic hydrocarbon in meat products |
| CN111443136B (en) * | 2020-03-03 | 2021-08-10 | 温州医科大学 | Double-positive ionic liquid as extractant and application thereof in enrichment and detection of polycyclic aromatic hydrocarbon in meat products |
| CN113252815A (en) * | 2021-06-16 | 2021-08-13 | 中国科学院地理科学与资源研究所 | Method for detecting triclosan and triclocarban in sludge compost |
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