CN111175370A - Direct detection method based on nonpolar solvent and ionic liquid - Google Patents
Direct detection method based on nonpolar solvent and ionic liquid Download PDFInfo
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Abstract
The invention discloses a direct detection method based on a nonpolar solvent and an ionic liquid, which comprises the following steps: (1) establishing a working curve by adopting an isotope internal standard method: I. preparing a series of samples containing isotope internal standards; II, assembling a normal-pressure sound velocity spray ionization device; cutting a sample to be detected, placing the sample on a glass plate sample table, starting an air source and a mass spectrometer, and setting mass spectrum parameters for detection; IV, quantifying by an isotope internal standard method; (2) and (3) detecting the actual sample by adopting the method of the step III. The invention applies the nonpolar solvent to the surface direct analysis, introduces the dicationic ionic liquid and improves the conductivity and the ionization efficiency of the liquid.
Description
Technical Field
The invention relates to the field of detection and detection, in particular to a simple open type method for directly detecting a perfluorinated compound by sound wave spray ionization based on the combination of nonpolar solvent desorption and dication ionic liquid static electricity.
Background
The mass spectrometry technology has the characteristics of high analysis speed, strong specificity and high sensitivity, and is favored in the field of analysis and detection all the time. The ion source is an important component of the mass spectrometer, the innovation of the ionization technology substantially expands the application range of the mass spectrometer and promotes the cross-over development of the mass spectrometer. The open type ionization technology is a new technology which directly carries out ionization mass spectrum detection on a sample without or only needing simple sample pretreatment and chromatographic separation. The open ionization technology has the characteristics of convenience and rapidness, desorption electrospray ionization is firstly proposed by professor Cooks of university of Puff 2004, and a plurality of open ionization technologies are developed. However, for the direct analysis of the solid sample surface, the problems of serious matrix interference, low desorption efficiency and the like still exist.
Disclosure of Invention
The invention aims to solve the technical problem of providing a direct detection and analysis method for perfluorinated compounds by simultaneously utilizing the combination of nonpolar solvent desorption and dicationic ionic liquid static electricity.
A direct detection method based on a nonpolar solvent and an ionic liquid comprises the following steps:
(1) establishing a working curve by adopting an isotope internal standard method:
I. preparing a series of samples containing isotope internal standards;
II. preparation of a cored borosilicate glass capillary tube to which was added 20. mu.l of a biscationic ionic liquid bis- (3-methyl-1-imidazole) butylidene difluoride [ C ] at a concentration of 20. mu. mol/l4(MIM)2]F2Assembling a normal-pressure sound velocity spray ionization device for the normal-pressure solution;
cutting a sample to be detected, placing the sample on a glass plate sample table, starting an air source and a mass spectrometer, and setting mass spectrum parameters for detection; the sample to be detected is a food packaging material;
IV, quantifying by an isotope internal standard method;
(2) and (3) detecting the actual sample by adopting the method of the step III.
The acoustic wave spray ionization device is the prior art, is not in the protective scope of the invention, the invention of the apparatus part is only to improve the angle of the sample platform, adopt the improved apparatus to develop a new detection method;
the invention relates to a direct detection method based on a non-polar solvent and an ionic liquid, wherein the method is used for detecting perfluorinated compounds.
The invention relates to a direct detection method based on a nonpolar solvent and an ionic liquid, wherein the parameters of a mass spectrometer are set as follows:
a positive ion detection mode;
the voltage of the inlet and the outlet of the transmission capillary is 2.0 kilovolt and 2.5 kilovolt respectively;
the temperature of the drying gas is 180 ℃;
the drying gas flow rate was 4 liters/min;
the data acquisition mode is as follows: multiple reaction monitoring mode.
The invention relates to a direct detection method based on a nonpolar solvent and an ionic liquid, wherein secondary mass spectrometry parameters are as follows:
the invention relates to a direct detection method based on a nonpolar solvent and an ionic liquid, wherein the preparation method of the glass capillary comprises the following steps: horizontally fixing a glass capillary blank on a pulling arm of a P-1000 type microelectrode drawing instrument, heating the middle of a capillary by a filament until glass is melted and broken, generating two spray capillaries with tips, wherein the inner diameters of the tips are 5 microns, and preparing the glass capillary.
