CN103630601A - Determination method for specific migration quantities of multiple elements in cigarette filter - Google Patents
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Abstract
The invention provides a determination method for specific migration quantities of multiple heavy metals in a cigarette filter. The determination method comprises the following steps: S1, putting a to-be-detected sample into a quantification flask, adding artificial simulated saliva, placing the quantification flask in a lukewarm bath and carrying out vibration so as to obtain a sample dissolution liquid; S2, filtering the sample dissolution liquid obtained in the step S1 so as to obtain a to-be-detected solution; and S3, subjecting the to-be-detected solution obtained in the step S2 to quantitative determination of specific migration quantities of a plurality of elements in the solution by cooperatively using an internal standard method and inductively coupled plasma mass-spectrometry. According to the invention, specific migration quantities of a plurality of heavy metals can be measured in one shot by cooperatively using the internal standard method and the inductively coupled plasma mass-spectrometry, so technical bases and support are provided for evaluation of smoking security of cigarette products.
Description
Technical field
the present invention relates to technical field of tobacco, more specifically, relate to the assay method of multiple element Special migration in a kind of cigarette filter.
Background technology
in tobacco and cigarette auxiliary material, the content of heavy metal, migration and control are the hot issues that vast tobacco scientific worker pays close attention to always.Cigarette filter material mainly comprises tipping paper, forming paper, vinegar fibre or the third fibre, adhesive etc. for cigarette, in these smoking materials, contain some chemical compositions to human body existence or potential hazard, as heavy metal, benzene and benzene homologues, phthalate, volatile organic matter etc.For meeting the requirements such as cigarette sign, rich colors, tipping paper conventionally will print, prints the operations such as aftertreatment and become final tipping paper product.At various cigarettes, with in filter tip auxiliary material, in tipping paper, the content of heavy metal is relatively high, and its main source is the various pigment in printing-ink.Forming paper, vinegar fibre or the third fibre, cigarette contain a certain amount of heavy metal element that obtains equally with adhesive.When people carry out smoking cigarette by filter tip, filter tip directly contacts with human oral cavity frequently, and the material of stripping is absorbed by the body by the digestion of gastric juice, and objectionable constituent wherein may cause certain threat or have potential harm smoker's health.
Industry relevant criterion or the document reported at present, the analysis that filter tip material heavy metal is carried out is all the contained total metals of material and measures, but how total amount does not represent the many of stripping state, because the stripping quantity of every kind of composition depends on its dissolution characteristics, but also relevant with typography, pigment matrix, sheet properties etc.Therefore, in cigarette filter, the detection analysis of element Special migration highlights importance, may be more realistic.
in ICP-MS analyte detection process, the signal of object element is often subject to mass spectrum and non-mass spectrum factor is disturbed.In mass spectrum disturbs, isobar interference overlapping and polyatomic molecule ion pair analytic signal is very important, as
204hg couple
204pb
+there is isobar interference, argon Diatomic molecular ion ArAr
+right
80se
+there is polyatomic molecule ion interference etc.
Summary of the invention
The object of the invention is to, the present situation that change can only check weighing total metal content, provides a kind of determination method that can detect the migration amount of certain heavy metal species.
In order to realize above goal of the invention, the invention provides the assay method of various heavy Special migration in a kind of cigarette filter, comprise the following steps:
S1. testing sample is packed in volumetric bottle, add manual simulation's saliva, volumetric bottle is placed in to tepidarium and shakes, obtain sample dissolution fluid;
S2. the sample dissolution fluid of step S1 gained is filtered, obtain solution to be measured;
S3. by the solution to be measured of step S2 gained, by internal standard method, coordinate the wherein Special migration of multiple element of inductively coupled plasma mass spectrometry quantitative measurement.
Described multiple element is in Al, As, B, Ba, Cd, Co, Cr, Cu, Fe, Hg, Mn, Ni, Pb, Sb, Se, Sn, Sr, V or Zn two kinds and two or more.
The interior mark that described multiple element is corresponding is respectively: Al:
45sc, As:
72ge, B:
45sc, Ba:
159tb, Cd:
115in, Co:
72ge, Cr:
72ge, Cu:
72ge, Fe:
72ge, Hg:
175lu, Mn:
72ge, Ni:
72ge, Pb:
175lu, Sb:
115in, Se:
72ge, Sn:
115in, Sr:
72ge, V:
45sc and Zn:
72ge.
