CN114441653A - Gas chromatography-mass spectrometry detection method for measuring content of tetraethylene glycol dimethyl ether - Google Patents
Gas chromatography-mass spectrometry detection method for measuring content of tetraethylene glycol dimethyl ether Download PDFInfo
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- CN114441653A CN114441653A CN202011199758.4A CN202011199758A CN114441653A CN 114441653 A CN114441653 A CN 114441653A CN 202011199758 A CN202011199758 A CN 202011199758A CN 114441653 A CN114441653 A CN 114441653A
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- ZUHZGEOKBKGPSW-UHFFFAOYSA-N tetraglyme Chemical compound COCCOCCOCCOCCOC ZUHZGEOKBKGPSW-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000001514 detection method Methods 0.000 title claims abstract description 13
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 title claims abstract description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 36
- 150000002500 ions Chemical class 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000012634 fragment Substances 0.000 claims abstract description 8
- 239000012528 membrane Substances 0.000 claims abstract description 6
- 239000011521 glass Substances 0.000 claims abstract description 5
- 238000002137 ultrasound extraction Methods 0.000 claims abstract description 5
- 238000010812 external standard method Methods 0.000 claims abstract description 4
- 239000006228 supernatant Substances 0.000 claims abstract description 4
- 239000000523 sample Substances 0.000 claims description 54
- 239000000126 substance Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 10
- 238000002347 injection Methods 0.000 claims description 8
- 239000007924 injection Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 230000005540 biological transmission Effects 0.000 claims description 5
- 238000004817 gas chromatography Methods 0.000 claims description 5
- 230000000630 rising effect Effects 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000004677 Nylon Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 229920001778 nylon Polymers 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 238000004949 mass spectrometry Methods 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 239000012488 sample solution Substances 0.000 claims description 2
- 230000014759 maintenance of location Effects 0.000 abstract description 4
- 238000004458 analytical method Methods 0.000 abstract description 2
- 239000012459 cleaning agent Substances 0.000 description 5
- 238000001819 mass spectrum Methods 0.000 description 5
- 239000011550 stock solution Substances 0.000 description 5
- 238000005303 weighing Methods 0.000 description 4
- 238000007865 diluting Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000003599 detergent Substances 0.000 description 2
- 238000013467 fragmentation Methods 0.000 description 2
- 238000006062 fragmentation reaction Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000004451 qualitative analysis Methods 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 206010074268 Reproductive toxicity Diseases 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 239000008199 coating composition Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- -1 coatings Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000007696 reproductive toxicity Effects 0.000 description 1
- 231100000372 reproductive toxicity Toxicity 0.000 description 1
- 238000002098 selective ion monitoring Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000012224 working solution Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/047—Standards external
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
- G01N2030/146—Preparation by elimination of some components using membranes
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
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Abstract
The invention belongs to the field of analysis and detection, and relates to a gas chromatography-mass spectrometry detection method for measuring the content of tetraethylene glycol dimethyl ether, which comprises the following steps: taking a proper amount of sample in a glass centrifuge tube, performing ultrasonic extraction by methanol, centrifuging, taking supernatant, passing through a membrane, performing gas chromatography-mass spectrometry, determining retention time and fragment ions, and quantifying by an external standard method. The method is simple and rapid, has accurate qualitative and quantitative determination, and meets the daily detection requirement.
Description
Technical Field
The invention belongs to the field of analysis and detection, and relates to a gas chromatography-mass spectrometry detection method for measuring the content of tetraethylene glycol dimethyl ether.
Background
The tetraglyme is a colorless transparent liquid, is soluble in water, can be mixed and dissolved with other hydrocarbon solvents, and has a structural formula shown in formula 1. The tetraethylene glycol dimethyl ether is widely applied to the fields of flue gas cleaning systems, paints, coatings, adhesives, printing ink, lithium batteries and the like, such as solvents for producing paint adhesives, coagulants in coating formulations, adsorption type liquid-gas detergents, paint removers and degumming agents, lubricants in automobile air-conditioning compressors and the like. Considering the reproductive toxicity of tetraglyme, the european chemical administration (ECHA) proposed to list tetraglyme as a candidate for the 24 th batch of REACH high interest material.