The direct detection method based on the nonpolar solvent and the ionic liquid, disclosed by the invention, is characterized in that the incident angle of the glass capillary is 45 degrees, the glass sample stage is inclined by 30 degrees, the reflection angle with the glass capillary is 10 degrees, the distance between the tip of the glass capillary and the sample inlet of the mass spectrometer is 3 millimeters, and the distance between the tip of the glass capillary and the sample stage of the glass plate is 1 millimeter. The tip of the glass capillary tube extends out of the sleeve by a distance of 3 mm.
The direct detection method based on the nonpolar solvent and the ionic liquid is characterized in that a nitrogen cylinder is used for supplying nitrogen to one end of a three-way vertical joint, and the pressure of the nitrogen is set to be 6.2 bar.
The invention relates to a direct detection method based on a nonpolar solvent and an ionic liquid, wherein a sample to be detected is cut into a square with the square size of 1 multiplied by 1 square centimeter and is placed on a glass plate sample table.
The invention relates to a direct detection method based on a nonpolar solvent and an ionic liquid, wherein a preparation method of a series of samples containing isotope internal standards comprises the following steps:
cutting a blank hamburger packaging paper into squares of 1 multiplied by 1 square centimeter, preparing 7 series of mixed standard solutions of perfluorooctanoic acid, perfluorooctane sulfonic acid and isotope internal standards thereof by using methanol, wherein the concentrations of the perfluorooctanoic acid and the perfluorooctane sulfonic acid are respectively 1, 2, 5, 10, 20, 50 and 100 ng/ml, and the concentrations of the two isotope internal standards are both 20 ng/ml; and (3) taking 100 microliters of the mixed standard solution by using a liquid transfer gun, uniformly dropwise adding the mixed standard solution on the cut square hamburger packaging paper sheet, and naturally drying to obtain a hamburger packaging paper sample containing a certain amount of isotope internal standard and having the perfluorooctanoic acid and perfluorooctane sulfonic acid series standard concentration.
The sleeve at the front end of the acoustic wave spray ionization device is a polytetrafluoroethylene sleeve, and coaxial high-speed airflow is generated in a gap between the glass capillary and the polytetrafluoroethylene sleeve, so that a Venturi effect is generated, and solution in the glass capillary is taken out and atomized into small liquid drops. At the same time, the high velocity gas flow charges the droplets due to electrostatic imbalance.
The charged spray droplets bombard the surface of the sample to form a layer of liquid film on the surface, so as to extract the perfluorinated compounds in the sample. Meanwhile, the dicationic ionic liquid splashed by the air flow is electrostatically combined with the perfluorinated compounds in the form of anions and detected by a mass spectrometer in a positive ion mode.
The direct detection method based on the nonpolar solvent and the ionic liquid is different from the prior art in that:
the simple open type acoustic wave spray ionization technology can realize ionization of an object to be detected through coaxial high-flow-rate gas at the tip of the capillary tube because the simple open type acoustic wave spray ionization technology does not need high voltage or auxiliary heating and other processes, and is the simplest open type ionization technology. The desorption ionization technology based on the solvent has higher requirements on the spray solvent, water with higher polarity, methanol or a mixed solvent of the water and the methanol with a certain proportion of the two solvents are needed in most cases, the weak-polarity or non-polar solvent is difficult to realize the ionization process, and for the compound with lower polarity, the extraction capability of the polar solvent on the weak-polarity substances is poorer according to the similar and compatible principle. Based on the method, the nonpolar solvent is applied to the surface direct analysis for the first time, and the dicationic ionic liquid is introduced to improve the conductivity of the liquid, so that the ionization efficiency is improved. Meanwhile, the dicationic ionic liquid is used as an ionic addition reagent and can be combined with the extracted perfluorinated compounds through electrostatic interaction. Under the dual guarantee of the extraction efficiency and the ionization efficiency, the detection sensitivity of the method is improved, so that the method is used for rapidly screening and detecting the perfluorinated compounds in the sample. The electrostatic combination reaction formula of the dicationic ionic liquid, the perfluorooctanoic acid and the perfluorooctane sulfonic acid is as follows:
electrostatic combination reaction of dicationic ionic liquid and perfluorooctanoic acid and perfluorooctane sulfonic acid
The direct detection method based on the nonpolar solvent and the ionic liquid of the present invention is further described below with reference to the accompanying drawings.
