CN101701943A - Method for measuring dimethyl fumarate in product by gas chromatography-mass spectrometry - Google Patents
Method for measuring dimethyl fumarate in product by gas chromatography-mass spectrometry Download PDFInfo
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Abstract
The invention discloses a method for measuring dimethyl fumarate in a product by gas chromatography-mass spectrometry. The method comprises the following steps of: pretreating a dimethyl fumarate product to be detected by using an ultrasonic extraction method; setting the temperature of a sample injection port of a gas chromatography-mass spectrometer to be 240-280 DEG C, a flow rate to be 0.8-1.5 ml/min and the temperature of a port to be 280-300 DEG C, and selecting a weak polar column for a chromatographic column; enabling a sample to enter the chromatographic column through the sample injection port, and carrying out temperature programming on the temperature of the chromatographic column to separate the components of the sample by the chromatographic column; and enabling the components separated by the chromatographic column to enter a mass spectrometric detection part through the port of the gas chromatography-mass spectrometer, wherein an electron impact ion source is adopted as the ion source of the mass spectrometric detection. The method for measuring the dimethyl fumarate in the product by the gas chromatography-mass spectrometry has low detection limit, good detection effect, little consumption of analysis solvent and low detection cost.
Description
Technical field
The present invention relates to the detection method of dimethyl fumarate in the product, particularly relate to the method that a kind of gas chromatography-mass spectrography is measured dimethyl fumarate in the product.
Background technology
Dimethyl fumarate (Dimethyl Fumarate, be called for short DMF) is the white powder crystalline solid, ester fragrance slightly, and it can effectively suppress and kill more than 30 kind of mould, saccharomycete and bacterium etc.Therefore, use application in industries such as industry, agricultural, food more, be used for the mildew-resistant of building materials, woodwork and plastic products as DMF, also be used for the anti-mould and anti-moth sterilization of food and catering trade, medicinal material, tobacco, textile, film, leather and goods thereof, paper, coating, dyestuff, bonding agent etc.
But, there are some researches show that DMF can enter human body through alimentary canal, respiratory tract and skin, cause allergicly, stimulate eyes, mucous membrane and the upper respiratory tract; DMF also will cause toxicity such as cellular oxidation damage and t cell proliferation; In addition, the DMF facile hydrolysis generates methyl alcohol, and long-term eating has very big spinoff to liver, kidney, and to human body, especially children's growth growth harm is very big, is inhibited in the food then and uses.In other industry it also there is strict qualification, announced the 4th edition correct copy of its global restrictive substance list RSL (Restricted Substances List) as U.S. clothes footwear association (AAFA), this part list has comprised the chemicals that national governments limit with the form of law or rules and other materials of comprising in product, wherein just comprised the up-to-date DMF of being forbidden by European Union materials such as (dimethyl fumarates), the final products that relate to mainly contain household textiles, clothes and footwear shoe etc.France also signed " containing the seat of dimethyl fumarate and issuing an order of footwear product listing about time-out " on Dec 4th, 2008 again; in 1 year time limit; time-out also has the seat of dimethyl fumarate and the import and the listing of footwear product; contain the seat and the footwear product of the appreciable dimethyl fumarate of content in all products or the packing, reclaim without exception.Therefore Enterprises for Export in China is the needs of reply international market, dimethyl fumarate content in the Related product of producing is carried out strictness measure, to guarantee the safety and sanitation of exported product.
At present, the existing method of liquid-phase chromatographic analysis dimethyl fumarate that adopts exists, though liquid phase chromatography analytical method has stronger compartment analysis ability, but, it can only be quantitative the mensuration product in each component concentration, for qualitative identification component fast and accurately certain limitation is arranged but, and use the liquid-phase chromatographic analysis solvent consumption big, it is higher to detect cost.
Summary of the invention
The present invention is directed to the above-mentioned deficiency of prior art, a kind of stronger compartment analysis ability that promptly has is provided, have qualitative identification ability fast and accurately again, and detect the method that the low gas chromatography-mass spectrography of cost is measured dimethyl fumarate in the product.