The inner mark solution of described internal standard method contains
45sc,
72ge,
115in,
159tb,
175lu element, described interior target concentration is 10 μ g/L.Only need disposable interpolation inner mark solution, need to not add specific interior mark for element-specific, easy use.
The volume ratio of the quality of the testing sample described in step S1 and manual simulation's saliva is 1:10～1:40.
The volume ratio of the quality of the testing sample described in step S1 and manual simulation's saliva is 1:30～1:40.
The running parameter of described inductively coupled plasma mass spectrometry: cooling gas flow 14.3 L/min; Assisted gas flow 0.8 L/min; Carrier gas flux 1.08 L/min; Spray chamber temperature: 2.0 ℃; Peristaltic pump gathers revolution: 0.1 rps, and sample promotes revolution: 0.5 rps; RF power 1500 W; Sampling depth: 8.0mm; Collection is counted: 3; Multiplicity: 3.Selection due to the parameter of ICP-MS, can effectively reduce the interference between each element.
The water temperature of the tepidarium described in step S1 is 36 ~ 38 ℃, and the speed of described concussion is 60r/min, and the time of concussion is 90 ~ 120 minutes.
Volumetric bottle described in step S1 is 50mL polyethylene terephthalate plastics volumetric bottles.
The invention has the advantages that:
1. set up the assay method of multiple element Special migration in a kind of reliable and stable, easy and simple to handle, reproducible cigarette filter, the safety evaluatio of sucking that can be cigarette product provides technology to rely on and supports.
Detection method provided by the invention can be comparatively actual environment that effectively analog roll cigarette filter tip contacts with saliva in human oral cavity, easy and simple to handle, highly sensitive, detection limit is low, the recovery good.In prior art, there is not yet under the base condition of artificial saliva and determine Al, As, B, Ba, Cd, Co, Cr, Cu, Fe, Hg, Mn, Ni, Pb, Sb, Se, Sn, Sr, V, Zn various heavy by ICP-MS simultaneously.
3. the signal for fear of object element is often subject to mass spectrum and the interference of non-mass spectrum factor, and the present invention has selected specific several isotope as interior mark, has effectively reduced interference.Selecting the corresponding interior timestamp of each object element, mainly follow following principle: in (1) test solution, do not contain this internal standard element; (2) object element mass number is close with interior target; (3) object element ionization energy and internal standard element is close.Through a large amount of experiments, find:
45sc,
72ge,
115in,
159tb,
175lu is suitable as internal standard element.
Embodiment
Below in conjunction with specific embodiment, further describe the present invention.Unless stated otherwise, reagent, equipment and the method that the present invention adopts is the conventional commercial reagent of the art, equipment and the conventional method of using.
Determining of embodiment 1 experiment condition
1.1 instruments and reagent
Agilent 7700x type icp ms (U.S. Agilent company); SIGMA 3-18K supercentrifuge (German SIGMA company); SHZ-82 type water-bath constant temperature oscillator (Jintan City Guo Wang experimental apparatus factory); Milli-Q Integral type ultrapure water system (U.S. Millipore company).
HNO
3(65%, top grade is pure, German Merck company); Al, As, B, Ba, Cd, Co, Cr, Cu, Fe, Hg, Mn, Ni, Pb, Sb, Se, Sn, Sr, V and Zn single element mark liquid (1000 mg/L, State Standard Matter Research Centre); Au single element mark liquid (10 mg/L, State Standard Matter Research Centre); Interior mark mixed solution (
45sc,
72ge,
115in,
159tb,
175lu, 10 mg/L, U.S. Agilent company); Tuning liquid (Ce, Co, Li, Mg, Tl, Y are 1 μg/L， U.S. Agilent company).