Drawings
FIG. 1 is a full scan first order mass spectrogram of the present invention for detecting perfluorooctanoic acid and perfluorooctane sulfonic acid in a labeled hamburger wrapper sample; wherein the embedded part is a secondary mass spectrogram and a mass spectrum fragmentation schematic diagram of perfluorooctanoic acid and perfluorooctane sulfonic acid;
FIG. 2 is a graph showing the effect of different atomizing gas pressures on perfluorooctane sulfonate signal strength in the present invention;
FIG. 3 is a graph showing the effect of different concentrations of dicationic ionic liquids on the signal strength of perfluorooctanoic acid and perfluorooctane sulfonic acid in the present invention;
FIG. 4 is the contact angle test results for samples contemplated in the present invention;
FIG. 5 is a graph showing the effect of different spray solvents on the signal strength of perfluorooctanoic acid and perfluorooctane sulfonic acid in the present invention;
FIG. 6 is a full scan first order mass spectrum of perfluorooctanesulfonic acid in a hamburger wrapper sample when methanol (a) and n-hexane (b) are used as spray solvents, respectively, in accordance with the present invention;
FIG. 7 is a secondary mass spectrum of isotope internal standards of perfluorooctanoic acid (a) and perfluorooctane sulfonic acid (b) in the present invention and a working curve of perfluorooctanoic acid and perfluorooctane sulfonic acid in a hamburger wrapper sample established by an isotope internal standard method;
FIG. 8 shows the results of the experiments performed in the present invention to detect perfluorooctanoic acid in a popcorn barrel sample.
All English Chinese translations in the figures are as follows:
relative Absundance: relative abundance; m/z: mass to charge ratio; normalized Intensity: normalizing the intensity; intensity: strength; concentration: concentration; pressure: pressure; CA left: left contact angle; CAright: right contact angle; PFOA: perfluorooctanoic acid; PFOS: perfluorooctanesulfonic acid; MeCN: acetonitrile; MeOH: methanol; me2CO: acetone; IPA: isopropyl alcohol; THF: tetrahydrofuran; EtOAC: ethyl acetate; hx: n-hexane; spray Solvent: spraying a solvent; S/N: signal-to-noise ratio; A/IS: abundance ratio of the test substance to the isotope internal standard.
Detailed Description
Instrument and device
An internal thread through tee (Shiviaoke fluid systems science and technology Limited, Cat: SS-200-3TFT) and an external thread connection through joint (Shiviaoke fluid systems science and technology Limited, Cat: SS-100-1-2 BT); a P-1000 type microelectrode drawing instrument, a borosilicate glass capillary (outer diameter 1.5 mm, inner diameter 0.86 mm, length 10 cm) (product number of Sutter company in USA: BF 150-86-10); bruker amaZon ion trap mass spectrometer (Bruker Dalton, USA); Milli-Q ultra-pure water devices (Millipore, USA); pipette tips used for the experiments were all imported (Bio-Rad, USA).
The specific structure of the sonic spray ionization device refers to the invention patent with application number 201710541576.2, and the differences are as follows: in the invention, the sample platform is inclined by 30 degrees, and the sleeve at the front end of the device is a polytetrafluoroethylene sleeve.
II, materials and reagents
The standard substances of the perfluoro caprylic acid, the perfluoro octane sulfonic acid and the isotope internal standard thereof used in the experiment are all commercial highest purity standard samples, the standard substances of the perfluoro caprylic acid, the perfluoro octane sulfonic acid and the isotope internal standard thereof are prepared into 1000mg/L standard stock solution by using methanol, and the standard stock solution is diluted into standard working solution by using methanol according to the requirement when in use; all the solvents are in chromatographic grade; the dicationic ionic liquid bis- (3-methyl-1-imidazole) butylene difluoride is purchased from Shanghai Chengjie ionic liquid company Limited, and is prepared and diluted into standard working solution by using different solvents according to requirements when in use.
