CN103983717B - A kind of method of decomposable asymmetric choice net carcinogenic aromatic amine dyestuff in Fast Measurement textile - Google Patents
A kind of method of decomposable asymmetric choice net carcinogenic aromatic amine dyestuff in Fast Measurement textile Download PDFInfo
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- CN103983717B CN103983717B CN201410217526.5A CN201410217526A CN103983717B CN 103983717 B CN103983717 B CN 103983717B CN 201410217526 A CN201410217526 A CN 201410217526A CN 103983717 B CN103983717 B CN 103983717B
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Abstract
The present invention relates to the method for decomposable asymmetric choice net carcinogenic aromatic amine dyestuff in a kind of Fast Measurement textile.The detection method that object is to provide should have that operation is easier, cost is lower.Technical scheme is: a kind of method of decomposable asymmetric choice net carcinogenic aromatic amine dyestuff in Fast Measurement textile, carry out according to the following steps: after 1) textile sample to be checked being shredded, put into tool plug reactor, then add the citrate buffer of preheating, jolting mixing is placed in water-bath and is incubated; 2) airtight jolting mixing after adding hydrogensulfite solution, then tool plug reactor is incubated in water-bath; Then in 2min, room temperature is cooled to; 3) in container, pipette a certain amount of sample liquid in tool plug centrifuge tube, add a certain amount of acetonitrile simultaneously and mix; 4) pipette a certain amount of hydrophobic solvent implantation step 3) mixed liquor in, jolting or vortex mixing after carry out centrifugal treating; 5) step 4 is got) centrifugal rear a certain amount of supernatant, upper machine carries out liquid phase or gas chromatographic analysis.
Description
Technical field
The present invention relates to a kind of method utilizing the solvent-induced extraction Fast Measurement textile decomposable asymmetric choice net carcinogenic aromatic amine dyestuff that is separated.
Background technology
Early stage research and clinical testing confirm, some azo dyes can be aromatic amine material human body or animal being had to potential carcinogenicity with different approaches deoxidization, degradation in the environment.Become one of most important quality control project in current textils and clothing trade both at home and abroad to the detection of decomposable asymmetric choice net carcinogenic aromatic amine dyestuff, routine testing sample size is very huge.
What adopts the mensuration of decomposable asymmetric choice net carcinogenic aromatic amine dyestuff in textile at present is traditional liquid-liquid extraction method, specifically extracts in organic solvent by the aromatic amine in aqueous phase, after concentrating constant volume, carries out instrumental analysis.Whole pretreatment process is complicated, and not only speed is slow, efficiency is lower, and the reappearance of testing result is not good; In addition extraction process needs to use disposable zeyssatite pillar and a large amount of organic solvent, and testing cost is high and unfriendly to environment, has a certain impact to the health of operating personnel.
Summary of the invention
The object of the invention is the deficiency overcoming above-mentioned background technology, provide a kind of and operate the detection method easier, cost is lower than current standard methods.
Technical scheme provided by the invention is: a kind of method of decomposable asymmetric choice net carcinogenic aromatic amine dyestuff in Fast Measurement textile, carries out according to the following steps:
1) put into tool plug reactor after textile sample to be checked for 1.0g being shredded (being usually less than 5mm × 5mm), then add the citrate buffer that 17mL has been preheating to 70 ± 2 DEG C, jolting mixing is placed in 70 ± 2 DEG C of water-baths and is incubated 30 ± 5min;
2) adding 3mL content is airtight jolting mixing after 200mg/mL hydrogensulfite solution, then tool plug reactor is incubated 30 ± 5min in 70 ± 2 DEG C of water-baths; Then in 2min, room temperature is cooled to;
3) in container, pipette a certain amount of sample liquid in tool plug centrifuge tube, add a certain amount of acetonitrile simultaneously and mix, the volume ratio of sample liquid and acetonitrile is 3.6-1.5: 1;
4) pipette a certain amount of hydrophobic solvent implantation step 3) mixed liquor in, jolting or vortex mixing after carry out centrifugal treating, the volume ratio of hydrophobic solvent and acetonitrile is 0.05-0.24: 1;
5) step 4 is got) centrifugal rear a certain amount of supernatant, upper machine carries out liquid phase or gas chromatographic analysis.
