CN112730662A - Method for simultaneously determining phthalate and adipate plasticizers in textile solid waste - Google Patents
Method for simultaneously determining phthalate and adipate plasticizers in textile solid waste Download PDFInfo
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Abstract
The invention discloses a method for simultaneously determining two plasticizers, namely phthalate and adipate, in textile solid waste, which simultaneously determines the two plasticizers, namely the phthalate and the adipate, in the textile solid waste by adopting a method of combining accelerated solvent extraction, solid-phase extraction purification, gas chromatography and mass spectrometry. The method specifically comprises the following steps of S1: standard solution preparation, S2: establishing chromatographic and mass spectrum conditions, S3: sample extraction, S4: sample purification, S5: and detecting a sample and the like. According to the method, phthalate and adipate components in the textile raw material solid waste are extracted by adopting normal hexane accelerated solvent extraction and solid phase extraction, and a method for simultaneously determining the plasticizer in 14 in the textile solid waste by using ASE-SPE-GC/MS is established. The method has the advantages of small interference, good reproducibility, accurate and reliable analysis result and small usage amount of chemical reagents, and is suitable for detecting phthalate and adipate components in textile solid waste.
Description
Technical Field
The invention relates to a method for simultaneously determining two plasticizers, namely phthalate and adipate in textile solid waste.
Technical Field
Phthalates (Phthalates) and Adipates (Adipates) are commonly used as plasticizers in textile elastic plastic parts and ornaments, are environmental hormone substances, can migrate out of carriers in use and enter human bodies through different approaches, interfere with normal regulation of nervous, immune and endocrine systems, and are extremely harmful to human bodies.
The textile raw material solid waste has wide sources and complex substances, and no related literature report is available at home and abroad on the quick screening technology aspect of Phthalates (Phthalates) and Adipates (adipats) in the textile raw material solid waste. The method has the advantages that trade fraud behaviors such as 'adulterated toxic textiles', 'smuggling textiles' and the like are forbidden, technical support is provided for national excellent in and out, textile raw material import regulation and control, international negotiation, risk analysis and the like, the requirement of 'detected, detected and accurate in' major customs work is met, meanwhile, waste textile raw materials which accord with safety, sanitation and environmental protection are comprehensively utilized according to the development concept of domestic circular economy and the principle of 'harmlessness, reduction and recycling' of wastes, and the important significance is achieved in establishing a technology for detecting toxic substances such as Phthalates (Phthalates) and Adipates (Adipates) in cross-border textile raw material solid wastes.
At present, the extraction technology of phthalate and adipate plasticizers mainly comprises solvent extraction methods such as Soxhlet extraction, ultrasonic extraction, Accelerated Solvent (ASE) extraction, solid phase micro-extraction and the like. ASE extraction is a new extraction technology in recent years, has the advantages of small organic solvent dosage, rapidness, small matrix influence, high recovery rate, good reproducibility and the like, and is widely applied to the fields of food, environment, agriculture, natural Chinese herbal medicine separation and extraction and the like. In order to detect phthalate and adipate plasticizers in the waste plant fiber textile raw materials more simply, conveniently, quickly, sensitively and accurately, the invention adopts an accelerated solvent extraction technology, and establishes a gas chromatography-mass spectrometry combined detection method after purification by a solid phase extraction column.
Disclosure of Invention
Aiming at the existing problems and achieving the purpose, the invention provides a method for simultaneously determining two plasticizers, namely phthalate and adipate, in textile solid waste, and establishes a detection method for simultaneously determining phthalate and adipate in the textile solid waste by using an Accelerated Solvent Extraction (ASE) -solid phase extraction purification (SPE) -gas chromatography-mass spectrometry (GC-MS) method. The specific technical scheme is as follows:
a method for simultaneously determining two plasticizers, namely phthalate and adipate, in textile solid waste is characterized in that the two plasticizers, namely the phthalate and the adipate, in the textile solid waste are simultaneously determined by adopting a method of accelerated solvent extraction-solid phase extraction purification-gas chromatography-mass spectrometry.