In order to solve the problems of the technologies described above, technical scheme of the present invention is: by the gas chromatograph-mass spectrometer (GCMS) of routine, carry out the detection method of the dimethyl fumarate in qualitative exactly, the quantitative product, comprise the steps:
(1) utilizes ultrasonic extraction to adopt organic solvent that the dimethyl fumarate sample that needs detect is extracted, then extract is filtered, finish the pre-treatment of dimethyl fumarate sample;
(2) with the dimethyl fumarate in the gas chromatograph-mass spectrometer (GCMS) test sample, the injector temperature of gas chromatograph-mass spectrometer (GCMS) is set at 240～280 ℃, flow rate of carrier gas is set at 0.8～1.5 ml/min, chromatographic column is selected low-pole column, and the interface temperature of gas chromatograph-mass spectrometer (GCMS) is set at 280～300 ℃;
(3) injection port of the gas chromatograph-mass spectrometer (GCMS) that will set by step (2) through the sample of step (1) pre-treatment enters in the chromatographic column, chromatogram column temperature is carried out temperature programme, since 60 ℃, speed with 5 ℃/min is warming up to 80～120 ℃, kept 0～10 minute, and then be warming up to 280～320 ℃ with 20～40 ℃/minute speed, and keeping 1～10 minute, each component of above-mentioned sample is separated by chromatographic column;
(4) interface of each component of the sample that is separated by chromatographic column of step (3) gained by gas chromatograph-mass spectrometer (GCMS) enters Mass Spectrometer Method and partly carries out Mass Spectrometer Method, the ion gun of described Mass Spectrometer Method adopts electron bombardment ionization source, the ion gun bombarding energy of Mass Spectrometer Method is 70eV, and ion source temperature is set at 230～250 ℃.
The organic solvent that ultrasonic extraction is used in the above-mentioned steps (1) is methylene chloride, methenyl choloride, and methyl alcohol, ethanol, acetone, any in the dehydration ethyl acetate etc., ethyl acetate more preferably dewaters.
The extraction time of ultrasonic extraction is preferably 30min in the above-mentioned steps (1), and the preferred temperature of ultrasonic extraction is 25 ℃, and the ultrasonic instrument frequency of operation is 40～60KHZ (KHz), is preferably 59KHZ.
The chromatographic column of low pole is preferably the low-pole column of 30m (length) * 0.32mm (internal diameter) * 0.25 μ m (thickness) in the above-mentioned steps (2).
Advantage of the present invention and beneficial effect are:
1. adopt the dimethyl fumarate of gas chromatography-mass spectrography technology GC-MS of the present invention (EI source) ionization in can qualitative exactly, quantitative different product, inexpensive, the safety of instrument, analytical approach accurately, fast, disturb for a short time, analyze fewly with solvent consumption, be suitable for standardization.
2. by selecting suitable chromatographic column, control suitable injector temperature, chromatogram column temperature and interface temperature, set suitable flow rate of carrier gas, can make dimethyl fumarate in the different product in mass ion source generation cracking and make each component of pyrolysis product carry out optimized analyzing and testing.
Description of drawings
The chromatogram of the dimethyl fumarate that Fig. 1 is detected for the embodiment of the invention 1, the ordinate in this chromatogram is represented the intensity at peak, and horizontal ordinate is represented retention time, and unit is minute.
The mass spectrogram of the dimethyl fumarate that Fig. 2 is detected for the embodiment of the invention 1, the ordinate in the mass spectrogram is represented the relative abundance of ion, and horizontal ordinate is represented the numerical value of ion mass-to-charge ratio.
The canonical plotting of the dimethyl fumarate that Fig. 3 is detected for the embodiment of the invention 1, the ordinate in this curve map is represented the response of gas chromatography peak area, and horizontal ordinate is represented the concentration of dimethyl fumarate.
Embodiment
Below in conjunction with accompanying drawing the present invention is described in further detail, but the present invention not only is confined to following examples.
