CN103399111B - Method for selectively measuring ethylene glycol monoethyl ether acetate in dry food packaging paper based on headspace-gas chromatography/mass spectrometry - Google Patents
Method for selectively measuring ethylene glycol monoethyl ether acetate in dry food packaging paper based on headspace-gas chromatography/mass spectrometry Download PDFInfo
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Abstract
The invention discloses a method for selectively measuring ethylene glycol monoethyl ether acetate in dry food packaging paper based on headspace-gas chromatography/mass spectrometry, and belongs to the technical field of detection for physicochemical indexes of packaging materials. The method comprises the following steps of: performing headspace treatment on the dry food packaging paper for 30 minutes at 140 DEG C, taking naphthalene as an interior label, detecting in a gas chromatography/mass spectrometry selective ion scanning mode and by virtue of an HP-VOC (HP-volatile organic compounds) gas chromatographic column, and quantifying by an internal standard method. According to the method, a quantitative detection limit on the target object, namely, ethylene glycol monoethyl ether acetate, is 0.031 mug/mL, the adding standard recovery rate is 87.5-96.0%, and the relative standard deviation is 1.97-3.91%. According to the measurement method, the cockamamie steps of solvent extraction are avoided, the detection sensitivity is greatly improved via selective ion detection quantifying; moreover, the method is few in interference factors, simple to operate, high in recovery rate, and good in repeatability.
Description
Technical field
The invention belongs to wrappage physical and chemical index detection technique field, be specifically related to a kind of method based on ethyl cellosolve acetate in head space-gas chromatography mass spectrometry selective determination dry food wrapping paper (mainly comprising fast food wrapping paper, candy paper using, wheaten food paper using etc.).
Background technology
Ethyl cellosolve acetate, also known as 2-ethoxy ethyl acetate, acetic cellosolve, ethyl cellosolve acetate, is colourless liquid, has the smell of faint similar fragrant fat, is slightly soluble in water, miscible in most organic solvents such as aromatic hydrocarbons.Ethyl cellosolve acetate is often used as cellulose nitrate, resin, the solvent of grease and paint stripper, is widely used in high-grade paint, has good intermiscibility and pigment-dispersing.On July 1st, 1998, State Bureau of Environmental Protection, economic and commercial committee, Ministry of Foreign Trade and Economic Cooperation, Ministry of Public Security's dispatch ([1998] No. 089) provide " National Hazard refuse register ", the wherein material such as bag ethylene glycol ethyl ether and ester class thereof.Calendar year 2001 health ministry No. 255 file regulations: indoor coating prohibits the use the materials such as ethyl cellosolve acetate.In June, 2011, ethyl cellosolve acetate is listed in the 5th batch of SVHC inventory by REACH regulation, is classified as 2 class reproductive system toxicants.
Dry food wrapping paper is important component part indispensable in packaging for foodstuff, and its security is the very important aspect of food overall security, and the source that packaging material for food security controls, be raw materials for production at all.In view of ethyl cellosolve acetate very likely as raw materials for production, can be used in the production run of paper.Therefore explore one ethyl cellosolve acetate phenol detection method fast and accurately, control effectively to the ethyl cellosolve acetate in dry food wrapping paper, ensureing the safety in utilization of dry food wrapping paper, is very urgent and necessary.