Step 3) in sample liquid volume be 1.2-1.9: 1 with the acetonitrile volume ratio that adds.
Step 4) in the volume ratio of the hydrophobic organic solvent volume that adds and acetonitrile be 0.07-0.14: 1.
Step 4) described hydrophobic solvent is methenyl choloride or chlorobenzene or toluene or 1-hexyl-3-methylimidazole hexafluorophosphate or 1-octyl group-3-methylimidazole hexafluorophosphate.
The present invention utilizes the hydrophobic solvent adding trace in the system of dissolving each other of acetonitrile and water can impel the principle of acetonitrile and water two-phase laminated flow, and adopt acetonitrile to be aromatic amine in extractant aqueous phase extracted, after two-phase laminated flow, organic phase can be directly used in stratographic analysis.Not only accuracy of detection can meet routine testing requirement, operation steps is simplified, and is only 1/2nd of existing detection method detection time, and inspection cost is reduced greatly (being reduced to less than 1/5th), and matrix interference is less, more friendly to environment; The routine check of this project of textile laboratory can be widely used in.
Accompanying drawing explanation
Fig. 1 is that embodiment 1 adopts the present invention and adopts national standard method to carry out the contrast colors spectrogram detected.
Embodiment
Detection method provided by the invention, mainly optimize pretreatment process, specifically adopt acetonitrile to be aromatic amine in extractant aqueous phase extracted, add after micro-hydrophobic solvent makes acetonitrile and water two-phase laminated flow, pipette a certain amount of upper organic phase and be directly used in stratographic analysis.
With existing Comparison between detecting methods, the advantage possessed is:
1, with the aromatic amine that acetonitrile replacement hydrophobic organic solvent is in extractant aqueous phase extracted, stratographic analysis can be directly used in, and single extraction efficiency is higher.
2, one is got and concentrated in treasury, and avoid rotary evaporation concentration process, operating process is more simple and quick, and cost is lower.
Embodiment 1
The detection of forbidding azo dyes in silk muffler
1, running program:
Get silk muffler sample that 1.0g shreds in 65mL tool plug reactor, add the citrate buffer that 17mL is preheating to (70 ± 2) DEG C, in DEG C water-bath that jolting is placed on (70 ± 2), be incubated 30min.Add airtight jolting immediately after 3.0mL200mg/mL hydrogensulfite solution, then reactor is incubated 30min in (70 ± 2) DEG C water-bath.Room temperature is cooled in 2min after taking out; Then pipette 3.0mL sample liquid in 15mL tool plug conical centrifuge tube, add 1.4mL acetonitrile, make to mix with the light jolting of have gentle hands, then pipette 120 μ L methenyl cholorides with micro syringe and inject acetonitrile/water mixed liquor.Centrifuge tube is mixed 1min on vortex mixer, then with the centrifugation 1min of 4000rpm.A certain amount of supernatant liquor is drawn in the sample bottle of band taper interpolation pipe, for liquid-phase chromatographic analysis with micro syringe.
2, liquid phase chromatogram condition
Instrument: Waters2695, is furnished with 2996 diode array detectors;
Chromatographic column:
c18 post (250mm × 4.6mm, 5 μm);
Mobile phase A: methyl alcohol, Mobile phase B: 0.575g ammonium dihydrogen phosphate (ADP)+0.7g sodium hydrogen phosphate, is dissolved in 1000mL ultrapure water;
Gradient: by 15% mobile phase A and 85% Mobile phase B time initial, then linearly change 80% mobile phase A and 20% Mobile phase B in 45min, keeps 5min.
Flow: 0.8mL/min;
Sample size: 20 μ L;
Column temperature: 40 DEG C.
Determined wavelength: 240nm, 280nm, 305nm.
3, testing result: detect biphenylamine, this method quantitative result is 475mg/kg, and the quantitative result adopting national standard method GB/T17592-2011 is 440mg/kg; Correlation ratio reaches more than 92%.
4, Fig. 1 is that sample adopts this method and adopts the contrast colors spectrogram of national standard method.
Be labeled as in figure:
1, biphenylamine
A: adopt national standard method GB/T17592-2011 to detect chromatogram; B: adopt the inventive method to detect chromatogram.
