CN103529146A - Method of extracting medicine residues of sulfonamides from chicken by utilization of ionic liquid - Google Patents
Method of extracting medicine residues of sulfonamides from chicken by utilization of ionic liquid Download PDFInfo
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- CN103529146A CN103529146A CN201310467886.6A CN201310467886A CN103529146A CN 103529146 A CN103529146 A CN 103529146A CN 201310467886 A CN201310467886 A CN 201310467886A CN 103529146 A CN103529146 A CN 103529146A
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Abstract
The invention relates to a method of extracting medicine residues of seven sulfonamides from chicken by utilization of an ionic liquid and achieving an objective of purification during extraction purification, through adjusting the pH value, the water amount and the salt amount in the ionic liquid to achieve homogeneous phase extraction and layered purification, wherein the seven sulfonamides residues comprise sulfathiazole (ST), sulfamerazine (SMR), sulfamethizole (STZ), sulfadimidine (SDMD), sulfachlorpyridazine (SCP), sulfamethoxazolum (SMZ), and sulfisoxazole (SIX). Liquid chromatographic analysis results show that the recovery rate of each of the sulfonamides is 82.1%-108%, and the relative standard deviation is 0.5%-5.9%. The green and simple extracting method is established so as to reduce pollution or harm of traditional organic solvent extraction methods to the environment and to experiment persons.
Description
Technical field
The invention belongs to ionic liquid extract separation technology field.Specifically, it is tasteless that this invention relates to a kind of ionic liquid that utilizes, do not fire, non-volatile and good dissolution characteristics, employing, by regulating pH value and adding a certain amount of salt, is extracted the object that then layering purifies thereby reach homogeneous state, thereby set up a kind of extracting method of simple environmental protection, to substitute traditional volatile organic solvent extracting method.
Background technology
Measure the residual method of generally using of sulfanilamide (SN) and be mainly liquid phase chromatography and Liquid Chromatography-Tandem Mass Spectrometry coupling method.In these methods, sulfanilamide (SN) is organic solvent acetonitrile extraction, and malicious class is larger, and acute toxicity is LD
502730mg/kg (rat oral); 1250mg/kg (rabbit is through skin); LC
5012663mg/m
3within 8 hours, people sucks > 500ppm, there will be the symptoms such as nauseating, vomiting, uncomfortable in chest, stomachache, long-term suction can cause that liver, kidney and lung pathology change, and cause that sex chromosome disappearance is not with separated, muscle skeleton dysplasia, its steam and air can form explosive mixture.Meet naked light, Gao Re or contact with oxygenant, having the danger of introducing combustion explosion.National standard is more at the impurity extracting with acetonitrile at present, also must purify with solid phase extraction column, and its complex steps, workload is large, and object is subject to loss during the course.
The pKa wide ranges of sulfa drugs is difficult to extract with separated simultaneously.In GB GBS/T20759-2006, sample is first used acetonitrile extracted twice, adds isopropyl alcohol, by rotary evaporated to dryness, more repeatedly adds mobile phase and normal hexane to carry out the purified treatment of liquid-liquid extraction degrease.And first with acetonitrile, extract in SN0498-95, more repeatedly carry out after liquid-liquid extraction with normal hexane and methenyl choloride, with diazomethane-ether, carry out alkylation derivatization reaction, in SN/T2580-2010, sample first extracts with ethyl acetate, then with using respectively MCX and C
18pillar carries out purified treatment.In above-mentioned pre-treatment overall process, all can use a large amount of organic solvents, operating personnel and organic solvent are long duration of contact, and complex steps, and workload is large, need expend a large amount of human and material resources.
Due to ionic liquid have non-volatile, non-combustible, thermal capacitance is large, vapour pressure is little, therefore can reduce the problem of environmental pollution producing because of volatilization, be conducive to experimenter healthy, more for the extraction research of ionic liquid sulfanilamide (SN) in Environmental Water at present, its method is mainly the enrichment function by ionic liquid, takes the sulfanilamide (SN) in the method enrichment water of liquid-liquid micro-extraction.The method is due to ionic liquid used trace, and can not be water-soluble, its method exist less stable and analysis time longer problem, and can only be for the simple Environmental Water of matrix, can not be for the sample of solid and matrix complexity.