At present paint and coating sample are mainly concentrated on to the detection of ethyl cellosolve acetate, adopt vapor-phase chromatography more.The people such as Guo Dengfeng establish the gas chromatography analysis method of ethyl cellosolve acetate content in automobile coating, adopt PEG-20M wide bore capillary column, and automobile coating sample, after n-hexane extraction, leaves standstill after oscillation extraction 20min, get supernatant and detect.The recovery of ethyl cellosolve acetate is 98.5% ~ 101.4%, and relative standard deviation is 0.65%.The people such as Nie Weian select dimethyl polysiloxane column capillary tube separating column AT.SE-30, with dimethyl carbonate-butyl acetate (volume ratio 2:1) mixed solvent for extraction solvent, inner mark method ration, establishes the gas chromatography analysis method of dimethylbenzene and ethyl cellosolve acetate content in Simultaneously test paint solvent.Use the method, the recovery of ethyl cellosolve acetate is 101.4% ~ 102.5%, and relative standard deviation is not more than 2.0%.The people such as Chen Huiming use HP-5 chromatographic column, adopt sherwood oil-acetone (volume ratio 1:1) mixed extractant solvent coating sample, centrifugal after ultrasonic extraction 15min, add anhydrous sodium sulfate dehydration, the ethyl cellosolve acetate in coating and butyl glycol ether acetic acid esters is detected after organic membrane filtration, wherein the detection of ethyl cellosolve acetate is limited to 0.1ng, and the recovery is 91.20%-102.58%, and relative standard deviation is 0.69%-2.1%.The people such as Zhu Huaiyuan adopt 5 kinds of objectionable impuritiess such as ethyl cellosolve acetate in GC/MS method Rapid Simultaneous Determination food wrapper.Sample uses methyl alcohol to be solvent, and after ultrasonic extraction, filtering, adopt GC/MS Select ion monitor method to analyze, detecting of ethyl cellosolve acetate is limited to 1.60mg/kg, and recovery of standard addition is 89.57% ~ 104.29%.
Above detection method all employs a certain amount of organic solvent to the process of sample, and some solvents can produce certain harm to human body, environment; Meanwhile, some analytical approach result insufficient sensitivity are desirable, and for the sample of matrix complexity, qualitative confirmation result is not ideal enough.
Summary of the invention
Goal of the invention: for the deficiencies in the prior art, the object of this invention is to provide the method for a kind of employing based on ethyl cellosolve acetate in head space-gas chromatography mass spectrometry selective determination dry food wrapping paper, fast, accurately can detect the content of ethyl cellosolve acetate in dry food wrapping paper, have measurement result accurately, measure the features such as interference is few.
Technical scheme: in order to realize foregoing invention object, the technical solution used in the present invention is as follows:
Based on a method for ethyl cellosolve acetate in head space-gas chromatography mass spectrometry selective determination dry food wrapping paper, comprise the steps:
(1) get standard substance ethyl cellosolve acetate, be made into Standard Stock solutions with glyceryl triacetate;
(2) get internal standard compound matter naphthalene, be made into the glyceryl triacetate solution of naphthalene with glyceryl triacetate, for subsequent use as host solvents;
(3) Standard Stock solutions many parts is got, add the host solvents of different amount respectively, and the standard working solution of a series of variable concentrations gradient is obtained with glyceryl triacetate constant volume, after respectively standard working solution being carried out head space balance, after transmission line sample introduction, carry out GC/MS-SIM detection; With the concentration (μ g/mL) of ethyl cellosolve acetate and interior mark naphthalene than X for horizontal ordinate, with the peak area ratio Y of ethyl cellosolve acetate and interior mark naphthalene for ordinate, carry out linear regression, draw the typical curve of object, calculate the regression equation of object typical curve;
(4) dry food wrapping paper is cut out be placed in ml headspace bottle, add host solvents, rapid sealing, carry out head space process, ready to balance enters gas chromatograph-mass spectrometer through transmission line after sampling well, carries out GC/MS-SIM and detects analysis, the ratio of the peak area of the ethyl cellosolve acetate obtained with the peak area of interior mark naphthalene is substituted in backhaul equation respectively, can be calculated the corresponding content of ethyl cellosolve acetate in dry food packaging.
In step (1), the concentration of Standard Stock solutions is 5 ~ 15 μ g/mL.
In step (2), the concentration of host solvents is 0.3 ~ 0.7 μ g/mL.
In step (3), the standard working solution of a series of variable concentrations gradient is 5 parts, and in solution, the concentration of ethyl cellosolve acetate is respectively 0.05,0.1,0.5,1 and 5 μ g/mL, and the concentration of interior mark naphthalene is 0.5 μ g/mL.
In step (3) and step (4), the analysis condition of head space is identical, is: Sample equilibration temperature: 140 DEG C; Sample loop temperature: 150 DEG C; Transmission line temperature: 160 DEG C; Sample equilibration time is 30min; Sample bottle moulding pressure: 15psi; Nebulizer gas pressure: 20psi; Pressing time: 0.2min; The qi of chong channel ascending adversely time: 0.2min; Sample loop equilibration time: 0.05min; Sample injection time: 0.5min.