Embodiment 2
The detection of forbidding azo dyes in jeans
1, running program:
Get jeans fabric that 1.0g shreds in 65mL tool plug reactor, add the citrate buffer that 17mL is preheating to (70 ± 2) DEG C, firmly jolting is placed in (70 ± 2) DEG C water-bath and is incubated 30min.Adding 3.0mL concentration is airtight jolting immediately after 200mg/mL hydrogensulfite solution, then reactor is incubated 30min in (70 ± 2) DEG C water-bath.Room temperature is cooled to after taking-up; Then pipette 2.0mL sample liquid in 10mL tool plug conical centrifuge tube, add 1.0mL acetonitrile, make to mix with the light jolting of have gentle hands, then pipette 80 μ L methenyl cholorides with micro syringe and inject acetonitrile/water mixed liquor.Centrifuge tube is mixed 1min on vortex mixer, then with the centrifugation 1min of 4000rpm.Draw 1 μ L upper organic phase with micro syringe and be directly used in gas chromatography-mass spectrometry analysis.
2, instrumental conditions
Instrument: ThermoTraceGCUltra/DSQIIMSD gas chromatograph-mass spectrometer (GCMS);
Chromatographic column: DB-5MS (30m × 0.25mm × 0.25 μm);
Injector temperature: 250 DEG C;
Mass spectrometer interface temperature: 280 DEG C;
Column temperature: 60 DEG C (1min)
10 DEG C/min190 DEG C
3 DEG C/min235 DEG C
10 DEG C/min280 DEG C (5min)
Carrier gas and carrier gas flux: helium (purity >99.999%), 1.0mL/min;
Ion source temperature: 250 DEG C;
Scan mode: full scan;
Mass scan range: 35-350amu.
3, testing result: detect 3,3 '-dimethoxy benzidine 32mg/kg; As a comparison, adopt 3 of European Union method EN14362.1-2012, it is 30mg/kg that 3 '-dimethoxy benzidine detects result.
Embodiment 3
The detection of forbidding azo dyes in cotton knit fabrie
1, running program:
Get cotton swatch that 1.0g shreds in 65mL tool plug reactor, add the citrate buffer that 17mL is preheating to 70 ± 2 DEG C, firmly jolting is placed in (70 ± 2) DEG C water-bath and is incubated 30min; Add airtight jolting immediately after 3.0mL200mg/mL hydrogensulfite solution, then reactor is incubated 30min in (70 ± 2) DEG C water-bath; Room temperature is cooled in 2min after taking out.Then pipette 3.0mL sample liquid in 10mL tool plug conical centrifuge tube, add 1.4mL acetonitrile, make to mix with the light jolting of have gentle hands, then pipette 160 μ L1-hexyl-3-methylimidazole hexafluorophosphates with micro syringe and inject acetonitrile/water mixed liquor; Centrifuge tube is mixed 1min on vortex mixer, then with the centrifugation 1min of 4000rpm.Draw a certain amount of supernatant liquor in the sample bottle of band taper interpolation pipe with micro syringe, liquid chromatograph is analyzed.
2, liquid phase chromatogram condition
Instrument: Waters2695, is furnished with 2996 diode array detectors;
Chromatographic column:
c18 post (250mm × 4.6mm, 5 μm);
Mobile phase A: methyl alcohol, Mobile phase B: 0.01mol/L sodium acetate (pH=3.6);
Gradient: by 15% mobile phase A and 85% Mobile phase B time initial, then linearly change 80% mobile phase A and 20% Mobile phase B in 45min, keeps 5min.
Flow: 0.8mL/min;
Sample size: 20 μ L;
Column temperature: 40 DEG C.
Determined wavelength: 240nm, 280nm, 305nm.
3, testing result: detect 2-naphthylamines 18mg/kg; As a comparison, adopting the 2-naphthylamines of national standard method GB/T17592-2011 to detect result is 15mg/kg.
