CN106680396A - Method for determining phthalic acid esters and tributyl phosphate plasticizers in exploding beads for cigarette - Google Patents
Method for determining phthalic acid esters and tributyl phosphate plasticizers in exploding beads for cigarette Download PDFInfo
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention relates to a method for determining phthalic acid esters and tributyl phosphate plasticizers in exploding beads for cigarette. The method is characterized by comprising the following steps: mixing protons of the exploding beads and inert ceramics under the existence of a solvent; adopting an external force shocking method (vortex) for breaking the exploding beads; and adopting a micro-membrane for filtering the mixed solution appearing after the breaking of the exploding beads, and then adopting gas chromatography-mass spectrum (GC-MS) combination for realizing the high throughput test for different plasticizers. According to the method, the breaking of the exploding beads and the extraction of the target objects are completed in one step, and meanwhile, the determination for the phthalic acid esters and the tributyl phosphate plasticizers is realized. The method has the advantages of higher determining flux, high recovery rate and high accuracy.
Description
Technical field
The invention belongs to cigarette additive harmful components physico-chemical analysis field, specifically one kind are suitable to cigarette adjacent benzene in quick-fried pearl
The assay method of dicarboxylic acid esters and tributyl phosphate class plasticizer.
Background technology
Cigarette is a kind of spherical little glue bead with quick-fried pearl, and inside is with high concentration fragrance（Generally mint flavored or other phases
The fragrance of pass）Liquid.Quick-fried pearl is typically placed in the filter stick of Medicated cigarette, smoker when smoking cigarette, with handss by quick-fried pearl
Crumb, perfume liquid therein flows out, make flue gas that there is ice-cold and moistening mediation sense, flue gas has been neutralized to a certain extent
Rough sense and zest, improve the jealous of flue gas.
Quick-fried pearl cigarette causes pursuing for many cigarette manufacturers once appearance, to the end of the year 2015, can see in China market
Nearly 20 sections of quick-fried pearl product.Although quick-fried pearl cigarette is considered a kind of characteristic cigarette product by FCTC, cigarette is anticipated with quick-fried pearl from certain
The one kind in cigarette additive is remained in justice.And the composition disclosure to cigarette additive and its Related product is with control
WHO is emphasized always and one of the direction paid close attention to.
Consumer, when sucking to quick-fried pearl cigarette, is that quick-fried pearl is crumbed first, and the liquid in quick-fried pearl is entered in flue gas
With human contact, the measure determined mainly to liquid in quick-fried pearl to Related Component in quick-fried pearl.Since Taiwan beverage in 2011
" mist generating agent " event after, supervision of the Chinese government to adjacent phenyl ester class plasticiser in food is further increased.Research shows, this
Class material can cause the feature of nervus centraliss and peripheral nervous system to change, and show stronger endocrine disrupting, be one
Environmental hormone is planted, its long term accumulation in vivo can have a strong impact on human normal physiological function, with teratogenesis, carcinogenic and cause is prominent
The harm such as change.And tributyl phosphate is also a kind of conventional plasticiser, initially mainly occur from the article of everyday use such as toothpaste, it is modern
Research shows that it has strong impulse to act on skin and respiratory tract, with the effect of whole body intoxicating
The cigarette measure of plasticizer in quick-fried pearl has no at present correlation technique recommendation, to phthalic acid ester and phosphorus of the cigarette in quick-fried pearl
The related supervision and inspection of industry will be provided necessary foundation by the detection of sour tributyl class plasticiser.
The content of the invention
A kind of cigarette phthalic acid in quick-fried pearl that the purpose of the present invention is based on above-mentioned prior art situation and provides
The assay method of ester and tributyl phosphate class plasticizer, the method be by cigarette with quick-fried pearl in the presence of a solvent, carry out thing
Reason is broken, the mixed solution after crushing after filtration, using gas chromatogram-mass spectrometry instrument（GC-MS）To neighbour therein
Phenyl ester and tributyl phosphate class plasticizer are measured.