1.2 instrument condition
Mixed standard solution with Ce, the Co of 1 μ g/L, Li, Mg, Tl, Y carries out tuning optimization to instrument parameter.ICP-MS running parameter: cooling gas flow 14.3 L/min; Assisted gas flow 0.8 L/min; Carrier gas flux 1.08 L/min; Spray chamber temperature: 2.0 ℃; Peristaltic pump gathers revolution: 0.1 rps, and sample promotes revolution: 0.5 rps; RF power 1500 W; Sampling depth: 8.0mm; Collection is counted: 3; Multiplicity: 3.Element mass number to be measured and corresponding internal standard element, integral time are as shown in table 1:
Table 1 element to be measured, corresponding internal standard element and integral time
1.3 sample preparation
The pre-prepared method of laboratory sample is for radially to cut sample in cross section apart from contact jaw 0.2 ~ 1.5cm place, filter tip oral cavity.Take 1.0g laboratory sample, be accurate to 0.001g, be placed in the 50mL polyethylene terephthalate plastics volumetric bottle with spiral cover, in volumetric bottle, add manual simulation's saliva that sample quality and manual simulation's saliva volume ratio are 1:10～1:40, screw bottle cap, be placed in temperature and be standing on the constant temperature oscillator of 37 ± 1 ℃ or vibrate 120 minutes.Then cross immediately 0.45 μ m water membrane filter, filtrate is ICP-MS test fluid.Each sample do 2 times parallel, do blank assay simultaneously.Manual simulation's saliva employing ISO/TR 10271 standards (Dentistry-Determination of Tarnish and Corrosion of Metals and Alloys[S] .1st Edition. Switzerland, 1993; 3.ISO/TR 10271) prepare: NaCl 0.4g, KCl 0.4g, Na
2hPO
42H
2o 0.78g, Na
2s2H
2o 0.005g, Urea 1.0g, CaCl
22H
2o 0.795g, ultrapure water is diluted to 1000mL, and regulating pH value is 6.8, is kept in 4 ℃ of refrigerators standby.
The drafting of 1.4 typical curves
Get respectively Al, As, B, Ba, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Sb, Se, Sn, Sr, V and Zn single element standard solution 1mL, be placed in 100 mL PET plastics volumetric flasks, 1% HNO
3solution dilution constant volume, being mixed with concentration is the one-level mixed standard solution of 10mg/L; According to using needs, pipetting appropriate one-level mixed standard solution uses artificial simulate saliva to carry out stepwise dilution, obtain Al, As, B, Ba, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Sb, Se, Sn, Sr, V and the Zn standard operation solution of variable concentrations, matching while using.For reducing memory effect, Hg element is mixed with separately mark liquid as stated above, and in the working solution of variant concentration, to add a small amount of concentration be the Au solution of 10mg/L.Simulate artificial saliva as blank, inner mark method ration.
1.5 migration of element quantitative determination results represent
In cigarette filter, each element Special migration represents with X, by formula (1), calculates:
X=
……………….. (1)
In formula: X: each element Special migration (μ g/kg);
2 results and discussions
The isotopic selection of 2.1 element to be measured
In ICP-MS analyte detection process, the signal of object element is often subject to mass spectrum and non-mass spectrum factor is disturbed.In mass spectrum disturbs, isobar interference overlapping and polyatomic molecule ion pair analytic signal is very important, as
204hg couple
204there is isobar interference, argon Diatomic molecular ion ArAr+ couple in Pb+
80there is polyatomic molecule ion interference etc. in Se+.In this research, in order to eliminate mass spectrum in analytic process, to disturb, the isotopic selection of part element to be measured is as follows: selenium element is selected
82se, chromium is selected
53cr, copper is selected
65cu, barium is selected
137ba etc.
Meanwhile, in order to reduce non-mass spectrum, disturb the salt constituents containing in the impact, particularly sample matrices on testing result to make detection signal unstable, it is 10 μ g/L's that this research adds concentration online
45sc,
72ge,
115in,
159tb and
175the mixed standard solution of Lu is as inner mark solution, and carries out inner mark method ration analysis.Experiment discovery, the mensuration of Hg is often subject to the impact of memory effect, in sample introducing, atomizer spray, quarter bend and sample cone, sample transmission etc., all has the residual of Hg, and this research adopts and in Hg standard operation solution, adds a certain amount of Au solution to reduce interference.