At present, no method for detecting the content of tetraethylene glycol dimethyl ether in related industrial products or chemicals exists, and in order to accurately determine the content of the tetraethylene glycol dimethyl ether, the invention establishes a gas chromatography-mass spectrometry method for quickly and accurately detecting the content of the tetraethylene glycol dimethyl ether, so that manufacturers and operators of related products in import and export trade can know the content of the tetraethylene glycol dimethyl ether in the products in time, and meanwhile, the harm of the substance to human can be better prevented.
Disclosure of Invention
The invention aims to provide a gas chromatography-mass spectrometry detection method for measuring the content of tetraglyme.
In order to realize the purpose of the invention, the technical scheme of the invention is as follows:
(1) sample preparation:
1) uniformly mixing liquid, milky and other non-solid samples to obtain a sample;
2) and (3) taking 20-50 g of a solid sample, cutting the solid sample into pieces about 1cm multiplied by 1cm, carrying out coarse powder by adopting an efficient cutting pulverizer, carrying out fine powder under the condition of liquid nitrogen, passing the fine powder through a standard sieve of 80 meshes, and taking the sieved powder as a sample.
(2) Extraction and determination:
putting 1-2 g of sample into a 50mL glass centrifuge tube, adding 20mL of methanol, mixing uniformly in a vortex manner, performing ultrasonic extraction for 30min, cooling to room temperature, diluting to 25mL with methanol at constant volume, mixing uniformly, centrifuging at 4000r/min for 5min, filtering supernate with a 0.22-micron nylon filter membrane, and analyzing the filtrate by gas chromatography-mass spectrometry;
(3) the instrument conditions were as follows:
1) gas chromatography conditions
Adopting chromatographic column Agilent DB-WAX (30m multiplied by 0.25mm multiplied by 0.25 mu m), constant current, and column flow rate of 1.2 mL/min; the sample injection volume is 1 mu L; split-flow sample injection is carried out, and the split-flow ratio is 5: 1; the temperature of a sample inlet is 220 ℃; the temperature raising procedure is that the initial temperature is 40 ℃, the temperature is kept for 2min, the temperature is raised to 60 ℃ at 8 ℃/min, then the temperature is raised to 240 ℃ at 15 ℃/min, and the temperature is kept for 6 min; or chromatographic column Agilent DB-5ms (30m × 0.25mm × 0.25 μm), constant flow, and column flow rate of 1.2 mL/min; the sample injection volume is 1 mu L; split-flow sample injection is carried out, and the split-flow ratio is 5: 1; the sample inlet temperature is 280 ℃; the temperature raising program is that the initial temperature is 50 ℃, the temperature is raised to 220 ℃ at the speed of 20 ℃/min, the temperature is kept for 10min, and then the temperature is raised to 290 ℃ at the speed of 100 ℃/min;
2) conditions of Mass Spectrometry
EI ionization mode, wherein ionization energy is 70eV, ion source temperature is 230 ℃, transmission line temperature is 240 ℃, solvent delay time is 3min, ion mode scanning is selected, and characteristic fragment ions are qualitative and quantitative; selected ion monitoring is shown in table 1:
table 1 ion monitoring (.' quantitative fragmentation)
(4) And (3) calculating: and (3) calculating by an external standard method, and calculating the content of the target object in the sample according to the following formula:
in the above formula:
x is the content of the substance to be detected in milligrams per kilogram (mg/kg) in the sample;
m-sample mass in grams (g);
v-volume to volume in milliliters (mL);
Csample (A)-target concentration in sample solution in micrograms per milliliter (μ g/mL);
f is dilution multiple;
note: the calculation results retain three significant digits.
Most preferably, the quantitative ion of the tetraethylene glycol dimethyl ether is m/z59, and the qualitative ion is m/z103, 45.