The present invention is directed to by regulating pH value, the consumption of ionic liquid, the consumption of water, temperature of reaction is carried out abstraction reaction under homogeneous phase condition, can make ionic liquid fully contact with matrix, and extraction efficiency is improved, and reduces the abstraction reaction time.And by controlling addition and the reaction conditions of salt, make its layering, play clean-up effect, and fully used the ionic liquid after layering again to extract, reduced and in analytic process, extracted solvent volume, by the step that circulation homogeneous phase extracts, layering purifies, the present invention utilizes ionic liquid to extract 7 kinds of sulfa drug residues in chicken, and its recovery is between 80%-114%.Its operating conditions is simple, and whole process steps seldom, thereby can guarantee that sulfa drugs loss is less; In addition the vapour pressure of ionic liquid is almost nil, there will not be as organic solvent because volatilization causes environmental problem.Experimentation agents useful for same amount is little; especially organic solvent acetonitrile amount only has 1.4mL; also only used in this step of constant volume; time is shorter; can protect well operating personnel to avoid sucking organic solvent; reducing the pollution of organic solvent to environment, is therefore a kind of extracting method of simple environmental protection, can be to substitute traditional volatile organic solvent extracting method.
Summary of the invention
For above-mentioned situation, the object of this invention is to provide seven kinds of sulfa drug residue extracting method in a kind of simple chicken efficiently.
The present invention is achieved through the following technical solutions.
(1) preparation of extract
Water, 1-hexyl-3-methyl imidazolium tetrafluoroborate and glacial acetic acid are put into container in the ratio of 5: 1: 0.1, after stirring, water and ionic liquid are dissolved each other, become homogeneous phase, as the residual extract of chicken sulfonamides.
(2) high speed dispersion
The extract that 6mL step (1) is obtained is heated to 30～40 ℃ of temperature, join in the chicken of 2 grams of left and right, then use the high speed dispersion instrument of 4000～8000rpm (preferably 5000-7000rpm) to disperse 60～90s, after vortex after ultrasonic extraction 3min, centrifugal 5min (8000r/min), draws supernatant.
(3) extract layering
The Na that adds 1.08g left and right in the supernatant obtaining in step (2)
2hPO
412H
2o, 1mL1-hexyl-3-methyl imidazolium tetrafluoroborate, vortex static layering, after water layer separates with ionic liquid, draws water layer to remove, and again adds 1mL1-hexyl-3-methyl imidazolium tetrafluoroborate.
(4) again extract
The ionic liquid obtaining in step (3), add in the chicken having extracted, add 1mL water, 0.1mL glacial acetic acid, then use the high speed dispersion instrument of 4000～8000rpm (preferably 5000-7000rpm) to disperse 60～90s, ultrasonic extraction 3min after vortex, centrifugal 5min (8000r/min), inclines and supernatant.
(5) secondary clearing again
Supernatant adds the centrifugal 2min of 0.54gNa2HPO412H2O, solion and water layer layering
(6) dilution constant volume
Draw this solion of 0.6mL to 2mL volumetric flask, with ultrapure water: glacial acetic acid (volume ratio 8: 2) mixed solution is settled to scale.
Beneficial effect of the present invention: adopt the simple extracting method such as high speed dispersion and vortex, utilize the character of ionic liquid to extract sulfa drug residue in chicken, overturned organic solvent extraction in classic method, the concept that Solid-Phase Extraction or liquid-liquid extraction purify.By adding glacial acetic acid to regulate pH value, make ionic liquid and water form homogeneous system, adopt high speed dispersion and ultrasonic power to extract the sulfanilamide (SN) in chicken, then by adding a certain amount of inorganic salts, adopt centrifugal mode, make water separated with ionic liquid, by sulfanilamide (SN) separation and concentration in ionic liquid, stay in water with the water miscible impurity of major part, thereby arrive the concentrated object of enrichment.According to above-described method, the method validation reclaiming with mark-on the validity of 7 kinds of sulfanilamide (SN) in ionic liquid extract chicken, combine Ultra Performance Liquid Chromatography the sulfanilamide (SN) in chicken detected, and method is assessed.Result shows that the recovery of 3 interpolation levels (0.05,0.1,0.2mg/kg) is between 82%～103%, and relative standard deviation (RSD) is 5.3%～9.6%.With the comparison of conventional organic solvents extraction, there is nontoxic, safe feature, and solvent species and consumption little, extraction cost is low, and simple and efficient, the recovery is high, meets rules residue limits monitoring requirement.
Embodiment
Below in conjunction with embodiment, the present invention is described in more detail.
7 kinds of sulfamido standard substances that the present invention uses are provided by German Dr.Ehrenstorfer company, and purity is all greater than 99.8%
(1) preparation of extract
Water, 1-hexyl-3-methyl imidazolium tetrafluoroborate and glacial acetic acid are put into container in the ratio of 5: 1: 0.1, regulate its pH value, after stirring, water and ionic liquid are dissolved each other, become homogeneous phase, as the residual extract of chicken sulfonamides.