The method for simultaneously determining the phthalate and adipate plasticizers in the textile solid waste specifically comprises the following steps:
s1: preparing a standard solution: respectively preparing standard substances of phthalate and adipate plasticizers into standard stock solutions, mixing a proper amount of each standard stock solution according to needs to prepare a mixed standard solution with a proper mass concentration, and storing the mixed standard solution in a brown storage bottle at 4 ℃;
s2: establishing chromatographic and mass spectrum conditions: performing solid phase extraction on the mixed standard solution prepared in the step S1 through a proper chromatographic column, and performing mass spectrum detection and full scanning to obtain a total ion current chromatogram of the mixed standard solution;
s3: sample extraction: shearing a textile solid waste sample to be detected into fragments, weighing a certain amount, and transferring the fragments into a stainless steel extraction tank for accelerated solvent extraction;
s4: sample purification: and (4) transferring the extract liquid extracted by the accelerated solvent in the step S3 to a solid phase extraction column, eluting by eluent, and filtering by nitrogen for later use.
S5: sample detection: and (4) detecting the sample extract purified in the step S4 by establishing chromatographic and mass spectrum conditions in the step S2, and determining two plasticizers, namely phthalate and adipate, contained in the textile solid waste sample to be detected.
In a preferred embodiment, in step S1, the standard includes 9 phthalate plasticizers and 5 adipate plasticizers, which are respectively: diethyl phthalate (DEP), dipropyl phthalate (DPHP), diisobutyl phthalate (DIBP), dibutyl phthalate (DBP), dipentyl phthalate (DAP), di-2-methoxyethyl phthalate (DMEP), dihexyl phthalate (DHP), di-2-ethylhexyl phthalate (DEHP), diheptyl phthalate (DHP); diethyl adipate (DEA), diisobutyl adipate (DIBA), dibutyl adipate (DBA), dioctyl adipate (DNOP), bis (2-butoxyethyl) adipate (BXA); the purity of the product is more than 98%. The solvents used for preparing the standard stock solution and the standard solution are chromatographic pure n-hexane, and the concentration of the standard stock solution is 1000 ug/mL; the concentration of the mixed standard solution is 1, 2, 5, 10 and 20ug/mL series of concentrations.
Preferably, in step S2, the chromatographic column used for establishing the chromatographic and mass spectrometric conditions is an HP-inowax capillary chromatographic column, the specification of which is 30m × 0.25mm, and the film thickness of which is 0.25 μm; the chromatographic column passing conditions are as follows: injecting sample without pulse flow division, wherein the temperature of a sample injection port is 220 ℃, the carrier gas is high-purity helium with the purity of 99.999 percent, and the flow rate is 1.0 mL/min; the temperature-raising program of the chromatographic column is as follows: keeping the initial column temperature at 60 ℃ for 1 min; raising the temperature of the column to 220 ℃ at a temperature raising rate of 20 ℃/min, and keeping the temperature for 2 min; then raising the temperature of the column to 250 ℃ at the speed of 5 ℃/min, and keeping the temperature for 5 min; the whole program time is 24 min; the temperature of a chromatography-mass spectrometry interface is 250 ℃, an ionization source is an EI source, the ionization energy is 70eV, and 149u, 129u, 185u, 111u and 57u of detected ions are selected; the amount of sample was 1. mu.l.
In a preferred embodiment, in step S3, the size of the pieces cut from the textile solid waste sample is 5mm × 5 mm; the specific operation of accelerating solvent extraction is as follows: injecting an extraction solvent, heating for 3min under the extraction pressure of 10MPa at a certain extraction temperature, performing static extraction for a certain time, performing cyclic extraction for 2 times, flushing the extraction pool with the volume of 40%, purging with nitrogen for 100s after extraction is finished, collecting the extract in a 60mL collection bottle, transferring the extract to a 100mL heart-shaped bottle, concentrating in a 40 ℃ water bath until the extract is nearly dry, and purifying. The extraction solvent is acetone, dichloromethane, methanol, n-hexane or ethyl acetate, preferably n-hexane; the extraction temperature is 80-120 ℃, and preferably 100 ℃; the static extraction time is 4-10 min, preferably 5 min.