Has the advantages that: the invention establishes a gas chromatography-mass spectrometry detection method for measuring the content of tetraethylene glycol dimethyl ether. Aiming at the characteristics mainly related to the sample, a methanol ultrasonic extraction method is adopted to ensure that the target object in the sample is fully extracted, the supernatant is taken after centrifugation and is filtered by a membrane, and the supernatant is detected on a computer. The optimal gas chromatography conditions ensure better separation effect, retention time and symmetrical peak shape, and the optimal mass spectrum conditions and fragment ion selection ensure stable baseline and accurate qualitative and quantitative determination of the target. The method is simple to operate, and avoids the loss of the target object in the extraction process caused by fussy pretreatment. The method is simple and rapid, has accurate quantification and qualification, has higher recovery rate and precision, and can meet the detection requirements of each matrix sample.
Drawings
The invention is further explained in detail by taking a cleaning agent as a sample and combining the attached drawings and a specific embodiment:
FIG. 1 total ion current chromatogram of tetraglyme standard substance
FIG. 2 histogram of mass spectrum fragment of tetraglyme standard
FIG. 3 standard curve of tetraglyme
FIG. 4 total ion current chromatogram of cleaning agent sample
FIG. 5 chromatogram of total ion current of cleaning agent sample with standard
Detailed Description
The present invention is further illustrated by the following examples, but is not limited thereto in any way, and any modification or improvement based on the present invention is within the scope of the present invention.
Example one
Weighing a tetraethylene glycol dimethyl ether standard substance with the purity of 99 percent in a volumetric flask, and dissolving and diluting the tetraethylene glycol dimethyl ether standard substance into a standard stock solution of 1000 mu g/mL by using methanol; absorbing a certain volume of liquid from the standard stock solution to prepare a standard solution with the concentration of 10 mug/mL, and performing qualitative and quantitative analysis by using a gas chromatography-mass spectrometer; chromatographic conditions are as follows: adopting chromatographic column Agilent DB-WAX (30m multiplied by 0.25mm multiplied by 0.25 mu m), constant flow, column flow of 1.2mL/min, sample introduction volume of 1 mu L, split flow sample introduction, and split flow ratio of 5: 1; the temperature of a sample inlet is 220 ℃, the temperature rising procedure is that the initial temperature is 40 ℃, the temperature is kept for 2min, the temperature is raised to 60 ℃ at the speed of 8 ℃/min, then the temperature is raised to 240 ℃ at the speed of 15 ℃/min, and the temperature is kept for 6 min; EI ionization mode, ionization energy 70eV, ion source temperature 230 ℃, transmission line temperature 240 ℃, solvent delay time 3min, ion mode scanning selected, and fragment ions monitored: m/z59 (quantitative ion), 103 (qualitative ion), 45 (qualitative ion). The total ion current result of the tetraglyme standard substance is shown in figure 1, and the mass spectrum fragmentation result is shown in figure 2.
Example two
Determination of content of tetraethylene glycol dimethyl ether in cleaning agent sample
(1) Standard curve
Weighing a tetraethylene glycol dimethyl ether standard substance with the purity of 99 percent in a volumetric flask, and dissolving and diluting the standard substance into a standard stock solution with the methanol concentration of 1000 mu g/mL; sucking a certain volume of liquid from the standard stock solution to prepare a series of standard working solutions with the concentrations of 0.5, 1.0, 2.0, 5.0, 10.0 and 20.0 mug/mL, and performing qualitative and quantitative analysis by using a gas chromatography-mass spectrometer, wherein a standard curve is shown in FIG. 3;
(2) chromatographic conditions
Gas chromatography conditions: adopting chromatographic column Agilent DB-WAX (30m multiplied by 0.25mm multiplied by 0.25 mu m), constant flow, column flow of 1.2mL/min, sample introduction volume of 1 mu L, split flow sample introduction, and split flow ratio of 5: 1; the temperature of a sample inlet is 220 ℃, the temperature rising procedure is that the initial temperature is 40 ℃, the temperature is kept for 2min, the temperature is raised to 60 ℃ at the speed of 8 ℃/min, then the temperature is raised to 240 ℃ at the speed of 15 ℃/min, and the temperature is kept for 6 min;
mass spectrum conditions: EI ionization mode, ionization energy 70eV, ion source temperature 230 ℃, transmission line temperature 240 ℃, solvent delay time 3min, ion mode scanning selected, and fragment ions monitored: m/z59 (quantitative ion), 103 (qualitative ion), 45 (qualitative ion);
(3) sample assay
50mL of the cleaning agent is taken and mixed evenly. Respectively weighing 1.00g of sample, adding 20mL of methanol into a 50mL glass centrifuge tube, uniformly mixing in a vortex manner, carrying out ultrasonic extraction for 30min, cooling an extracting solution to room temperature, then carrying out constant volume to 25mL by using methanol, uniformly mixing, centrifuging at 4000r/min for 5min, taking supernate, filtering by using a 0.22 mu m nylon filter membrane, and analyzing a filtrate by using a gas chromatography-mass spectrometer;
(4) qualitative and quantitative results
And no chromatographic peak consistent with the target monitoring ion retention time appears in the retention time window, which indicates that the content of the tetraglyme in the sample is not detected by the calculation of an external standard method, and the result is shown in figure 4.