Experiment shows that PH size has larger impact to extraction efficiency, pH size is influential to the polarity of solion, when pH < 3, solion has Precipitation phenomenon, the effect that the solion of different pH sizes extracts sulfanilamide (SN) in water is different, and every kind of influenced varying in size of sulfanilamide (SN), as when the pH=6, the extraction efficiency of solion is less, and the recovery of ST is only 54.0%; When pH=4, the extraction efficiency of solion is less, and the recovery of ST is only 60.0%; When pH=2, the extraction efficiency of solion is less, and the recovery of ST is only 53.0%; And PH is between 3-3.5 time, its recovery, all 80%, therefore determines that best PH scope is between 3-3.5.
(2) high speed dispersion
The extract that 6mL step (1) is obtained is heated to 30～40 ℃ of temperature, join in the chicken of 2 grams of left and right, then use the high speed dispersion instrument of 4000～8000rpm (preferably 5000-7000rpm) to disperse 60～90s, after vortex after ultrasonic extraction 3min, centrifugal 5min (8000r/min), draws supernatant.
The material ratio of extract and chicken is larger, and its extraction efficiency is better, but material ratio is excessive, and its experimental cost can increase, and causes unnecessary consumption.But the too small meeting of material ratio has influence on extraction efficiency.Through experiment, repeatedly prove that material ratio is is the best at 3: 1.Heating can make the solubleness of sulfa drugs in extracting solution improve, and increases the recovery, but excess Temperature can make again sulfanilamide (SN) decompose, and therefore controlling and extracting temperature is 30～40 ℃.High speed disperser can be used for animal, plant tissue homogenate is pulverized, and cell disperses, and is conducive to the extraction of medicament residue in fowl carcass.First chicken and aqueous solution have formed heterogeneous system, and the effect of dispersion is to make Chicken Tissues broken, and along with the fragmentation of Chicken Tissues, extract and chicken form homogeneous system on the one hand, and extract contacts fully with chicken, is easy to extract; On the other hand, sulfa drugs is fully stripping under peptizaiton, has increased the recovery of object.Ultrasonic and vortex is equal
(3) extract layering
The Na that adds 1.08g left and right in the supernatant obtaining in step (2)
2hPO
412H
2o, 1mL1-hexyl-3-methyl imidazolium tetrafluoroborate, vortex static layering, after water layer separates with ionic liquid, draws water layer to remove, and again adds 1mL1-hexyl-3-methyl imidazolium tetrafluoroborate.
Experimental results show that: salinity is the obvious effect of comparing with separated and ionic liquid with the water of water to ionic liquid.The increase that has just started to compare with salinity increases, but be increased to, to a certain degree compare afterwards and reduces with the increase of salinity, and downtrending tends towards stability.The reason that causes this phenomenon may be due to the upper and lower two alternate salting-out effects that occurred, so the solubleness of salt is also larger on the one-tenth phase situation impact of ionic liquid aqueous two-phase.The obvious effect compared of the concentration of ionic liquid to ionic liquid aqueous two-phase, compares along with the increase of ionic liquid concentration and increases.In order to save the consumption of ionic liquid and salt, increase concentration effect, we have determined ionic liquid 1-hexyl-3-methyl imidazolium tetrafluoroborate and Na
2hPO
412H
2it is 1-hexyl-3-methyl imidazolium tetrafluoroborate: Na that the best of O becomes phase condition
2hPO
412H
2o: cumulative volume is 1.08: 1: 6
(4) again extract
The ionic liquid obtaining in step (3), add in the chicken having extracted, add 1mL water, 0.1mL glacial acetic acid, then use the high speed dispersion instrument of 4000～8000rpm (preferably 5000-7000rpm) to disperse 60～90s, ultrasonic extraction 3min after vortex, centrifugal 5min (8000r/min), inclines and supernatant.
For obtaining optimum extraction effect, we have determined ionic liquid 1-hexyl-3-methyl imidazolium tetrafluoroborate and Na
2hPO
412H
2it is 1-hexyl-3-methyl imidazolium tetrafluoroborate: Na that the best of O becomes phase condition
2hPO
412H
2o: cumulative volume is 1.08: 1: 6
(5) secondary clearing again
Supernatant adds 0.54gNa
2hPO
412H
2the centrifugal 2min of O, solion and water layer layering.