In a preferred embodiment, in step S4, the solid phase extraction column is a magnesium silicate Florisil solid phase extraction column, which is prepared by adding 2g anhydrous sodium sulfate into the column, sequentially activating with 5mL eluent, and then balancing with 5mL n-hexane; the accelerated solvent extraction is eluted for 2 times by using an eluent; the filtration was performed using an organic filter membrane with a gauge of 0.22 μm. The eluent is a mixture of n-hexane and dichloromethane, and the volume ratio of the mixture is 4: 1; the dosage of the eluent used for the accelerated solvent extraction is 10mL, and the dosage of the eluent used for each time is 5 mL.
The invention has the beneficial effects that:
the method adopts the Accelerated Solvent Extraction (ASE) -solid phase extraction purification (SPE) -gas chromatography-mass spectrometry combined (GC-MS) method to simultaneously determine the phthalate and the adipate existing in the textile raw material solid waste, and is not only quick, but also sensitive and accurate. Because of the double extraction and purification of Accelerated Solvent Extraction (ASE) and solid phase extraction and purification (SPE), the detection has small interference, good reproducibility and accurate and reliable analysis result. The usage amount of chemical reagents in the whole detection process is small, the phthalic acid ester and adipate components in the textile solid waste are detected, and meanwhile, the method is low in cost, generates few secondary pollutants, and has good practicability and environmental benefits.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail and fully below with reference to the examples.
Example 1
The method adopts a method of combining accelerated solvent extraction, solid phase extraction purification, gas chromatography and mass spectrometry to simultaneously determine the two plasticizers of phthalate and adipate in the textile solid waste. The method specifically comprises the following steps:
s1: preparing a standard solution: preparing standard substances of phthalate and adipate plasticizers into standard stock solutions respectively, mixing a proper amount of each standard stock solution according to needs to prepare a mixed standard solution with a proper mass concentration, and storing the mixed standard solution in a brown storage bottle at 4 ℃. The standards included 9 phthalate and 5 adipate plasticizers supplied by drehrenstontorfer, respectively: diethyl phthalate (DEP), dipropyl phthalate (DPHP), diisobutyl phthalate (DIBP), dibutyl phthalate (DBP), dipentyl phthalate (DAP), di-2-methoxyethyl phthalate (DMEP), dihexyl phthalate (DHP), di-2-ethylhexyl phthalate (DEHP), diheptyl phthalate (DHP); diethyl adipate (DEA), diisobutyl adipate (DIBA), dibutyl adipate (DBA), dioctyl adipate (DNOP), bis (2-butoxyethyl) adipate (BXA); the purity of the product is more than 98%. The solvents used for preparing the standard stock solution and the standard solution are chromatographically pure n-hexane, and the concentration of the standard stock solution is 1000 ug/mL; the concentration of the mixed standard solution is 1, 2, 5, 10 and 20ug/mL series of concentrations.
S2: establishing chromatographic and mass spectrum conditions: and (4) performing solid phase extraction on the mixed standard solution prepared in the step S1 through a proper chromatographic column, and performing mass spectrum detection and full scanning to obtain a total ion current chromatogram of the mixed standard solution. The chromatographic column used for solid phase extraction is an HP-INNOWAX capillary chromatographic column, the specification of the chromatographic column is 30m multiplied by 0.25mm, and the film thickness of the chromatographic column is 0.25 mu m; the conditions of the chromatographic column are as follows: injecting sample without pulse flow division, wherein the temperature of a sample injection port is 220 ℃, the carrier gas is high-purity helium with the purity of 99.999 percent, and the flow rate is 1.0 mL/min; the temperature rising procedure of the chromatographic column is as follows: keeping the initial column temperature at 60 ℃ for 1 min; the column was warmed to 220 ℃ at a rate of 20 ℃/min and held for 2 min; then raising the temperature of the column to 250 ℃ at the speed of 5 ℃/min, and keeping the temperature for 5 min; the total program time was 24 min. The temperature of a chromatography-mass spectrometry interface is 250 ℃, an ionization source is an EI source, the ionization energy is 70eV, and 149u, 129u, 185u, 111u and 57u of detected ions are selected; the amount of sample was 1. mu.l.