EXAMPLE III
And taking a detergent sample with a negative detection result of the tetraglyme in the second example. Weighing 1.00g of sample, putting the sample into a 50mL glass centrifuge tube, adding 0.1mL of 1000 mu g/mL of tetraethylene glycol dimethyl ether standard stock solution, standing for 30min, adding 20mL of methanol, whirlpool mixing, ultrasonic extracting for 30min, cooling the extracting solution to room temperature, metering the volume to 25mL by using methanol, mixing uniformly, centrifuging for 5min at 4000r/min, taking supernate, filtering the supernate by using a 0.22 mu m nylon filter membrane, and analyzing the filtrate by using a gas chromatography-mass spectrometer; gas chromatography conditions: adopting a chromatographic column Agilent DB-WAX (30m multiplied by 0.25mm multiplied by 0.25 mu m), constant flow, column flow rate of 1.2mL/min, sample introduction volume of 1 mu L, split flow and sample introduction, and split flow ratio of 5: 1; the temperature of a sample inlet is 220 ℃, the temperature rising procedure is that the initial temperature is 40 ℃, the temperature is kept for 2min, the temperature is raised to 60 ℃ at the speed of 8 ℃/min, then the temperature is raised to 240 ℃ at the speed of 15 ℃/min, and the temperature is kept for 6 min; mass spectrum conditions: EI ionization mode, ionization energy 70eV, ion source temperature 230 ℃, transmission line temperature 240 ℃, solvent delay time 3min, ion mode scanning selected, and fragment ions monitored: the results of m/z59 (quantitative ion), 103 (qualitative ion) and 45 (qualitative ion) are shown in FIG. 5.
The above examples are provided for illustrative purposes only and are not intended to limit the scope of the present invention; it should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention, which fall within the scope of the invention; therefore, all equivalent changes and modifications that are within the scope of the claims of the present invention should be covered by the claims of the present invention.
Claims (2)
1. A gas chromatography-mass spectrometry detection method for measuring the content of tetraethylene glycol dimethyl ether is characterized in that,
(1) sample preparation:
1) uniformly mixing liquid, milky and other non-solid samples to obtain a sample;
2) and (3) taking 20-50 g of a solid sample, cutting the solid sample into pieces about 1cm multiplied by 1cm, carrying out coarse powder by adopting an efficient cutting pulverizer, carrying out fine powder under the condition of liquid nitrogen, passing the fine powder through a standard sieve of 80 meshes, and taking the sieved powder as a sample.