The purpose of the present invention is achieved through the following technical solutions：
A kind of cigarette assay method of phthalate and tributyl phosphate plasticizer in quick-fried pearl, is broken to cigarette with quick-fried pearl sample
Determinand is extracted while broken, using gas chromatography-mass spectrography（GC-MS）Realize the high pass of different type plasticizer
Amount detection, concrete step excessively is as follows：
（1）Cigarette is crushed with quick-fried pearl
The quick-fried pearl samples of 0.2-0.3g are weighed into 25 mL conical flask with stopper, accurately to 0.0001 g, some ceramic homogenizing is added
Son, adds 5-10 mL isopropanols and 100 L inner mark solutions, using vortex oscillation instrument, carries out under conditions of 2000 rpm
The min of vortex oscillation 5, after quick-fried pearl is broken, takes appropriate supernatant, through 0.22 m nylon leaching films.
（2）Blank experiment
Sample is not added with, is repeated（1）Step.Because scope is wider used in plastic laboratory, and plasticizer is in plastic
In also generally existing, in order to avoid external plasticizer is polluted to sample, it is necessary to do blank assay.
（3）Instrumental Analysis
Determined using GC-MS, condition determination is as follows：
GC conditions：
Injector temperature：280℃；Sample size：1 μ L, split sampling（Split ratio：10:1）；Carrier gas：Helium（Purity >=
99.999%）, constant current mode, flow velocity：1.0 mL/min；Heating schedule：60 DEG C of initial temperature, keeps 1 min, with 20 DEG C/min
Speed to 220 DEG C, keep 1 min, then with the speed of 5 DEG C/min to 280 DEG C, keep 15 min.
Mass Spectrometry Conditions：
Ionization mode：Electron bombardment ionization source（EI）；Ionizing energy：70 eV；Transmission line temperature：280℃；Ion source temperature：230℃；
Quadrupole rod temperature：150℃；Mensuration mode：Select ion surveillance style（SIM）Scanning；Solvent delay：6 min.Each compound
SIM conditions are shown in Table 1.Each compound SIM conditions are shown in Table 1.
Deuterated-dibutyl phthalate is adopted in the present invention（Dibutyl phthalate-3,4,5,6-D4, No. CAS：
93952-11-5）As internal standard substance, purity >=99%, isopropanol is adopted when using, concentration is 0.1 mg/mL.
Measure of the present invention to quick-fried pearl sample, is primarily directed to the measure of content in quick-fried pearl, how in quick-fried pearl
It is tolerant to carry out extracting the problem for being this experiment firstly the need of consideration solution.Present invention selection carries out physics to quick-fried pearl sample and crushes.
Relative to chemically fragmenting, physics crushes the primary characteristic for contributing to preferably ensureing sample, is conducive to the stability of measurement result
With repeatability.Experiment is crushed using the method for adding liquid flux and ceramics proton and carrying out vortex oscillation to quick-fried pearl, quick-fried
During pearl is broken, extraction of the solvent to quick-fried pearl content is also achieved.Test result indicate that, the broken time of quick-fried pearl with it is molten
The type of agent is respectively provided with certain relation with the number of ceramics proton, but relative to the number of ceramic proton, solvent
Type is bigger to the impact for crushing the time.Experiment weighs first the quick-fried pearl sample of 3 parts of 0.2g, each ceramics for adding 1 internal diameter for 1cm
Proton, adds respectively 10mL ethanol, isopropanol, normal hexane in 3 parts of samples.Every part of sample（The experiment of every kind of different solvents
Condition）Parallel assay 3 times.Fig. 3 is listed and the average consumption that the quick-fried pearl sample of quality is all crushed is similar under the conditions of 3 kinds of different solvents
When.As can be seen from Figure 3, ethanol and isopropanol short time consumption are essentially identical（5min or so）, and normal hexane is then time-consuming longer（>
30min）, it is time-consuming to have reduced when by the ceramics number of proton is increased in normal hexane sample, but relative to other two kinds
Reagent, hence it is evident that crushing efficiency is relatively low.It is not strong in view of adjacent benester compound polarity itself, and with the increase of carbochain, polarity
Further weaken, and ethanol polarity and dissolubility are stronger relative to isopropanol, easily bring into some impurity in sample, affect to survey
It is fixed, therefore, experimental selection isopropanol is crushed to quick-fried pearl sample.Mixed solution clarification after broken, without lamination.
Plastic containers can not be adopted in experiment, all using glass drying oven after glass drying oven used is cleaned, one-level water should be used
Drip washing three times, the h of acetone soak 1 after room temperature volatilization is dry, toasts 2 h at 200 DEG C, is cooled to room temperature standby.