The impact of 2.2 different feed liquid control experiment results
Accurately take four parts, 1.0g cigarette filter sample, use respectively 10mL, 20mL, 30mL, 40mL simulation artificial saliva is made testing liquid, by " 1.3 sample preparation " method, tests, and obtains different feed liquid than the concentration of each element in test fluid under condition, the results are shown in Table 2:
Table 2 different feed liquid is the concentration in test fluid (μ g/L) than each element under condition
Note: * represents not reach detection limit.
As known from Table 2, along with the increase of simulation artificial saliva volume, the concentration of each element in test fluid reduces gradually, illustrates that in 1.0g sample, each element can reach most of stripping balance at 10 ~ 40 mL volume simulation artificial salivas.When solid-liquid ratio is 1:10 and 1:20, the relative concentration of each element in test fluid is larger, but exist Partial Elements not reach stripping balance, as Al, B, V, Zn etc., and find in experimentation, part cigarette filter sample cannot, by the complete submergence of 10 mL simulation artificial saliva, may cause migration of element incomplete.When solid-liquid ratio is 1:40, the concentration of Partial Elements in test fluid is less, and some even, near detection limit, will increase the error of experiment.The above analysis, the simulation artificial saliva that this research employing volume is 30mL is as testing liquid.
2.3 impacts of different migration patterns on experimental result
Accurately take ten parts, 1.0g cigarette filter sample, add respectively 30mL simulation artificial saliva, under standing and two kinds of modes of vibration, respectively carry out 30,60,90,120 and 150 minutes migration tests, obtain the concentration of each element in test fluid under different extracting modes, the results are shown in Table 3:
The concentration (μ g/L) of each element in test fluid under the different migration patterns of table 3
Note: * represents not reach detection limit.
As known from Table 3, along with the growth of transit time, the concentration change trend of each element in test fluid tends to be steady after increasing gradually, substantially reaches migration balance when 120 min.In standing and two kinds of migration patterns of vibration, vibration makes object element reach sooner migration balance.The above analysis, this research is preferably vibrated 120 min as transit time condition.
2.4 working curves and detection limit
Take in working solution the contained concentration of element as horizontal ordinate (x), instrument signal response with corresponding in the ratio of mark signal response value be that ordinate (y) carries out linear regression, obtain the regression equation of each element; To blank reagent solution METHOD FOR CONTINUOUS DETERMINATION 11 times, calculate standard deviation, the detection limit of preparation method.The above results is in Table 4:
Table 4 regression equation, related coefficient and detection limit
| Element to be measured | The range of linearity (μ g/L) | Equation of linear regression | Related coefficient | Detection limit (μ g/L) |
| 27Al | 5～1000 | y=0.0752x+0.0432 | 0.9998 | 0.006 |
| 75As | 0.2～25 | y=0.8001x+0.0216 | 0.9996 | 0.014 |
| 11B | 1～200 | y=0.0103x-0.0032 | 0.9997 | 0.008 |
| 137Ba | 0.2～50 | y=0.0354x+0.0706 | 1.0000 | 0.004 |
| 111Cd | 0.2～25 | y=0.2029x-0.0012 | 0.9996 | 0.005 |
| 59Co | 0.2～25 | y=13.9719x+0.1134 | 1.0000 | 0.003 |
| 53Cr | 0.2～25 | y=0.8435x+0.0238 | 0.9997 | 0.009 |
| 63Cu | 0.2～50 | y=10.5013x+1.7287 | 0.9999 | 0.013 |
| 56Fe | 1～100 | y=4.2533x+4.6485 | 0.9995 | 0.021 |
| 202Hg | 0.2～25 | y=0.3601x-0.0237 | 0.9995 | 0.006 |
| 55Mn | 0.2～25 | y=2.5028x+0.4121 | 0.9997 | 0.009 |
| 60Ni | 0.2～25 | y=3.8344x-0.5051 | 0.9995 | 0.004 |
| 208Pb | 0.2～10 | y=0.6273x+0.1155 | 0.9999 | 0.005 |
| 121Sb | 0.2～10 | y=0.4325x+0.0055 | 0.9999 | 0.011 |
| 82Se | 0.2～10 | y=0.0378x-0.0098 | 0.9996 | 0.015 |
| 118Sn | 0.2～10 | y=0.3227x+0.0083 | 0.9995 | 0.005 |
| 88Sr | 5～500 | y=2.5024x+0.4061 | 0.9998 | 0.003 |
| 51V | 0.2～10 | y=4.3233x-0.0561 | 0.9999 | 0.004 |
| 66Zn | 0.2～50 | y=1.3377x+0.0411 | 0.9999 | 0.006 |
2.5 recovery and precision
This research discovery, while adopting cigarette filter sample substrate mark-on to carry out recovery test, sample has absorption or reagentia largely to object element, causes recovery test result undesirable (in Table 5, only listing Partial Elements).