Third, detection method
Example 1
Working curve established by isotope internal standard method
1. Serial sample preparation with isotopic internal standard
Cutting a blank hamburger packaging paper into squares of 1 multiplied by 1 square centimeter, preparing a series of mixed standard solutions (7) of perfluorooctanoic acid, perfluorooctane sulfonic acid and isotope internal standards thereof by using methanol, wherein the concentrations of the perfluorooctanoic acid and the perfluorooctane sulfonic acid in the 7 standard solutions are respectively 1, 2, 5, 10, 20, 50 and 100 ng/ml; the concentrations of both isotopic internal standards were 20 ng/ml. And (3) taking 100 microliters of the mixed standard solution by using a liquid transfer gun, uniformly dropwise adding the mixed standard solution on the cut square hamburger packaging paper sheet, and naturally drying to obtain a hamburger packaging paper sample containing a certain amount of isotope internal standard and having a perfluorooctanoic acid and perfluorooctane sulfonic acid series standard concentration.
2. Building device
Horizontally fixing a glass capillary on a tension arm of a P-1000 type microelectrode drawing instrument, heating the middle of the capillary by a filament until glass is melted and broken, and generating two spray capillaries with tips, wherein the inner diameters of the tips are 5 microns; adding 20 microliter of dicationic ionic liquid bis- (3-methyl-1-imidazole) butylene difluoride [ C ] with the concentration of 20 micromoles/liter into a capillary tube by using a liquid-transferring gun4(MIM)2]F2A n-hexane solution of (1); the pointed capillary tube, to which the spray solution was added beforehand, was inserted into a 1/8 inch stainless steel three-way joint and a 1/16 adapter and screwed in place. The capillary tip was surrounded on one side by a teflon sleeve, and the tip extended beyond the sleeve by a distance of 3 mm. Adjusting the incident angle of the simple open type acoustic wave spray ionization device to be 45 degrees, wherein the distance between the tip of the capillary tube and the sample inlet of the mass spectrometer is 3 millimeters, the distance between the tip of the capillary tube and the sample platform of the glass plate is 1 millimeter, and the reflection angle between the tip of the capillary tube and the sample platform of the glass plate is 10 degrees; placing a marked sample to be detected on a glass plate sample table; a nitrogen cylinder was used to supply nitrogen to one end of the tee vertical joint, the pressure of the nitrogen was set at 6.2 bar.
3. Mass spectrometric detection
The mass spectrometer parameters were set as follows:
a positive ion detection mode;
the voltage of the inlet and the outlet of the transmission capillary is 2.0 kilovolt and 2.5 kilovolt respectively;
the temperature of the drying gas is 180 ℃;
the drying airflow rate was 4 liters/min;
the secondary mass spectrometry parameters of the multi-reaction monitoring mode are as follows:
4. results of the experiment
The primary mass spectra of perfluorooctanoic acid and perfluorooctane sulfonic acid in the labeled hamburger wrapper samples are shown in fig. 1, and the peaks of perfluorooctanoic acid and perfluorooctane sulfonic acid are detected at mass-to-charge ratios of 633.1 and 719.1 respectively. In FIG. 1, the embedded part is a secondary mass spectrum and a mass spectrum fragmentation schematic diagram of perfluorooctanoic acid and perfluorooctane sulfonic acid.
5. Optimization of atomization gas pressure
The simple open type acoustic wave spray ionization technology depends on coaxial high-speed atomizing gas to enable small liquid drops to be electrified due to unbalanced static electricity, so that the pressure of the atomizing gas has great influence on the ionization efficiency, and the experiment optimizes the pressure of the atomizing gas.
A series of nitrogen pressures (20, 30, 40, 50, 60, 70, 80, 90, 100, 110, 120psi) were experimentally set and the signal response intensity of the perfluorooctanesulfonic acid target conjugate was detected and recorded, and the results are shown in fig. 2. The results show that in the range of 20-90 psi, the signal response intensity increases with increasing atomization gas pressure, reaches a maximum value at 90psi, and after that, the target signal intensity decreases inversely with increasing atomization gas pressure, so 90psi is selected as the experimental nitrogen pressure.
6. Optimization of concentration of dicationic ionic liquids
The detection mode is changed into the positive ion mode due to the electrostatic combination of the dicationic ionic liquid and the perfluorinated compound in the anion form, so that the detection sensitivity is obviously improved, and the concentration of the dicationic ionic liquid has great influence on the detection result, so that the concentration of the dicationic ionic liquid is optimized in the experiment.