S3: sample extraction: and shearing the textile solid waste sample to be detected into fragments, weighing a certain amount, and transferring the fragments into a stainless steel extraction tank for accelerated solvent extraction. In this embodiment, the to-be-detected textile solid waste sample is a surface waste polyester fabric sample, and includes: sample 1: waste polyester fabric, off-white; sample 2: waste polyester cotton printed fabrics are alternated with blue and white; sample 3: the waste polyester-cotton blended fabric is light pink; sample 4: the waste nylon fabric is dark red; sample 5: waste nylon fabric, white; sample 6: waste spandex fabric, yellow. These samples were cut into pieces of about 5mm by 5mm and mixed well, and 1g was weighed and transferred to a 34mL stainless steel extraction cell for accelerated solvent extraction. Injecting acetone, dichloromethane, methanol, n-hexane or ethyl acetate as extraction solvent, preferably n-hexane; the extraction pressure is 10MPa, and the extraction temperature is 80-120 ℃, preferably 100 ℃, and the heating is carried out for 3 min; performing static extraction for 4-10 min, preferably for 5min, and performing cyclic extraction for 2 times; the flushing volume is 40 percent of the volume of the extraction pool, nitrogen is used for purging for 100s after extraction is finished, the extract is collected into a 60mL collection bottle, the extract is transferred into a 100mL heart-shaped bottle and is concentrated to be nearly dry in water bath at 40 ℃ for purification.
S4: sample purification: and (4) transferring the extract liquid extracted by the accelerated solvent in the step S3 to a solid phase extraction column, eluting by eluent, and filtering by nitrogen for later use. The solid phase extraction column is a magnesium silicate Florisil solid phase extraction column, 2g of anhydrous sodium sulfate is added into the magnesium silicate Florisil solid phase extraction column before use, 5mL of eluent (mixed solution of n-hexane and dichloromethane) is used for activation in sequence, 5mL of n-hexane is used for balancing, then a sample to be purified is transferred into the solid phase extraction column, and the eluent is used for elution for 2 times; then, 1mL of the solution was purged with nitrogen, and the solution was filtered through an organic filter of 0.22 μm in size. In this embodiment, the eluent is a mixture of n-hexane and dichloromethane, and the volume ratio of the mixture is 4: 1; the dosage of the eluent used for the accelerated solvent extraction is 10mL, namely 5mL of the eluent is used for each time.
S5: sample detection: and (4) detecting the sample extract purified in the step S4 by establishing chromatographic and mass spectrum conditions in the step S2, and determining two plasticizers, namely phthalate and adipate, contained in the textile solid waste sample to be detected.
Example 2
In this example, the method for simultaneously determining two types of plasticizers, i.e., phthalate and adipate, in the textile solid waste described in example 1 is subjected to correlation and detection limit verification, and the recovery rate and precision of the method are simultaneously verified.
In this embodiment, the correlation and detection limit verification method includes: preparing the standard stock solution of the standard substance into mixed standard working nights with the series concentrations of 1, 2, 5, 10 and 20ug/mL, measuring under the conditions of the chromatogram and the mass spectrum established in the step S2, and taking the concentration (X) and the peak area (Y) as standard curves to obtain a linear equation and a correlation coefficient; the recovery rate and precision of the method described in this example were verified as: and (3) carrying out standard addition recovery experiments on the target object at three levels of standard addition concentration of 2, 5 and 10mg/L, repeating the experiment 6 times at each standard addition level, and quantifying by an external standard method. As shown in table 1.
Table 1.14 correlation coefficient, linear equation, recovery and relative standard deviation (n ═ 6) limits for plasticizers
According to the detection method, the correlation coefficient r of the two plasticizers is larger than 0.99 within the linear range of 1-20 ug/mL, and the detection limit (S/N is 3) is 0.06-0.48 mg/kg. The limit of quantitation (S/N10) is 0.21-1.63 mg/kg. The recovery rate of 14 plasticizers in the range of standard concentration is 88.7-107.6%, and the Relative Standard Deviation (RSD) is 0.33-2.68%, so that the detection requirement of the plasticizers in the textile raw material solid waste can be met.