Ion detection used in measure（SIM）Function, the capillary chromatographic column for using：Fixing phase：5% phenyl/95% methyl
Polysiloxanes；Specification：[30 m（Length）× 0.25 mm（Internal diameter）× 0.25 μm（Thickness）.
Due to plasticizer class material generally existing in the environment, therefore, determine be both needed to do blank every time, in calculating process
In, should be by blank deduction.
The configuration of standard solution and inner mark solution：
Mixed standard solution I：0.02 g is weighed respectively（It is accurate to 0.1 mg）Various plasticizer standard substance, are placed in same 10 mL
In volumetric flask, dissolved with isopropanol and constant volume, be configured to the mixed standard solution I that concentration is 2 mg/mL.In 0 DEG C~4 DEG C ice
Keep in dark place in case, 6 months effect duration.
Mixed standard solution II：0.5 mL mixed standard solutions I are accurately pipetted, in being placed in 10 mL volumetric flasks, with isopropanol
Constant volume, is configured to the mixed standard solution II that concentration is 0.1 mg/mL.Keep in dark place in 0 DEG C~4 DEG C refrigerators, effect duration 6
Individual month.
Standard working solution：Accurately pipette 10 μ L, 20 μ L, 40 μ L, 100 μ L, 200 μ L, the hybrid standard of 500 μ L
Solution II, in being placed in respective 10 mL volumetric flasks, then accurately adds 100 μ L inner mark solutions, and with isopropanol scale is settled to,
Obtain final product series standard working solution.The series standard solution concentration of preparation is： 0.1 μg/mL、0.2 μg/mL、0.4 μg/mL、
1 μg/mL、2 μg/mL、5 μg/mL。
Taking standard working solution carries out GC/MS analyses, and vertical coordinate is the quota ion peak area and internal standard of each analyte
The ratio of thing quota ion peak area, abscissa is each analyte concentration, takes 5 points of wherein at least, does the mark of each analyte
Quasi- working curve.19 kinds of plasticizers are linear good in the concentration range of 0.1-5 g/mL, and correlation coefficient is from 0.9992-
1.0000。
Test positive is chosen, recovery of standard addition experiment is carried out, plus scalar is respectively 0.2, Isosorbide-5-Nitrae g/mL, each
Equal parallel assay 5 times, average in mark-on level, and calculate the relative mean standard deviation of 5 parallel assays（RSD）, by
This obtains average recovery rate and RSD of 19 kinds of plasticisers in different mark-on levels, and concrete outcome is shown in Table 2 and table 3.
Can be obtained by table 2, the low mark recovery of standard addition scope of 19 kinds of plasticizers is 95.5 ~ 106.7%；Acceptance of the bid mark-on reclaims
, 92.0 ~ 105.4%, high standard recovery of standard addition scope is 96.0 ~ 107.3%, and this method response rate result is good for rate scope.
As shown in Table 3, the relative standard deviation of 5 parts of measurement results illustrates that this method is very stable within 8%, repeatability
It is good.
Test positive is chosen, mark-on is carried out with the minimum cup concentration of standard curve, replication 10 times is calculated and determined
As a result SD, using 3SD and 10SD as the detection limit of method（LOD）And quantitative limit（LOQ）, the results are shown in Table 4.
Description of the drawings
Fig. 1 is the chromatogram of Plays solution of the present invention；
In Fig. 1：1-DMP, 2-DEP, 3-DAP, 4-DIBP, 5-DBP, 6-DMEP, 7-BMPP, 8-DEEP, 9-DPP, 10-DHXP,
11-BBP, 12-DBEP, 13-DCHP, 14-DEHP, 15- diphenyl phthalate, 16-DNOP, 17-DINP, 18-DNP, 19-
TBP, IS- internal standard.
Fig. 2 is the chromatogram of mark-on sample determination in the present invention；
In Fig. 2：2-DEP 14-DEHP IS- internal standards.
Fig. 3 is different solvents, the broken time difference contrast of different condition.
Specific embodiment
Embodiment：Cigarette adds the measure of plasticizer in standard specimen with quick-fried pearl.