In step (3) and step (4), the analysis condition of GC/MS is identical, is:
GC conditions: adopt HP-VOC(60m × 0.32mm × 1.80 μm) capillary chromatographic column, carrier gas is helium, flow is 1.5 mL/min, sample size is 1 μ L, and injector temperature is 220 DEG C, adopts Splitless injecting samples mode, heating schedule is initial temperature is 50 DEG C, keep 5min, be increased to 200 DEG C with the speed of 8 DEG C/min, keep 5min;
Mass spectrophotometry condition: transmission line temperature is 240 DEG C, ionization mode is EI, and ion source temperature is 230 DEG C;
Quadrupole rod temperature is 150 DEG C, the solvent delay time is 15min, and scan mode is selectivity ion scan pattern (SIM), and wherein the Selective ion mode of object ethyl cellosolve acetate is 128,102, the Selective ion mode of interior mark naphthalene is 43,59,72, is 50ms to the monitoring time of each ion.
In step (3), the regression equation Y=0.1875X-0.000442 of ethyl cellosolve acetate, related coefficient 0.9999, the range of linearity 0.05 ~ 5 μ g/mL and detection limit 0.031 μ g/mL.
In step (4), be 80cm often cutting out area
21 ~ 5mL host solvents is added in testing sample.
Beneficial effect: compared with prior art, employing of the present invention is based on the method for ethyl cellosolve acetate in head space-gas chromatography mass spectrometry selective determination dry food wrapping paper, can extract from dry food wrapping paper and obtain ethyl cellosolve acetate, thus utilize GC/MS method carry out qualitative confirmation to it and quantitatively detect, there is following remarkable advantage:
(1) for the mensuration of ethyl cellosolve acetate, prior art is mainly with quantified by external standard method, and for the complex background system that different paper brings, the quantitative measurement of object has interference unavoidably; And the inventive method utilizes inner mark method ration, without constant volume, and the error brought by pre-treating method reappearance and instrument precision problem can be reduced;
(2) method pre-treatment of the present invention is simple, avoids the laborious steps of solvent process, and is detected quantitatively by SIM, substantially increases sensitivity.Experimental result shows that this assay method has the features such as sample pre-treatments is easy, reproducible, accuracy is high, rapid sensitive, is suitable for the content measuring ethyl cellosolve acetate in dry food wrapping paper.
Accompanying drawing explanation
Fig. 1 is that head space equilibration time affects result figure to peak area;
Fig. 2 is that head space equilibrium temperature affects result figure to peak area;
Fig. 3 is the chromatogram of the Selective ion mode of standard working solution; In figure, peak 1 is ethyl cellosolve acetate, and peak 2 is naphthalene;
Fig. 4 is the chromatogram of the Selective ion mode of typical mark-on sample; In figure, peak 1 is ethyl cellosolve acetate, and peak 2 is naphthalene.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described.
The material used in following examples, reagent and instrument are specific as follows:
20 dry food wrapping papers such as fast food wrapping paper, candy paper using, wheaten food paper using; Glyceryl triacetate (analyzing pure, chemical reagent Ltd of traditional Chinese medicines group); Ethyl cellosolve acetate, naphthalene (chromatographically pure, Dr Ehrenstorfer company); 6890N/5975 gas chromatography-GC-MS (Agilent company of the U.S.), is equipped with the automatic head space instrument of G1888; HP-VOC capillary chromatographic column (60m × 0.32mm × 1.80 μm); Electronic balance (METTLER TOLEDO company, sensibility reciprocal 0.1mg).
Embodiment 1 sample preparation and analysis
Accurately take 0.1g ethyl cellosolve acetate in 100mL volumetric flask, use glyceryl triacetate constant volume, obtain the primary standard stock solution that concentration is 1000 μ g/mL.Pipette 1mL primary standard stock solution to be settled in 100mL volumetric flask, obtain the secondary standard stock solution that concentration is 10 μ g/mL.