(6) dilution constant volume
Draw this solion of 0.6mL to 2mL volumetric flask, with ultrapure water: glacial acetic acid (volume ratio 8: 2) mixed solution is settled to scale.
According to above-described method, the method validation reclaiming with mark-on the validity of 7 kinds of sulfanilamide (SN) in ionic liquid extract chicken, combine Ultra Performance Liquid Chromatography the sulfanilamide (SN) in chicken detected, and method is assessed.Result shows that the recovery of 3 interpolation levels (0.05,0.1,0.2mg/kg) is between 82%～103%, and relative standard deviation (RSD) is 5.3%～9.6%.With the comparison of conventional organic solvents extraction, there is nontoxic, safe feature, and solvent species and consumption little, extraction cost is low, and simple and efficient, the recovery is high, meets rules residue limits monitoring requirement.
Embodiment 1
Method of the present invention is used for extracting Wenchang chicken sulfanilamide (SN), and the step of the method is as follows:
The meat stirrer of commercially available Wenchang Chicken is made to homogenate state, get 2g and put into 10mL polypropylene tube, add the series standard solution of variable concentrations.
(1) preparation of extract
Water, 1-hexyl-3-methyl imidazolium tetrafluoroborate and glacial acetic acid are put into container in the ratio of 5: 1: 0.1, after stirring, water and ionic liquid are dissolved each other, become homogeneous phase, as the residual extract of chicken sulfonamides.
(2) high speed dispersion
The extract temperature that 6mL step (1) is obtained is heated to 30～40 ℃, join in the chicken of 2 grams of left and right, then use the high speed dispersion instrument of 4000～8000rpm (preferably 5000-7000rpm) to disperse 60～90s, after vortex after ultrasonic extraction 3min, centrifugal 5min (8000r/min), draws supernatant.
(3) extract layering
The Na that adds 1.08g left and right in the supernatant obtaining in step (2)
2hPO
412H
2o, 1mL1-hexyl-3-methyl imidazolium tetrafluoroborate, vortex static layering, after water layer and ionic liquid layering, draws water layer to remove, and again adds 1mL1-hexyl-3-methyl imidazolium tetrafluoroborate.
(4) again extract
The ionic liquid obtaining in step (3), add in the chicken having extracted, add 1mL water, 0.1mL glacial acetic acid, then use the high speed dispersion instrument of 4000～8000rpm (preferably 5000-7000rpm) to disperse 60～90s, ultrasonic extraction 3min after vortex, centrifugal 5min (8000r/min), inclines and supernatant.
(5) secondary clearing again
Supernatant adds 0.54gNa
2hPO
412H
2the centrifugal 2min of O, solion and water layer layering
(6) dilution constant volume
Draw this solion of 0.6mL to 2mL volumetric flask, with ultrapure water: glacial acetic acid (volume ratio 8: 2) mixed solution is settled to scale.
The different recovery and precision test data (n=5) of adding concentration in Wenchang Chicken
Embodiment 2
Method of the present invention is for extracting the sulfanilamide (SN) of three yellow chicken, and the step of the method is as follows:
The meat stirrer of commercially available Wenchang Chicken is made to homogenate state, get 2g and put into 10mL polypropylene tube, add the series standard solution of variable concentrations.
(1) preparation of extract
Water, 1-hexyl-3-methyl imidazolium tetrafluoroborate and glacial acetic acid are put into container in the ratio of 5: 1: 0.1, after stirring, water and ionic liquid are dissolved each other, become homogeneous phase, as the residual extract of chicken sulfonamides.
(2) high speed dispersion
The extract that 6mL step (1) is obtained is heated to 30～40 ℃ of temperature, join in the chicken of 2 grams of left and right, then use the high speed dispersion instrument of 4000～8000rpm (preferably 5000-7000rpm) to disperse 60～90s, after vortex after ultrasonic extraction 3min, centrifugal 5min (8000r/min), draws supernatant.
(3) extract layering
The Na that adds 1.08g left and right in the supernatant obtaining in step (2)
2hPO
412H
2o, 1mL1-hexyl-3-methyl imidazolium tetrafluoroborate, vortex static layering, after water layer separates with ionic liquid, draws water layer to remove, and again adds 1mL1-hexyl-3-methyl imidazolium tetrafluoroborate.
(4) again extract
The ionic liquid obtaining in step (3), add in the chicken having extracted, add 1mL water, 0.1mL glacial acetic acid, then use the high speed dispersion instrument of 4000～8000rpm (preferably 5000-7000rpm) to disperse 60～90s, ultrasonic extraction 3min after vortex, centrifugal 5min (8000r/min), inclines and supernatant.