A series of concentrations (5, 10, 15, 20, 25, 30 and 35 micromoles/liter) of bis- (3-methyl-1-imidazole) butylene difluoride salt in a dicationic ionic liquid are set in the experiment, and the signal intensity of a target object is detected and recorded as shown in figure 3. The experimental result shows that the signal intensity of the target object increases along with the increase of the concentration of the dicationic ionic liquid within the range of 5-20 micromoles/liter and reaches the maximum value at 20 micromoles/liter, and thereafter, the signal intensity of the target object does not change obviously along with the further increase of the concentration of the dicationic ionic liquid, so that 20 micromoles/liter is selected as the experimental concentration of the dicationic ionic liquid.
7. Contact Angle testing of samples in accordance with the invention
The physicochemical properties of the sample surface had a large influence on the experimental results, and in order to further optimize the experimental conditions, the contact angles of hamburger wrappers and popcorn buckets with water were tested, and the test results are shown in fig. 4. It can be seen that the contact angles of the hamburger wrapper (a) and the popcorn barrel (b) are both greater than 90 degrees, i.e., the sample surface exhibits hydrophobic characteristics.
8. Optimization of spray solvents
In the simple open type spray ionization process, the spray droplets bombard the surface of a sample to form a layer of liquid film, and the liquid film extracts a target substance in the sample, so that the subsequent ionization is detected by a mass spectrometer, and the type of a solvent has an important influence on the extraction effect according to the similarity and intermiscibility principle, so that the experiment optimizes the type of the spray solvent.
Acetonitrile, methanol, acetone, isopropanol, tetrahydrofuran, ethyl acetate and n-hexane are set as spraying solvents in the experiment, and the signal intensity of the comparative target object is respectively detected and recorded under the same other conditions as shown in figure 5. The experimental result shows that the n-hexane has the best extraction effect on the target object due to the characteristics of strong hydrophobicity, low saturated vapor pressure and the like, so the n-hexane is selected as the experimental spray solvent.
In addition, compared with polar solvents such as methanol and the like, n-hexane as a non-polar solvent significantly reduces the matrix interference of surfactants such as alkylphenol ethoxylates and the like in the simple sonic spray ionization process, and the comparison result is shown in fig. 6.
9. Solvent surface tension test
To further explain the experimental results of the present invention, the surface tensions of the different solvents described above were tested at room temperature at 20 degrees celsius for a concentration of 20 micromoles/liter of dicationic ionic liquid, and the test results are shown in table 1. The test results show that overall, the smaller the surface tension, the stronger the detection signal intensity.
TABLE 1 surface tension of different solvents with 20. mu. mol/l concentration of dicationic ionic liquid
10. Quantitation by isotope internal standard method
In the experiment, working curves of the perfluorooctanoic acid and the perfluorooctane sulfonic acid are established by adopting an isotope internal standard method, a secondary mass spectrogram of the perfluorooctanoic acid (a), the perfluorooctane sulfonic acid (b) and the isotope internal standard thereof is shown in fig. 7, a working curve (c) of the method is obtained by drawing according to the abundance ratio concentration of the object to be detected and the isotope internal standard thereof, the result shows that the linearity is good in the range of 0.1-100 micrograms/square meter, and the quantitative limit, the detection limit and the recovery rate of the method are shown in table 2.
TABLE 2 detection limits, quantitation limits, and recovery of perfluorooctanoic acid and perfluorooctane sulfonic acid in hamburger wrappers
11. Actual sample detection
The method of the invention is adopted to detect the perfluorooctanoic acid and perfluorooctane sulfonic acid in 30 hamburger packing paper samples and popcorn barrel samples purchased by various ways such as fast food restaurant market, online shopping and the like, the detection result shows that the perfluorooctanoic acid is detected in a certain popcorn barrel sample, the quantitative result by adopting an isotope internal standard method is shown in figure 8, and the perfluorooctanoic acid content is 6.5 micrograms per square meter according to the established working curve.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (9)
1. A direct detection method based on a nonpolar solvent and an ionic liquid is characterized in that: the method comprises the following steps:
(1) establishing a working curve by adopting an isotope internal standard method:
I. preparing a series of samples containing isotope internal standards;
II. preparation of a cored borosilicate glass capillary tube to which was added 20. mu.l of a biscationic ionic liquid bis- (3-methyl-1-imidazole) butylidene difluoride [ C ] at a concentration of 20. mu. mol/l4(MIM)2]F2Assembling a normal-pressure sound velocity spray ionization device for the normal-pressure solution;
cutting a sample to be detected, placing the sample on a glass plate sample table, starting an air source and a mass spectrometer, and setting mass spectrum parameters for detection; the sample to be detected is a food packaging material;
IV, quantifying by an isotope internal standard method;
(2) and (3) detecting the actual sample by adopting the method of the step III.