(2) Extraction and determination:
putting 1-2 g of sample into a 50mL glass centrifuge tube, adding 20mL of methanol, mixing uniformly in a vortex manner, carrying out ultrasonic extraction for 30min, cooling to room temperature, fixing the volume to 25mL by using methanol, mixing uniformly, centrifuging at 4000r/min for 5min, taking supernatant, filtering by using a 0.22 mu m nylon filter membrane, and analyzing the filtrate by using a gas chromatography-mass spectrometer;
(3) the instrument conditions were as follows:
1) gas chromatography conditions
Adopting chromatographic column Agilent DB-WAX (30m multiplied by 0.25mm multiplied by 0.25 mu m), constant current, and column flow rate of 1.2 mL/min; the sample injection volume is 1 mu L; split-flow sample injection is carried out, and the split-flow ratio is 5: 1; the temperature of a sample inlet is 220 ℃; temperature rising procedure: the initial temperature is 40 ℃, the temperature is kept for 2min, the temperature is raised to 60 ℃ at the speed of 8 ℃/min, then the temperature is raised to 240 ℃ at the speed of 15 ℃/min, and the temperature is kept for 6 min; or chromatographic column Agilent DB-5ms (30m × 0.25mm × 0.25 μm), constant flow, and column flow rate of 1.2 mL/min; the sample injection volume is 1 mu L; split-flow sample injection is carried out, and the split-flow ratio is 5: 1; the sample inlet temperature is 280 ℃; temperature rising procedure: the initial temperature is 50 ℃, the temperature is increased to 220 ℃ at the speed of 20 ℃/min, the temperature is kept for 10min, and then the temperature is increased to 290 ℃ at the speed of 100 ℃/min;
2) conditions of Mass Spectrometry
EI ionization mode, wherein ionization energy is 70eV, ion source temperature is 230 ℃, transmission line temperature is 240 ℃, solvent delay time is 3min, ion mode scanning is selected, and characteristic fragment ions are qualitative and quantitative;
(4) and (3) calculating: calculating by an external standard method, and calculating the content of the target object in the sample according to the following formula:
in the above formula:
x is the content of the substance to be detected in milligrams per kilogram (mg/kg) in the sample;
m-sample mass in grams (g);
v-volume volumetric volume in milliliters (mL);
Csample (A)-target concentration in sample solution in micrograms per milliliter (μ g/mL);
f is dilution multiple;
note: the calculation results retain three significant digits.
2. The gas chromatography-mass spectrometry detection method for measuring the content of tetraglyme of claim 1, wherein the quantitative ion of tetraglyme is m/z59 and the qualitative ions are m/z103 and 45.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07223974A (en) * | 1994-02-14 | 1995-08-22 | Kansai Tec:Kk | Treatment of polychlorinated aromatic compound |
| CN102998387A (en) * | 2012-11-23 | 2013-03-27 | 江苏中烟工业有限责任公司 | Method for determining ethylene glycol monomethyl ether, glycol ether, ethylene glycol ether acetate, glycol and diglycol in food wrap paper |
| CN103675132A (en) * | 2013-12-05 | 2014-03-26 | 陈东 | Method for detecting amino acids, saccharides and organic acids in cells through gas chromatography-mass spectrometry |
| CN103713062A (en) * | 2013-12-31 | 2014-04-09 | 深圳出入境检验检疫局工业品检测技术中心 | Method for fast detection of residual amount of restricted organic solvents in textile |
| CN108037231A (en) * | 2017-12-13 | 2018-05-15 | 中国检验检疫科学研究院 | Method that is a kind of while measuring 8 kinds of gylcol ether compounds in cosmetics |
| CN110672768A (en) * | 2019-10-24 | 2020-01-10 | 无限极（中国）有限公司 | Method for determining diethoxydiol in oral care product |
-
2020
- 2020-10-30 CN CN202011199758.4A patent/CN114441653A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07223974A (en) * | 1994-02-14 | 1995-08-22 | Kansai Tec:Kk | Treatment of polychlorinated aromatic compound |
| CN102998387A (en) * | 2012-11-23 | 2013-03-27 | 江苏中烟工业有限责任公司 | Method for determining ethylene glycol monomethyl ether, glycol ether, ethylene glycol ether acetate, glycol and diglycol in food wrap paper |
| CN103675132A (en) * | 2013-12-05 | 2014-03-26 | 陈东 | Method for detecting amino acids, saccharides and organic acids in cells through gas chromatography-mass spectrometry |
| CN103713062A (en) * | 2013-12-31 | 2014-04-09 | 深圳出入境检验检疫局工业品检测技术中心 | Method for fast detection of residual amount of restricted organic solvents in textile |
| CN108037231A (en) * | 2017-12-13 | 2018-05-15 | 中国检验检疫科学研究院 | Method that is a kind of while measuring 8 kinds of gylcol ether compounds in cosmetics |
| CN110672768A (en) * | 2019-10-24 | 2020-01-10 | 无限极（中国）有限公司 | Method for determining diethoxydiol in oral care product |
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