(5) secondary clearing again
Supernatant adds the centrifugal 2min of 0.54gNa2HPO412H2O, solion and water layer layering
(6) dilution constant volume
Draw this solion of 0.6mL to 2mL volumetric flask, with ultrapure water: glacial acetic acid (volume ratio 8: 2) mixed solution is settled to scale.
The different recovery and the precision test number picks (n=5) of adding concentration in three yellow chickens
The above, be only the specific embodiment of the present invention, but protection scope of the present invention is not limited to this, and any variation of expecting without creative work or replacement, within all should being encompassed in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain that claims were limited.
Claims (9)
1. adopt the method for sulfa drug residue in ionic liquid extract chicken, it is characterized in that comprising the following steps:
(1) preparation of extract
Water, ionic liquid 1-hexyl-3-methyl imidazolium tetrafluoroborate and glacial acetic acid are put into container according to a certain percentage, after stirring, water and ionic liquid are dissolved each other, become homogeneous phase, as the residual extract of sulfonamides in chicken, the pH value of described extract is between 3-3.5;
(2) disperse
The extract temperature that step (1) is obtained is heated to 30～40 ℃, join in chicken, then use the high speed dispersion instrument of 4000～8000rpm (preferably 5000-7000rpm) to disperse 60～90s, after vortex after ultrasonic extraction 2-4min, centrifugal 4-6min (6000-10000r/min), draws supernatant;
(3) extract layering
In the supernatant obtaining in step (2), add appropriate Na
2hPO
412H
2o and 1-hexyl-3-methyl imidazolium tetrafluoroborate, vortex static layering, after water layer separates with ionic liquid, draws water layer to remove, and again adds 1-hexyl-3-methyl imidazolium tetrafluoroborate;
(4) again extract
The ionic liquid obtaining in step (3), add in the chicken having extracted, adding volume ratio is 8-12: 1 water and glacial acetic acid, then use the high speed dispersion instrument of 4000～8000rpm (preferably 5000-7000rpm) to disperse 60～90s, ultrasonic extraction 2-4min after vortex, centrifugal 4-6min (6000-10000r/min), inclines and supernatant;
(5) secondary clearing again
The resulting supernatant of step (4) adds Na
2hPO
412H
2the centrifugal 2min of O, solion and water layer layering;
(6) dilution constant volume
Draw the resulting solion of step (5) to volumetric flask, with ultrapure water: glacial acetic acid (volume ratio 6-10: 2) mixed solution is settled to scale.
2. method according to claim 1, is characterized in that, in described step (1) ratio of water, ionic liquid be 5: 1 or more than, with glacial acetic acid, regulate pH value in 3-3.5 left and right.
3. method according to claim 1, is characterized in that, described step (1) intermediate ion liquid is 1-hexyl-3-methyl imidazolium tetrafluoroborate.
4. method according to claim 1, is characterized in that, the material ratio of described step (1) intermediate ion liquid extraction liquid and chicken be 2: 1 or more than.
5. method according to claim 1, is characterized in that, the ionic liquid 1-hexyl-3-methyl imidazolium tetrafluoroborate, the Na that in described step (3), newly add
2hPO
412H
2o becomes phase condition with the best of former extract cumulative volume be 1-hexyl-3-methyl imidazolium tetrafluoroborate: Na
2hPO
412H
2o: cumulative volume 1: 1.08: 6.
6. method according to claim 1, it is characterized in that, in described step (4), extract is the supernatant of step (3) gained for the second time, and add ionic liquid 1-hexyl-3-methyl imidazolium tetrafluoroborate, water and glacial acetic acid, the ionic liquid newly adding with water, glacial acetic acid with volume of material than 1: 1: 0.1.
7. method according to claim 1, is characterized in that, in described step (5), it is 0.54: 3 that the Na2HPO412H2O newly adding becomes phase condition with the best of ionic liquid volume.
8. method according to claim 1, it is characterized in that, in described step (5), draw resulting this solion of step (5) to volumetric flask, with ultrapure water and glacial acetic acid mixed solution, be settled to scale, ultrapure water: the volume ratio of glacial acetic acid is 8: 2.
9. method according to claim 1, it is characterized in that sulfa drugs be selected from sulphathiazole (ST), sulfamerazine (SMR), ayerlucil (STZ), sulfadimidine (SDMD), cistosulfa (SCP), sulfamethoxine uh azoles (SMZ), sulfanilamide (SN) diformazan different uh in azoles (SIX) one or more or all.
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Application publication date: 20140122 |