1）Sample pre-treatments
The quick-fried pearl samples of 0.2-0.3g are weighed into 25 mL conical flask with stopper, accurately to 0.0001 g, some ceramic homogenizing is added
Son, is separately added into the diethyl phthalate that certain volume concentration is about 0.1mg/mL（DEP）With (the 2- second of phthalic acid two
Base) own ester（DEHP）Singly mark solution（Solvent is isopropanol）, 5-10 mL isopropanols and 100 L inner mark solutions（Deuterated-adjacent benzene two
Formic acid dibutyl ester concentration is the aqueous isopropanol of 0.1 mg/mL）, using vortex oscillation instrument, carry out under conditions of 2000 rpm
The min of vortex oscillation 5, after quick-fried pearl is broken, takes appropriate supernatant, through 0.22 m nylon leaching films.
2）Blank experiment
Sample is not added with, is repeated（1）Step.
3）Instrumental Analysis
Determined using GC-MS, condition determination is as follows.
GC conditions：
Injector temperature：280℃；Sample size：1 μ L, split sampling（Split ratio：10:1）；Carrier gas：Helium（Purity >=
99.999%）, constant current mode, flow velocity：1.0 mL/min；Heating schedule：60 DEG C of initial temperature, keeps 1 min, with 20 DEG C/min
Speed to 220 DEG C, keep 1 min, then with the speed of 5 DEG C/min to 280 DEG C, keep 15 min.
Mass Spectrometry Conditions：
Ionization mode：Electron bombardment ionization source（EI）；Ionizing energy：70 eV；Transmission line temperature：280℃；Ion source temperature：230℃；
Quadrupole rod temperature：150℃；Mensuration mode：Select ion surveillance style（SIM）Scanning；Solvent delay：6 min.Each compound
SIM conditions are shown in Table 1.
4）The preparation of standard solution is as it was previously stated, be not repeated herein.
5）Taking standard working solution carries out GC/MS analyses, vertical coordinate be the quota ion peak area of each analyte with it is interior
The ratio of mark thing quota ion peak area, abscissa is each analyte concentration, takes 5 points of wherein at least, does each analyte
Standard working curve.
6）Computing formula
The content of each analyte presses formula in sample（1）Calculated：
…………………………………（1）
In formula：
X i --- the content of plasticizer in sample, unit for milligrams per kilogram（mg/kg）；
C i --- plasticizer concentration in the sample drawn by standard curve, unit is micrograms per millilitre（μg/mL）；
C i0 --- plasticizer concentration in the blank drawn by standard curve, unit is micrograms per millilitre（μg/mL）；
V--- the volume of test fluid, unit is milliliter（mL）, it is herein the volume of isopropanol, 10 mL；
m--- sample mass, unit for gram（g）.
With the meansigma methodss of parallel assay twice as final measurement result, 1 mg/kg is accurate to.
Phthalic acid ester content in mark-on sample is calculated by above formula, concrete outcome is shown in Table 5, and chromatogram is shown in accompanying drawing 2.
The sample size of table 5
Claims (5)
1. a kind of cigarette assay method of phthalate and tributyl phosphate plasticizer in quick-fried pearl, it is characterised in that：It is right
Determinand is extracted while cigarette is with quick-fried pearl sample broke, using gas chromatography-mass spectrography（GC-MS）Realize inhomogeneity
The high throughput testing of type plasticizer, comprises the following steps that：
The quick-fried pearl samples of 0.2-0.3g are weighed into 25 mL conical flask with stopper, accurately to 0.0001 g, some ceramic homogenizing is added
Son, adds 5-10 mL isopropanols and 100 L inner mark solutions, using vortex oscillation instrument, carries out under conditions of 2000 rpm
The min of vortex oscillation 5, after quick-fried pearl is broken, takes appropriate supernatant, through 0.22 m nylon leaching films, is detected using GC-MS；
Blank assay is done per batch, that is, is not added with sample, repeat the above steps.
2. method according to claim 1, it is characterised in that：Inner mark solution is deuterated-dibutyl phthalate concentration
For the aqueous isopropanol of 0.1 mg/mL.
3. method according to claim 1, it is characterised in that：The analysis condition of GC-MS is as follows：
GC conditions：
Injector temperature：280℃；Sample size：1 μ L, split sampling, split ratio：10:1；Carrier gas：Helium, constant current mode, stream
Speed：1.0 mL/min；Heating schedule：60 DEG C of initial temperature, keeps 1 min, with the speed of 20 DEG C/min to 220 DEG C, keeps 1
Min, then with the speed of 5 DEG C/min to 280 DEG C, keep 15 min；
Mass Spectrometry Conditions：
Ionization mode：Electron bombardment ionization source（EI）；Ionizing energy：70 eV；Transmission line temperature：280℃；Ion source temperature：230℃；
Quadrupole rod temperature：150℃；Mensuration mode：Select ion surveillance style（SIM）Scanning；Solvent delay：6 min.