Accurately take 0.1g naphthalene in 100mL volumetric flask, use glyceryl triacetate constant volume, obtain the one-level interior mark stock solution that concentration is 1000 μ g/mL.Pipette mark stock solution in 1mL one-level to be settled in 100mL volumetric flask, obtain the secondary interior mark stock solution that concentration is 10 μ g/mL.Get mark stock solution in 0.5mL secondary and, in 10mL volumetric flask, use glyceryl triacetate constant volume, for subsequent use as host solvents, in it, mark concentration is 0.5 μ g/mL.
Accurately cut out 80cm
2sample, is placed in ml headspace bottle, and adding mark concentration in 1mL is the host solvents of 0.5 μ g/mL, compresses bottle cap rapidly, puts into head-space sampler and carries out GC/MS detection analysis.Detection analysis condition is:
Head space condition: Sample equilibration temperature: 140 DEG C; Sample loop temperature: 150 DEG C; Transmission line temperature: 160 DEG C; Sample equilibration time is 30min; Sample bottle moulding pressure: 15psi; Nebulizer gas pressure: 20psi; Pressing time: 0.2min; The qi of chong channel ascending adversely time: 0.2min; Sample loop equilibration time: 0.05min; Sample injection time: 0.5min.
GC/MS condition: HP-VOC(60m × 0.32mm × 1.80 μm) capillary chromatographic column, carrier gas is helium, flow is 1.5mL/min, sample size is 1 μ L, injector temperature is 220 DEG C, and adopt Splitless injecting samples mode, heating schedule is initial temperature is 50 DEG C (5min), 8 DEG C/min, 200 DEG C (5min); Mass spectrophotometry condition: transmission line temperature is 240 DEG C, ionization mode is EI, ion source temperature is 230 DEG C, quadrupole rod temperature is 150 DEG C, the solvent delay time is 15min, and scan mode is selectivity ion scan pattern (SIM), and wherein the Selective ion mode of object ethyl cellosolve acetate is 128,102, the Selective ion mode of interior mark naphthalene is 43,59,72, is 50ms to the monitoring time of each ion.
Retention time is compared in employing, characteristic ion abundance ratio is qualitative, inner mark method ration under SIM pattern.Wherein object and interior target retention time and characteristic ion as shown in table 1 below.
Table 1 object and interior target retention time and characteristic ion
Embodiment 2
Accurately pipette each 6 parts of the secondary standard stock solution that 50 μ L concentration are 10 μ g/mL, add the secondary interior mark stock solution that 50 μ L concentration are 10 μ g/mL more respectively, and be settled to 1mL with glyceryl triacetate, obtain the inner mark solution that standard solution that concentration is 0.5 μ g/mL and concentration are 0.5 μ g/mL.With reference to the method for embodiment 1, under identical equilibration time, (30min) headspace gas to different equilibrium temperature (60,80,100,120,140 and 160 DEG C) is analyzed, and investigating equilibrium temperature affects (see figure 1) to response.From result, along with the raising of equilibrium temperature, object and interior mark peak area response increase gradually, and between 60 ~ 100 DEG C, speedup is comparatively slow, and between 100 ~ 140 DEG C, speedup is very fast, eases up subsequently.Consider the factor of self physicochemical property of different dryness food wrapper and boiling point two aspect of object, selecting 140 DEG C is Sample equilibration temperature.
Embodiment 3
By the method for embodiment 2, prepare the inner mark solution that standard solution that concentration is 0.5 μ g/mL and concentration are 0.5 μ g/mL.Under identical temperature-time, (140 DEG C) headspace gas to different equilibration time (5,10,15,20,30 and 40min) is analyzed, and investigating equilibration time affects (see figure 2) to response.Object through 5 ~ 30min substantially object and interior mark peak area response increase gradually, after 30min, speedup tends towards stability, and considers detection efficiency, and preferred 30min is as the equilibration time of sample.