Experiment condition: GC (7890)-MS (5975C) type gas chromatograph-mass spectrometer (GCMS) of using the production of Agilent company detects, and agents useful for same is chromatographically pure, the HP-5MS type chromatographic column that chromatographic column selects for use Agilent company to produce.The injector temperature of gas chromatograph-mass spectrometer (GCMS) is set at 240～280 ℃, and the interface temperature of gas chromatograph-mass spectrometer (GCMS) is set at 280～300 ℃; Carrier gas is high-purity helium, and flow velocity is 0.8～1.5 ml/min; The pattern of temperature programme is adopted in chromatogram column temperature control, since 60 ℃, is warming up to 100 ℃ with 5 ℃/minute speed, keeps 0～10 minute; And then be warming up to 280～320 ℃ with 20～40 ℃/minute speed, kept 1～10 minute; The ion gun of Mass Spectrometer Method adopts electron bombardment ionization source (EI source), and the ion gun bombarding energy is 70eV, and ion source temperature is set at 230～250 ℃; Sample size 1～2 microlitre.Computer system record chromatogram and mass spectrum figure with the peak area of the dimethyl fumarate response as object, carry out qualitative and quantitative analysis to this sample.It is as follows to use the specific embodiment that above-mentioned test condition does:
Precision takes by weighing dimethyl fumarate 5.0mg, behind an amount of dehydration acetic acid ethyl dissolution, is transferred in the volumetric flask of 250ml, and is settled to scale with dehydration ethyl acetate, shakes up, and leaves standstill, and promptly gets the DMF standard solution of 20 μ g/ml.The used solution of test job curve of DMF is by above 20 μ g/ml standard solution stepwise dilutions, be mixed with the serial solution of 0.1,0.2,0.5,1.0,2.0 μ g/ml respectively, carry out gas chromatograph-mass spectrometer (GCMS) GC-MS analyzing and testing by above-mentioned experiment condition, wherein the gas chromatograph-mass spectrometer (GCMS) injector temperature is set at 280 ℃, and interface temperature is set at 280 ℃; Carrier gas is high-purity helium, flow velocity 1 ml/min; The pattern of temperature programme is adopted in chromatogram column temperature control, since 60 ℃, is warming up to 100 ℃ with 5 ℃/minute speed; And then be warming up to 280 ℃ with 20 ℃/minute speed, kept 3 minutes; The ion gun of Mass Spectrometer Method adopts electron bombardment ionization source (EI source), and the ion gun bombarding energy is 70eV, and ion source temperature is set at 230 ℃; Sample size 1 microlitre.
The chromatogram of the dimethyl fumarate that Fig. 1 is detected for the embodiment of the invention 1, the ordinate in this chromatogram is represented the intensity at peak, and horizontal ordinate is represented retention time, and unit is minute; The full scan mass spectrogram of the dimethyl fumarate that Fig. 2 is detected for the embodiment of the invention 1, the ordinate in the mass spectrogram is represented the relative abundance of ion, and horizontal ordinate is represented the numerical value of ion mass-to-charge ratio; As qualitative ion, as quota ion,, sample is carried out qualitative and quantitative analysis with characteristic ion m/z 85,113 and 114 with the area at institute object appearing peak response as object with the strongest ion m/z 113 of kurtosis.Fig. 3 is the canonical plotting of the dimethyl fumarate that detected, and the ordinate in this curve map is represented the response of gas chromatography peak area, and horizontal ordinate is represented the concentration of dimethyl fumarate; As shown in Figure 3, the funtcional relationship of gained typical curve is y=(6E-05) x+0.0411, and its linearly dependent coefficient is R
2=0.9994, wherein y represents the concentration of dimethyl fumarate, and x represents the response of gas chromatography peak area, shows that this typical curve has the better linearity correlativity.The instrument detection limit that utilizes this gas chromatograph-mass spectrometer (GCMS) to detect reaches 0.1 μ g/ml, and quantitative limit can reach 0.3 μ g/ml.
Textile samples is cut into 4mm * 4mm (ISO 4044:1998) size with scissors, take by weighing about 0.5g, put into the head space bottle, (sample needs wetting by shake well to add 5ml dehydration acetic acid ethyl acetate extract, and be extracted the liquid submergence), 25 ℃ of ultrasonic extractions 30 minutes, the ultrasonic instrument frequency of operation is 59KHZ.Ultrasonic extraction liquid carries out test analysis with the extract after filtering with gas chromatograph-mass spectrometer (GCMS) with the membrane filtration of 0.45 μ m, and the gas chromatograph-mass spectrometer (GCMS) testing conditions is with embodiment 1, and external standard method is quantitative.Textile samples has been made 3 parallel sample, and test number is A, B, C, and analysis result sees Table 1, and to first parallel sample (test number A) replication 5 times, analysis result sees Table 2.As shown in Table 1, the relative standard deviation of parallel sample (RSD) is 1.42%; As shown in Table 2, the relative standard deviation of reperformance test is 1.64%.