Table 5 sample substrate recovery of standard addition test findings
| Element to be measured | Former content (μ g/L) | Addition (μ g/L) | Measure concentration (μ g/L) | The recovery (%) |
| 27Al | 88.16 | 100.00 | 115.32 | 27.2 |
| 75As | 0.21 | 2.00 | 1.57 | 68.0 |
| 111Cd | ND | 2.00 | 0.14 | 7.0 |
| 53Cr | 0.35 | 2.00 | 0.89 | 27.0 |
| 56Fe | 4.51 | 2.00 | 4.77 | 13.0 |
| 55Mn | 6.27 | 2.00 | 7.79 | 76.0 |
| 60Ni | 0.08 | 2.00 | 0.53 | 22.5 |
| 208Pb | ND | 2.00 | 0.26 | 13.0 |
| 66Zn | 0.62 | 2.00 | 1.09 | 23.5 |
For this reason, this research employing reagent blank adds target mode and carries out recovery experiment, and parallel 6 times of each concentration, calculates method precision data, and the above results is in Table 6:
Table 6 recovery and precision result
| Element to be measured | Former content (μ g/L) | Addition (μ g/L) | Measure concentration (μ g/L) | The recovery (%) | R.S.D(%) |
| 27Al | 0.07 | 20.0 | 19.76 | 98.5 | 3.62 |
| 75As | ND | 2.0 | 1.86 | 93.0 | 3.34 |
| 11B | 0.05 | 2.0 | 1.60 | 77.5 | 4.49 |
| 137Ba | 0.01 | 20.0 | 20.94 | 104.7 | 3.77 |
| 111Cd | ND | 2.0 | 1.89 | 94.5 | 6.13 |
| 59Co | ND | 2.0 | 2.06 | 103.0 | 3.09 |
| 53Cr | ND | 2.0 | 1.89 | 94.5 | 5.01 |
| 63Cu | ND | 2.0 | 1.62 | 81.0 | 2.98 |
| 56Fe | 0.19 | 20.0 | 22.07 | 109.4 | 3.91 |
| 202Hg | ND | 2.0 | 1.54 | 77.0 | 4.96 |
| 55Mn | 0.05 | 2.0 | 1.67 | 81.0 | 3.25 |
| 60Ni | 0.05 | 2.0 | 1.87 | 91.0 | 4.10 |
| 208Pb | ND | 2.0 | 1.77 | 88.5 | 3.02 |
| 121Sb | ND | 2.0 | 2.08 | 104.0 | 3.13 |
| 82Se | ND | 2.0 | 1.43 | 71.5 | 4.25 |
| 118Sn | ND | 2.0 | 1.57 | 78.5 | 3.06 |
| 88Sr | 0.22 | 20.0 | 22.51 | 111.5 | 2.56 |
| 51V | 0.01 | 2.0 | 1.93 | 96.0 | 3.14 |
| 66Zn | ND | 2.0 | 1.90 | 95.0 | 3.11 |
Embodiment 2 sample analysis
The method of setting up according to embodiment 1 has carried out analyzing mensuration to 3 kinds of cigarette filter samples, and concrete steps are as follows:
(1) take the prefabricated cigarette filter sample of getting ready of 1.0g, be accurate to 0.001g, be placed in the 50mL polyethylene terephthalate plastics volumetric bottle with spiral cover;
(2) in the described volumetric bottle of step (1), add manual simulation's saliva that sample quality and manual simulation's saliva volume ratio are 1:30, screw bottle cap;
(3) plastics volumetric bottle is placed in to the standing or vibration certain hour of the water bath chader of 37 ± 1 ℃, obtains the specific dissolution fluid of sample;
(4) dissolution fluid, through 0.45 μ m water membrane filter, obtains test solution;
(5) adopt icp ms (ICP-MS) to measure the Special migration of multiple element in test solution.