Example 3
In this example, 6 actual samples were tested for the presence of 14 components to be tested by the method described in example 1 for simultaneous determination of two types of plasticizers, phthalate and adipate, in textile solid waste. The results are shown in Table 2.
TABLE 2 measurement of plasticizers in the actual samples
From the results of the above table, plasticizer contamination was found in all 6 samples, with higher DEHP content in the printed fabric. However, when the detection was carried out by the national standard method (LOD of 40mg/kg), no detection could be carried out except for DEHP in sample 2.
The method adopts normal hexane accelerated solvent extraction combined with solid phase extraction to extract phthalate and adipate components in the textile raw material solid waste, and establishes a method for simultaneously determining 9 phthalate plasticizers and 5 adipate plasticizers in the textile solid waste by ASE-SPE-GC/MS. The relevant samples are detected, and the results show that: the method has the advantages of small interference, good reproducibility, accurate and reliable analysis result and small usage amount of chemical reagents, and is suitable for detecting phthalate and adipate components in textile solid waste.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. Furthermore, it should be understood that although the present specification describes embodiments, these embodiments are not intended to be included solely, and such description is for clarity only, and those skilled in the art will be able to make the present specification as a whole, and the embodiments of the present invention may be appropriately combined to form other embodiments understood by those skilled in the art.
Claims (10)
1. A method for simultaneously determining two types of plasticizers, namely phthalate and adipate in textile solid waste is characterized by comprising the following steps: the method adopts a method of combining accelerated solvent extraction, solid phase extraction purification, gas chromatography and mass spectrometry to simultaneously determine two plasticizers, i.e. phthalate and adipate, in the textile solid waste.
2. The method for simultaneously determining the two types of plasticizers, phthalate and adipate, in textile solid waste according to claim 1, characterized in that: the method specifically comprises the following steps:
s1: preparing a standard solution: respectively preparing standard substances of phthalate and adipate plasticizers into standard stock solutions, mixing a proper amount of each standard stock solution according to needs to prepare a mixed standard solution with a proper mass concentration, and storing the mixed standard solution in a brown storage bottle at 4 ℃;
s2: establishing chromatographic and mass spectrum conditions: performing solid phase extraction on the mixed standard solution prepared in the step S1 through a proper chromatographic column, and performing mass spectrum detection and full scanning to obtain a total ion current chromatogram of the mixed standard solution;
s3: sample extraction: shearing a textile solid waste sample to be detected into fragments, weighing a certain amount, and transferring the fragments into a stainless steel extraction tank for accelerated solvent extraction;
s4: sample purification: transferring the extract liquid extracted by the accelerating solvent in the step S3 to a solid phase extraction column, eluting by eluent, and filtering by nitrogen for later use;
s5: sample detection: and (4) detecting the sample extract purified in the step S4 by establishing chromatographic and mass spectrum conditions in the step S2, and determining two plasticizers, namely phthalate and adipate, contained in the textile solid waste sample to be detected.
3. The method for simultaneously determining the two types of plasticizers, phthalate and adipate, in textile solid waste according to claim 2, characterized in that: in step S1, the standard substance includes 9 phthalate plasticizers and 5 adipate plasticizers, which are respectively: diethyl phthalate, dipropyl phthalate, diisobutyl phthalate, dibutyl phthalate, dipentyl phthalate, di-2-methoxyethyl phthalate, dihexyl phthalate, di-2-ethylhexyl phthalate, diheptyl phthalate; diethyl adipate, diisobutyl adipate, dibutyl adipate, dioctyl adipate, di (2-butoxyethyl) adipate; the purity of the product is more than 98%.
4. The method for simultaneously determining the two types of plasticizers, phthalate and adipate, in textile solid waste according to claim 2, characterized in that: in step S1, the solvents used for preparing the standard stock solution and the standard solution are chromatographically pure n-hexane, and the concentration of the standard stock solution is 1000 ug/mL; the concentration of the mixed standard solution is 1, 2, 5, 10 and 20ug/mL series of concentrations.