Embodiment 4
The detection of forbidding azo dyes in sheet
1, running program:
Get sheet sample that 1.0g shreds in 65mL tool plug reactor, add the citrate buffer that 17mL is preheating to (70 ± 2) DEG C, firmly jolting is placed in (70 ± 2) DEG C water-bath and is incubated 30min.Add airtight jolting immediately after 3.0mL200mg/mL hydrogensulfite solution, then reactor is incubated 30min in (70 ± 2) DEG C water-bath.Room temperature is cooled to after taking-up; Then pipette 3.0mL sample liquid in 10mL tool plug conical centrifuge tube, add 1.4mL acetonitrile, make to mix with the light jolting of have gentle hands, then pipette 100 μ L chlorobenzenes with micro syringe and inject acetonitrile/water mixed liquor.Centrifuge tube is mixed 1min on vortex mixer, then with the centrifugation 1min of 4000rpm.Draw 1 μ L upper organic phase with micro syringe and be directly used in gas chromatography-mass spectrometry analysis.
2, instrumental conditions
Instrument: ThermoTraceGCUltra/DSQIIMSD gas chromatograph-mass spectrometer (GCMS);
Chromatographic column: DB-5MS (30m × 0.25mm × 0.25 μm);
Injector temperature: 250 DEG C;
Mass spectrometer interface temperature: 280 DEG C;
Column temperature: 60 DEG C (1min)
10 DEG C/min190 DEG C
3 DEG C/min235 DEG C
10 DEG C/min280 DEG C (5min)
Carrier gas and carrier gas flux: helium (purity >99.999%), 1.0mL/min;
Ion source temperature: 250 DEG C;
Scan mode: full scan;
Mass scan range: 35-350amu.
3, testing result: detect biphenylamine 89mg/kg; As a comparison, adopting the biphenylamine of national standard method GB/T17592-2011 to detect result is 78mg/kg.
Claims (1)
1. the method for decomposable asymmetric choice net carcinogenic aromatic amine dyestuff in Fast Measurement textile, carry out according to the following steps:
1) put into tool plug reactor after textile sample to be checked for 1.0g being shredded, then add the citrate buffer that 17mL has been preheating to 70 ± 2 DEG C, jolting is placed in 70 ± 2 DEG C of water-baths and is incubated 30 ± 5min;
2) add airtight jolting immediately after 3mL200mg/mL hydrogensulfite solution, then reactor is incubated 30 ± 5min in 70 ± 2 DEG C of water-baths; Then room temperature is cooled to;
3) in container, pipette a certain amount of sample liquid in tool plug centrifuge tube, add a certain amount of acetonitrile simultaneously and mix, the volume ratio of sample liquid and acetonitrile is 1.2-1.9: 1;
4) pipette a certain amount of hydrophobic solvent implantation step 3) mixed liquor in, jolting or vortex mixing after carry out centrifugal treating, the volume ratio of hydrophobic solvent and acetonitrile is 0.07-0.14: 1;
5) step 4 is got) centrifugal rear a certain amount of supernatant, upper machine carries out liquid phase or gas chromatographic analysis;
Described hydrophobic solvent is methenyl choloride or chlorobenzene or toluene or 1-hexyl-3-methylimidazole hexafluorophosphate or 1-octyl group-3-methylimidazole hexafluorophosphate.
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Cited By (2)
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| CN106770833A (en) * | 2017-01-10 | 2017-05-31 | 深圳市北测检测技术有限公司 | A kind of method of decomposable asymmetric choice net aromatic amine dyestuff in measure textile |
| CN109085273A (en) * | 2018-07-10 | 2018-12-25 | 福建省产品质量检验研究院 | The high performance liquid chromatography while method for separating and detecting of 12 kinds of direct dyess of cosmetics |
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| CN106153780A (en) * | 2016-07-29 | 2016-11-23 | 杭州吉华江东化工有限公司 | A kind of detect the method for organochlorine residue in azo dye product |
| CN110261523A (en) * | 2019-05-28 | 2019-09-20 | 广东产品质量监督检验研究院 | Testing methods of banned azo dyes and appraisement system construction method in crocodile leathercraft |
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| CN106770833A (en) * | 2017-01-10 | 2017-05-31 | 深圳市北测检测技术有限公司 | A kind of method of decomposable asymmetric choice net aromatic amine dyestuff in measure textile |
| CN109085273A (en) * | 2018-07-10 | 2018-12-25 | 福建省产品质量检验研究院 | The high performance liquid chromatography while method for separating and detecting of 12 kinds of direct dyess of cosmetics |
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