Described multiple element comprises one or more in aluminium (Al), arsenic (As), boron (B), barium (Ba), cadmium (Cd), cobalt (Co), chromium (Cr), copper (Cu), iron (Fe), mercury (Hg), manganese (Mn), nickel (Ni), plumbous (Pb), antimony (Sb), selenium (Se), tin (Sn), strontium (Sr), vanadium (V) and zinc (Zn).
The described prefabricated cigarette filter sample of getting ready is finished cigarettes filter tip, and the length of filter tip is 0.2 ~ 1.5cm, and its preparation method is for radially to cut in cross section apart from contact jaw 0.2 ~ 1.5cm place, filter tip oral cavity.
The described water bath chader time standing or vibration is 120 minutes.Preferred oscillation treatment mode, speed is 60r/min.
Described inductively coupled plasma mass spectrometry is quantitatively for adding online internal standard method, working curve to take concentration as horizontal ordinate, and element to be measured is that linear recurrence of ordinate drawn with the response ratio of corresponding internal standard element.
In described element correspondence to be measured, mark is respectively Al:
45sc, As:
72ge, B:
45sc, Ba:
159tb, Cd:
115in, Co:
72ge, Cr:
72ge, Cu:
72ge, Fe:
72ge, Hg:
175lu, Mn:
72ge, Ni:+Ge, Pb:
175lu, Sb:
115in, Se:
72ge, Sn:
115in, Sr:
72ge, V:
45sc and Zn:
72ge, in each, target concentration is 10 μ g/L.
Each element migration amount under given conditions the results are shown in Table 7:
Table 7 sample determination result (unit: μ g/kg)
| Element to be measured | 1# | 2# | 3# |
| 27Al | 13099.06 | 2309.23 | 3454.66 |
| 75As | 8.81 | 4.49 | 1.67 |
| 11B | 725.83 | 674.00 | 903.89 |
| 137Ba | 228.31 | 402.42 | 264.29 |
| 111Cd | ND | ND | ND |
| 59Co | 1.02 | 0.49 | 1.40 |
| 53Cr | 66.44 | 9.23 | 2.64 |
| 63Cu | 20.61 | 12.45 | 21.17 |
| 56Fe | 627.45 | 130.24 | 101.49 |
| 202Hg | 0.26 | 0.15 | ND |
| 55Mn | 158.46 | 197.20 | 162.25 |
| 60Ni | 76.21 | 3.44 | 4.40 |
| 208Pb | ND | ND | ND |
| 121Sb | 0.81 | 1.44 | 1.43 |
| 82Se | ND | ND | ND |
| 118Sn | 2.02 | 1.62 | 1.47 |
| 88Sr | 815.07 | 2062.36 | 1042.60 |
| 51V | 4.23 | 24.29 | 16.41 |
| 66Zn | 12.60 | ND | 17.68 |
Claims (9)
1. an assay method for various heavy Special migration in cigarette filter, is characterized in that, comprises the following steps:
S1. testing sample is packed in volumetric bottle, add manual simulation's saliva, volumetric bottle is placed in to tepidarium and shakes, obtain sample dissolution fluid;
S2. the sample dissolution fluid of step S1 gained is filtered, obtain solution to be measured;
S3. by the solution to be measured of step S2 gained, by internal standard method, coordinate the wherein Special migration of multiple element of inductively coupled plasma mass spectrometry quantitative measurement.
2. the assay method of various heavy Special migration in cigarette filter according to claim 1, it is characterized in that, described multiple element is in Al, As, B, Ba, Cd, Co, Cr, Cu, Fe, Hg, Mn, Ni, Pb, Sb, Se, Sn, Sr, V or Zn two kinds and two or more.
3. the assay method of various heavy Special migration in cigarette filter according to claim 2, is characterized in that, the interior mark that described multiple element is corresponding is respectively: Al:
45sc, As:
72ge, B:
45sc, Ba:
159tb, Cd:
115in, Co:
72ge, Cr:
72ge, Cu:
72ge, Fe:
72ge, Hg:
175lu, Mn:
72ge, Ni:
72ge, Pb:
175lu, Sb:
115in, Se:
72ge, Sn:
115in, Sr:
72ge, V:
45sc and Zn:
72ge.