Embodiment 4
Accurately pipetting concentration is that secondary standard stock solution 5,10,50, the 100 and 500 μ L of 10 μ g/mL is in the ml headspace bottle of 5 20mL, add the secondary interior mark stock solution that 50 μ L concentration are 10 μ g/mL more respectively, and be settled to 1mL with glyceryl triacetate, obtain the standard working solution that concentration is respectively 0.05,0.1,0.5,1 and 5 μ g/mL, wherein, target concentration is 0.5 μ g/mL.With reference to the method for embodiment 1, respectively head space balance is carried out to this series standard working solution, then GC/MS analysis (typical standard working solution chromatogram is shown in Fig. 3) is carried out, with the concentration (μ g/mL) of ethyl cellosolve acetate and interior mark naphthalene than X for horizontal ordinate, with the peak area ratio Y of ethyl cellosolve acetate and interior mark naphthalene for ordinate, carry out linear regression, draw the typical curve of object, calculate the regression equation of object typical curve, calculate method quantitative limit with 10 times of signal to noise ratio (S/N ratio)s (S/N=10).Result is: the regression equation Y=0.1875X-0.000442 of ethyl cellosolve acetate, related coefficient 0.9999, the range of linearity 0.05 ~ 5 μ g/mL and detection limit 0.031 μ g/mL.
With a fast food wrapping paper (actual detected value is not for detecting) for research object, add low, to neutralize high 3 variable concentrations (0.1,0.5 and 2 μ g/mL) standard solution respectively, head space-gas chromatography mass spectrometry selectivity method is adopted to measure corresponding object content (mean value measured for 6 times), according to measurement result and standard substance addition, the recovery of standard addition (seeing the following form 2) of computing method.Result shows, and the recovery of standard addition of method, between 87.5% ~ 96.0%, illustrates that the accuracy of this method is higher; Relative standard deviation RSD is 3.91%, is less than 5%, shows that the repeatability of this method is better.
The recovery of standard addition of table 2 method and precision (n=6)
Mark-on level | The recovery (%) | RSD(%) |
Low | 87.5 | 3.91 |
In | 92.3 | 2.25 |
High | 96.0 | 1.97 |
As stated above, get 20 dry food wrapping paper samples (comprising fast food wrapping paper, candy paper using, wheaten food paper using etc.) and detect, all do not detect ethyl cellosolve acetate.In addition, with a candy paper using for determination object (measured value is not for detecting), add to it standard specimen that concentration is 2 μ g/mL, fructufy measured value is 1.93mg/kg, relative deviation is 1.78%, and as shown in Figure 4, the accuracy of visible measurement result is better for the chromatogram of Selective ion mode.
Therefore, method based on ethyl cellosolve acetate in head space-gas chromatography mass spectrometry selective determination dry food wrapping paper provided by the invention, effectively can avoid solvent-extracted laborious steps in sample pretreatment process, and detected quantitatively by SIM, greatly can improve detection sensitivity and qualitative accuracy.Experimental result shows that this assay method has the features such as sample pre-treatments is easy, reproducible, accuracy is high, rapid sensitive, is suitable for the content measuring ethyl cellosolve acetate in dry food wrapping paper.
Interior mark liquid used by the present embodiment and standard solution are only described for one of them concentration, the typical curve that the interior mark liquid that other concentration value configures and standard solution obtain through chromatograph mass spectrum analysis and regression equation same as the previously described embodiments, do not enumerating at this.Illustrated embodiment just method for a better understanding of the present invention, do not have any restriction, namely the method for said method or equivalent above-mentioned situation is all included in the protection domain of technical scheme of the present invention.