5. The method for simultaneously determining the two types of plasticizers, phthalate and adipate, in textile solid waste according to claim 2, characterized in that: in step S2, the chromatographic column used for establishing the chromatographic and mass spectrometric conditions is HP-INNOWAX capillary chromatographic column, the specification of which is 30m × 0.25mm, and the film thickness of which is 0.25 μm; the chromatographic column passing conditions are as follows: injecting sample without pulse flow division, wherein the temperature of a sample injection port is 220 ℃, the carrier gas is high-purity helium with the purity of 99.999 percent, and the flow rate is 1.0 mL/min; the temperature rising procedure of the chromatographic column is as follows: keeping the initial column temperature at 60 ℃ for 1 min; raising the temperature of the column to 220 ℃ at a temperature raising rate of 20 ℃/min, and keeping the temperature for 2 min; then raising the temperature of the column to 250 ℃ at the speed of 5 ℃/min, and keeping the temperature for 5 min; the whole program time is 24 min; the temperature of a chromatography-mass spectrometry interface is 250 ℃, an ionization source is an EI source, the ionization energy is 70eV, and 149u, 129u, 185u, 111u and 57u of detected ions are selected; the amount of sample was 1. mu.l.
6. The method for simultaneously determining the two types of plasticizers, phthalate and adipate, in textile solid waste according to claim 2, characterized in that: in step S3, the specification of the pieces cut from the textile solid waste sample is 5mm × 5 mm; the specific operation of accelerating solvent extraction is as follows: injecting an extraction solvent, heating for 3min under the extraction pressure of 10MPa at a certain extraction temperature, performing static extraction for a certain time, performing cyclic extraction for 2 times, flushing the extraction pool with the volume of 40%, purging with nitrogen for 100s after extraction is finished, collecting the extract in a 60mL collection bottle, transferring the extract to a 100mL chicken heart bottle, concentrating in a 40 ℃ water bath until the extract is nearly dry, and purifying.
7. The method for simultaneously determining the two types of plasticizers, phthalate and adipate, in textile solid waste according to claim 6, characterized in that: the extraction solvent is acetone, dichloromethane, methanol, n-hexane or ethyl acetate; the extraction temperature is 80-120 ℃; the static extraction time is 4-10 min.
8. The method for simultaneously determining the two types of plasticizers, phthalate and adipate, in textile solid waste according to claim 7, characterized in that: the extraction solvent is n-hexane; the extraction temperature is 100 ℃; the static extraction time was 5 min.
9. The method for simultaneously determining the two types of plasticizers, phthalate and adipate, in textile solid waste according to claim 2, characterized in that: in step S4, the solid phase extraction column is a magnesium silicate Florisil solid phase extraction column, which is added with 2g anhydrous sodium sulfate, activated with 5mL of eluent in sequence, and then equilibrated with 5mL of n-hexane before use; the accelerated solvent extraction is eluted 2 times with an eluent; the filtration was performed using an organic filter membrane with a gauge of 0.22 μm.
10. The method for simultaneously determining the two types of plasticizers, phthalate and adipate, in the textile solid waste according to claim 8, characterized in that: the eluent is a mixture of n-hexane and dichloromethane, and the volume ratio of the mixture is 4: 1; the dosage of the eluent used for the accelerated solvent extraction is 10mL, and the dosage of the eluent used for each time is 5 mL.
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| CN112684042A (en) * | 2020-12-15 | 2021-04-20 | 湖南省地质测试研究院(国土资源部长沙矿产资源监督检测中心) | Method for simultaneously purifying various semi-volatile organic pollutants in soil analysis process |
| CN113917021A (en) * | 2021-10-08 | 2022-01-11 | 合肥国轩高科动力能源有限公司 | Method for testing phthalate substances in anode material or coating of lithium ion battery |
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| CN113917021A (en) * | 2021-10-08 | 2022-01-11 | 合肥国轩高科动力能源有限公司 | Method for testing phthalate substances in anode material or coating of lithium ion battery |
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