2. The non-polar solvent and ionic liquid based direct detection method according to claim 1, characterized in that: the method is used to detect perfluorinated compounds.
3. The non-polar solvent and ionic liquid based direct detection method according to claim 2, characterized in that: the parameters of the mass spectrometer are set as follows:
a positive ion detection mode;
the voltage of the inlet and the outlet of the transmission capillary is 2.0 kilovolt and 2.5 kilovolt respectively;
the temperature of the drying gas is 180 ℃;
the drying gas flow rate was 4 liters/min;
the data acquisition mode is as follows: multiple reactions monitor the secondary mass spectral mode.
4. The non-polar solvent and ionic liquid based direct detection method according to claim 3, characterized in that:
the secondary mass spectrometry parameters are shown in the table above.
5. The non-polar solvent and ionic liquid based direct detection method according to claim 4, characterized in that: the preparation method of the glass capillary comprises the following steps: horizontally fixing a glass capillary blank on a pulling arm of a P-1000 type microelectrode drawing instrument, heating the middle of a capillary by a filament until glass is melted and broken, generating two spray capillaries with tips, wherein the inner diameters of the tips are 5 microns, and preparing the glass capillary.
6. The non-polar solvent and ionic liquid based direct detection method according to claim 5, characterized in that: the incident angle of the glass capillary is 45 degrees, the glass sample stage is inclined by 30 degrees, the reflection angle between the glass capillary is 10 degrees, the tip of the glass capillary and the distance between the sample inlets of the mass spectrometer is 3 millimeters, and the distance between the glass plate sample stages is 1 millimeter.
7. The non-polar solvent and ionic liquid based direct detection method according to claim 6, characterized in that: a nitrogen cylinder was used to supply nitrogen to one end of the tee vertical joint, the pressure of the nitrogen was set at 6.2 bar.
8. The non-polar solvent and ionic liquid based direct detection method according to claim 7, characterized in that: and cutting the sample to be detected into a square with the size of 1 multiplied by 1 square centimeter, and placing the square on a glass plate sample table.
9. The non-polar solvent and ionic liquid based direct detection method according to claim 8, characterized in that: the preparation method of a series of samples containing isotope internal standards comprises the following steps:
cutting a blank hamburger packaging paper into squares of 1 multiplied by 1 square centimeter, preparing 7 series of mixed standard solutions of perfluorooctanoic acid, perfluorooctane sulfonic acid and isotope internal standards thereof by using methanol, wherein the concentrations of the perfluorooctanoic acid and the perfluorooctane sulfonic acid are respectively 1, 2, 5, 10, 20, 50 and 100 ng/ml, and the concentrations of the two isotope internal standards are both 20 ng/ml; and (3) taking 100 microliters of the mixed standard solution by using a liquid transfer gun, uniformly dropwise adding the mixed standard solution on the cut square hamburger packaging paper sheet, and naturally drying to obtain a hamburger packaging paper sample containing a certain amount of isotope internal standard and having the perfluorooctanoic acid and perfluorooctane sulfonic acid series standard concentration.
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| 万萍: ""保健食品中违禁添加物的敞开式质谱分析"", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114200037A (en) * | 2021-11-11 | 2022-03-18 | 山东中科恒联生物基材料有限公司 | Method for detecting purity of ionic liquid in preparation of regenerated cellulose material |
| CN114200037B (en) * | 2021-11-11 | 2024-04-05 | 山东中科恒联生物基材料有限公司 | Method for detecting purity of ionic liquid in preparation of regenerated cellulose material |
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