Claims (6)
1., based on a method for ethyl cellosolve acetate in head space-gas chromatography mass spectrometry selective determination dry food wrapping paper, it is characterized in that, comprise the steps:
(1) get standard substance ethyl cellosolve acetate, be made into Standard Stock solutions with glyceryl triacetate;
(2) get internal standard compound matter naphthalene, be made into the glyceryl triacetate solution of naphthalene with glyceryl triacetate, for subsequent use as host solvents;
(3) Standard Stock solutions many parts is got, add the host solvents of different amount respectively, and the standard working solution of a series of variable concentrations gradient is obtained with glyceryl triacetate constant volume, after respectively standard working solution being carried out head space balance, after transmission line sample introduction, carry out GC/MS-SIM detection; With the concentration ratio X of ethyl cellosolve acetate and interior mark naphthalene for horizontal ordinate, with the peak area ratio Y of ethyl cellosolve acetate and interior mark naphthalene for ordinate, carry out linear regression, draw the typical curve of object, calculate the regression equation of object typical curve;
(4) dry food wrapping paper is cut out be placed in ml headspace bottle, add host solvents, rapid sealing, carry out head space process, ready to balance enters gas chromatograph-mass spectrometer through transmission line after sampling well, carries out GC/MS-SIM and detects analysis, the ratio of the peak area of the ethyl cellosolve acetate obtained with the peak area of interior mark naphthalene is substituted in backhaul equation respectively, can be calculated the corresponding content of ethyl cellosolve acetate in dry food packaging;
Wherein, in step (3) and step (4), the analysis condition of head space is identical, is: Sample equilibration temperature: 140 DEG C; Sample loop temperature: 150 DEG C; Transmission line temperature: 160 DEG C; Sample equilibration time is 30min; Sample bottle moulding pressure: 15psi; Nebulizer gas pressure: 20psi; Pressing time: 0.2min; The qi of chong channel ascending adversely time: 0.2min; Sample loop equilibration time: 0.05min; Sample injection time: 0.5min;
In step (3) and step (4), the analysis condition of GC/MS is identical, is:
GC conditions: adopt HP-VOC capillary chromatographic column, carrier gas is helium, flow is 1.5mL/min, sample size is 1 μ L, and injector temperature is 220 DEG C, adopts Splitless injecting samples mode, heating schedule is initial temperature is 50 DEG C, keep 5min, be increased to 200 DEG C with the speed of 8 DEG C/min, keep 5min;
Mass spectrophotometry condition: transmission line temperature is 240 DEG C, ionization mode is EI, and ion source temperature is 230 DEG C;
Quadrupole rod temperature is 150 DEG C, the solvent delay time is 15min, and scan mode is selectivity ion scan pattern, and wherein the Selective ion mode of object ethyl cellosolve acetate is 128,102, the Selective ion mode of interior mark naphthalene is 43,59,72, is 50ms to the monitoring time of each ion.
2. the method based on ethyl cellosolve acetate in head space-gas chromatography mass spectrometry selective determination dry food wrapping paper according to claim 1, is characterized in that, in step (1), the concentration of Standard Stock solutions is 5 ~ 15 μ g/mL.
3. the method based on ethyl cellosolve acetate in head space-gas chromatography mass spectrometry selective determination dry food wrapping paper according to claim 1 and 2, is characterized in that, in step (2), the concentration of host solvents is 0.3 ~ 0.7 μ g/mL.
4. the method based on ethyl cellosolve acetate in head space-gas chromatography mass spectrometry selective determination dry food wrapping paper according to claim 1 and 2, it is characterized in that, in step (3), the standard working solution of a series of variable concentrations gradient is 5 parts, in solution, the concentration of ethyl cellosolve acetate is respectively 0.05,0.1,0.5,1 and 5 μ g/mL, and the concentration of interior mark naphthalene is 0.5 μ g/mL.
5. the method based on ethyl cellosolve acetate in head space-gas chromatography mass spectrometry selective determination dry food wrapping paper according to claim 1, it is characterized in that, in step (3), the regression equation Y=0.1875X-0.000442 of ethyl cellosolve acetate, related coefficient 0.9999, the range of linearity 0.05 ~ 5 μ g/mL and detection limit 0.031 μ g/mL.
6. the method based on ethyl cellosolve acetate in head space-gas chromatography mass spectrometry selective determination dry food wrapping paper according to claim 1, it is characterized in that, in step (4), be 80cm often cutting out area
21 ~ 5mL host solvents is added in testing sample.
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CN106872620B (en) * | 2017-04-27 | 2019-11-26 | 上海烟草集团有限责任公司 | The measuring method of glycol ether substance in a kind of cigarette packaging paper |
CN109444295A (en) * | 2018-12-29 | 2019-03-08 | 深圳出入境检验检疫局工业品检测技术中心 | Measure 8 kinds of methods for limiting spent glycol ether solvent content in dyeing and finishing auxiliaries for textile |
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