4. the assay method of various heavy Special migration in cigarette filter according to claim 1, is characterized in that, the inner mark solution of described internal standard method contains
45sc,
72ge,
115in,
159tb,
175lu element, described interior target concentration is 10 μ g/L.
5. the assay method of various heavy Special migration in cigarette filter according to claim 1, is characterized in that, the quality of testing sample and the volume ratio of manual simulation's saliva described in step S1 are 1:10～1:40.
6. the assay method of various heavy Special migration in cigarette filter according to claim 5, is characterized in that, the quality of testing sample and the volume ratio of manual simulation's saliva described in step S1 are 1:30～1:40.
7. the assay method of various heavy Special migration in cigarette filter according to claim 1, is characterized in that the running parameter of described inductively coupled plasma mass spectrometry: cooling gas flow 14.3 L/min; Assisted gas flow 0.8 L/min; Carrier gas flux 1.08 L/min; Spray chamber temperature: 2.0 ℃; Peristaltic pump gathers revolution: 0.1 rps, and sample promotes revolution: 0.5 rps; RF power 1500 W; Sampling depth: 8.0mm.
8. the assay method of various heavy Special migration in cigarette filter according to claim 1, is characterized in that, the water temperature of the tepidarium described in step S1 is 36 ~ 38 ℃, and the speed of described concussion is 60r/min, and the time of concussion is 90 ~ 120 minutes.
9. the assay method of various heavy Special migration in cigarette filter according to claim 1, is characterized in that, the volumetric bottle described in step S1 is 50mL polyethylene terephthalate plastics volumetric bottles.
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| CN108535141A (en) * | 2018-05-16 | 2018-09-14 | 云南中烟工业有限责任公司 | The detection device and detection method of Rosa Damascana ingredient the amount of migration in a kind of filter stick |
| CN109613103A (en) * | 2018-12-14 | 2019-04-12 | 广州广电计量检测股份有限公司 | The detection method of 11 kinds of migration of element amounts in a kind of stainless steel food containers |
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| CN115586238A (en) * | 2022-09-27 | 2023-01-10 | 首钢京唐钢铁联合有限责任公司 | Metal element migration detection method for tin plate |
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| CN105424538A (en) * | 2015-11-05 | 2016-03-23 | 江苏中烟工业有限责任公司 | Method for measuring total non-volatile migration amount in cigarette tipping paper |
| CN105424538B (en) * | 2015-11-05 | 2018-12-25 | 江苏中烟工业有限责任公司 | Method for measuring total non-volatile migration amount in cigarette tipping paper |
| CN107894414A (en) * | 2017-10-25 | 2018-04-10 | 上海烟草集团有限责任公司 | The assay method of heavy metal element burst size in a kind of buccal cigarette |
| CN107894414B (en) * | 2017-10-25 | 2020-04-14 | 上海烟草集团有限责任公司 | Method for determining release amount of heavy metal elements in buccal cigarette |
| CN108535142A (en) * | 2018-05-16 | 2018-09-14 | 云南中烟工业有限责任公司 | A kind of detection method of the Peppermint essential oil ingredient the amount of migration of special flavoring filter stick |
| CN108535141A (en) * | 2018-05-16 | 2018-09-14 | 云南中烟工业有限责任公司 | The detection device and detection method of Rosa Damascana ingredient the amount of migration in a kind of filter stick |
| CN109613103A (en) * | 2018-12-14 | 2019-04-12 | 广州广电计量检测股份有限公司 | The detection method of 11 kinds of migration of element amounts in a kind of stainless steel food containers |
| CN110988098A (en) * | 2019-11-19 | 2020-04-10 | 甘肃烟草工业有限责任公司 | Method for measuring various heavy metals in water-based adhesive for cigarettes after direct dilution |
| CN115586238A (en) * | 2022-09-27 | 2023-01-10 | 首钢京唐钢铁联合有限责任公司 | Metal element migration detection method for tin plate |
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