The test content of dimethyl fumarate in this textile samples of table 1
Test repeatability in this textile samples of table 2
| Number of times numbering (μ g/g) | ??1 | ??2 | ??3 | ??4 | ??5 | Mean value | ??RSD％ |
| ??A | ??6.47 | ??6.64 | ??6.54 | ??6.35 | ??6.22 | ??6.44 | ??1.64 |
Embodiment 3
Standard solution among the embodiment 1 is joined in ready known negative (not containing target compound after tested) result's the test fluid, experimentize according to instrument analyzing detecting method among the embodiment 1.This sample is done 10 horizontal surveies average,, calculate the recovery of standard addition of this sample according to actual addition and measured result, test findings sees Table 3, as shown in Table 3, the recovery of standard addition of sample reaches between 90～110%, and the relative standard deviation of horizontal survey is 2.14%.
The recovery of standard addition of this sample of table 3
| Sequence number | Actual concentrations μ g/ml | Record concentration μ g/ml | Recovery of standard addition % |
| ??1 | ??1 | ??0.9256 | ??92.56 |
| ??2 | ??1 | ??0.9331 | ??93.31 |
| ??3 | ??1 | ??0.9384 | ??93.84 |
| ??4 | ??1 | ??0.9468 | ??94.68 |
| ??5 | ??1 | ??0.9604 | ??96.04 |
| ??6 | ??1 | ??0.9685 | ??96.85 |
| ??7 | ??1 | ??0.9701 | ??97.01 |
| Sequence number | Actual concentrations μ g/ml | Record concentration μ g/ml | Recovery of standard addition % |
| ??8 | ??1 | ??0.9739 | ??97.39 |
| ??9 | ??1 | ??0.9759 | ??97.59 |
| ??10 | ??1 | ??0.9859 | ??98.59 |
| Mean value | ??-- | ??0.9579 | ??95.79 |
| ??RSD％ | ??-- | ??2.14 | ??-- |
Claims (4)
1. a gas chromatography-mass spectrography is measured the method for dimethyl fumarate in the product, it is characterized in that: comprise the steps:
(1) utilizes ultrasonic extraction to adopt organic solvent that the dimethyl fumarate sample that needs detect is extracted, then extract is filtered, finish the pre-treatment of dimethyl fumarate sample;
(2) with the dimethyl fumarate in the gas chromatograph-mass spectrometer (GCMS) test sample, the injector temperature of gas chromatograph-mass spectrometer (GCMS) is set at 240～280 ℃, flow rate of carrier gas is set at 0.8～1.5 ml/min, chromatographic column is selected low-pole column, and the interface temperature of gas chromatograph-mass spectrometer (GCMS) is set at 280～300 ℃;
(3) injection port of the gas chromatograph-mass spectrometer (GCMS) that will set by step (2) through the sample of step (1) pre-treatment enters in the chromatographic column, chromatogram column temperature is carried out temperature programme, since 60 ℃, speed with 5 ℃/min is warming up to 80～120 ℃, kept 0～10 minute, and then be warming up to 280～320 ℃ with 20～40 ℃/minute speed, and keeping 1～10 minute, each component of above-mentioned sample is separated by chromatographic column;
(4) interface of each component of the sample that is separated by chromatographic column of step (3) gained by gas chromatograph-mass spectrometer (GCMS) enters Mass Spectrometer Method and partly carries out Mass Spectrometer Method, the ion gun of described Mass Spectrometer Method adopts electron bombardment ionization source, the ion gun bombarding energy of Mass Spectrometer Method is 70eV, and ion source temperature is set at 230～250 ℃.
2. gas chromatography-mass spectrography according to claim 1 is measured the method for dimethyl fumarate in the product, it is characterized in that: the organic solvent that ultrasonic extraction is used in the described step (1) is methylene chloride, methenyl choloride, methyl alcohol, ethanol, acetone, any in the dehydration ethyl acetate.
3. gas chromatography-mass spectrography according to claim 2 is measured the method for dimethyl fumarate in the product, it is characterized in that: the organic solvent that ultrasonic extraction is used in the described step (1) is dehydration ethyl acetate.
4. gas chromatography-mass spectrography according to claim 1 is measured the method for dimethyl fumarate in the product, it is characterized in that: the extraction time of ultrasonic extraction is 30min in the described step (1), the temperature of ultrasonic extraction is 25 ℃ of room temperatures, and the ultrasonic instrument frequency of operation is 40～60KHZ.