4. method according to claim 1, it is characterised in that：When being detected using GC-MS, each analyte in sample
Content press formula（1）Calculated：
…………………………………（1）
In formula：
X i --- the content of plasticizer in sample, unit for milligrams per kilogram（mg/kg）；
C i --- plasticizer concentration in the sample drawn by standard curve, unit is micrograms per millilitre（μg/mL）；
C i0 --- plasticizer concentration in the blank drawn by standard curve, unit is micrograms per millilitre（μg/mL）；
V--- the volume of test fluid, unit is milliliter（mL）, it is herein the volume of isopropanol, 10 mL；
m--- sample mass, unit for gram（g）；
With the meansigma methodss of parallel assay twice as final measurement result, 1 mg/kg is accurate to.
5. method according to claim 1, it is characterised in that：The phthalate and tributyl phosphate plasticizer
Specifically include following 19 kinds：Dimethyl phthalate, diethyl phthalate, diallyl phthalate, adjacent benzene two
Diisobutyl formate, dibutyl phthalate, phthalic acid two (2- methoxyl groups) ethyl ester, phthalic acid two (4- methyl-
2- amyl groups) ester, phthalic acid two (2- ethyoxyls) ethyl ester, diamyl phthalate, dihexylphthalate, adjacent benzene two
Formic acid butyl benzyl ester, phthalic acid two (2- butoxy) ethyl ester, the dicyclohexyl phthalate, (2- of phthalic acid two
Ethyl) own ester, diphenyl phthalate, dinoctyl phthalate, diisononyl phthalate, phthalic acid two
Nonyl ester, tributyl phosphate.
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| CN107807186A (en) * | 2017-10-24 | 2018-03-16 | 中国烟草总公司郑州烟草研究院 | The assay method of the quick-fried pearl spices rate of transform in total particulate matter in mainstream smoke of mouth rod |
| CN108645939A (en) * | 2018-02-28 | 2018-10-12 | 浙江省林产品质量检测站（浙江省林木种苗质量监督检验站） | The extraction and purification methods of phthalate plasticiser in one vegetable oil |
| CN108680691A (en) * | 2018-05-15 | 2018-10-19 | 国家烟草质量监督检验中心 | The assay method of phthalic acid ester in essence spice for cigarette |
| CN109142570A (en) * | 2018-08-14 | 2019-01-04 | 广东中烟工业有限责任公司 | A kind of the cigarette extraction of flavor component and content assaying method in quick-fried pearl |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107807186A (en) * | 2017-10-24 | 2018-03-16 | 中国烟草总公司郑州烟草研究院 | The assay method of the quick-fried pearl spices rate of transform in total particulate matter in mainstream smoke of mouth rod |
| CN108645939A (en) * | 2018-02-28 | 2018-10-12 | 浙江省林产品质量检测站（浙江省林木种苗质量监督检验站） | The extraction and purification methods of phthalate plasticiser in one vegetable oil |
| CN108645939B (en) * | 2018-02-28 | 2021-04-16 | 浙江省林产品质量检测站（浙江省林木种苗质量监督检验站） | Method for extracting and purifying phthalate plasticizer in vegetable oil |
| CN108680691A (en) * | 2018-05-15 | 2018-10-19 | 国家烟草质量监督检验中心 | The assay method of phthalic acid ester in essence spice for cigarette |
| CN108680691B (en) * | 2018-05-15 | 2020-06-19 | 国家烟草质量监督检验中心 | Method for determining phthalate in tobacco flavor and fragrance |
| CN109142570A (en) * | 2018-08-14 | 2019-01-04 | 广东中烟工业有限责任公司 | A kind of the cigarette extraction of flavor component and content assaying method in quick-fried pearl |
| CN110967087A (en) * | 2019-10-11 | 2020-04-07 | 广东中烟工业有限责任公司 | Method for measuring volume of liquid exuded from bead blasting filter tip |
| CN110967087B (en) * | 2019-10-11 | 2021-07-09 | 广东中烟工业有限责任公司 | Method for measuring volume of liquid exuded from bead blasting filter tip |
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