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| CN102230926A (en) * | 2011-06-22 | 2011-11-02 | 红云红河烟草(集团)有限责任公司 | Method for testing content of benzoic acid in tobacco additive |
| 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 |
| CN103926363A (en) * | 2014-04-24 | 2014-07-16 | 江苏中烟工业有限责任公司 | Gas chromatography/mass spectrometry (GC/MS) method for detecting dimethyl fumarate in food additive |
| CN104049046A (en) * | 2014-06-18 | 2014-09-17 | 南京麦思德餐饮管理有限公司 | Method for detecting dimethyl fumarate in body lotion |
| US8906420B2 (en) | 2009-01-09 | 2014-12-09 | Forward Pharma A/S | Pharmaceutical formulation comprising one or more fumaric acid esters in an erosion matrix |
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| CN111537625A (en) * | 2020-04-08 | 2020-08-14 | 宁波卫生职业技术学院 | Method for detecting dimethyl fumarate in medical textiles and leather |
| US11052062B2 (en) | 2004-10-08 | 2021-07-06 | Biogen Swiss Manufacturing Gmbh | Controlled release pharmaceutical compositions comprising a fumaric acid ester |
| CN114814049A (en) * | 2022-03-11 | 2022-07-29 | 陕西渭河煤化工集团有限责任公司 | Method for analyzing dimethyl oxalate |
| CN116046969A (en) * | 2023-01-07 | 2023-05-02 | 上海国齐检测技术有限公司 | Method for detecting fumaric acid diformate in soil |
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| US11052062B2 (en) | 2004-10-08 | 2021-07-06 | Biogen Swiss Manufacturing Gmbh | Controlled release pharmaceutical compositions comprising a fumaric acid ester |
| US11229619B2 (en) | 2004-10-08 | 2022-01-25 | Biogen Swiss Manufacturing Gmbh | Controlled release pharmaceutical compositions comprising a fumaric acid ester |
| US8906420B2 (en) | 2009-01-09 | 2014-12-09 | Forward Pharma A/S | Pharmaceutical formulation comprising one or more fumaric acid esters in an erosion matrix |
| US11173123B2 (en) | 2009-01-09 | 2021-11-16 | Biogen Swiss Manufacturing Gmbh | Pharmaceutical formulation comprising one or more fumaric acid esters in an erosion matrix |
| CN102230926A (en) * | 2011-06-22 | 2011-11-02 | 红云红河烟草(集团)有限责任公司 | Method for testing content of benzoic acid in tobacco additive |
| 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 |
| CN103713062B (en) * | 2013-12-31 | 2015-07-29 | 深圳出入境检验检疫局工业品检测技术中心 | The method for quick of Determination of Residual Organic Solvents is limited the use of in a kind of textile |
| CN103926363A (en) * | 2014-04-24 | 2014-07-16 | 江苏中烟工业有限责任公司 | Gas chromatography/mass spectrometry (GC/MS) method for detecting dimethyl fumarate in food additive |
| CN103926363B (en) * | 2014-04-24 | 2015-05-13 | 江苏中烟工业有限责任公司 | Gas chromatography/mass spectrometry (GC/MS) method for detecting dimethyl fumarate in food additive |
| CN104049046A (en) * | 2014-06-18 | 2014-09-17 | 南京麦思德餐饮管理有限公司 | Method for detecting dimethyl fumarate in body lotion |
| CN106610408A (en) * | 2015-10-22 | 2017-05-03 | 江苏维赛科技生物发展有限公司 | Method for detecting dimethyl fumarate content in textile product |
| CN105911182A (en) * | 2016-04-15 | 2016-08-31 | 海南省三亚质量技术监督技术所 | Pretreatment device for measuring dimethyl fumarate in textile and analysis method |
| CN111537625A (en) * | 2020-04-08 | 2020-08-14 | 宁波卫生职业技术学院 | Method for detecting dimethyl fumarate in medical textiles and leather |
| CN111537625B (en) * | 2020-04-08 | 2022-09-20 | 宁波卫生职业技术学院 | Method for detecting dimethyl fumarate in medical textiles and leather |
| CN114814049A (en) * | 2022-03-11 | 2022-07-29 | 陕西渭河煤化工集团有限责任公司 | Method for analyzing dimethyl oxalate |
| CN114814049B (en) * | 2022-03-11 | 2023-12-19 | 陕西渭河煤化工集团有限责任公司 | Analysis method of dimethyl oxalate |
| CN116046969A (en) * | 2023-01-07 | 2023-05-02 | 上海国齐检测技术有限公司 | Method for detecting fumaric acid diformate in soil |
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