CN103954707A - Method for analyzing speciation of arsenic elements in smoke of cigarettes - Google Patents
Method for analyzing speciation of arsenic elements in smoke of cigarettes Download PDFInfo
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- CN103954707A CN103954707A CN201410206285.4A CN201410206285A CN103954707A CN 103954707 A CN103954707 A CN 103954707A CN 201410206285 A CN201410206285 A CN 201410206285A CN 103954707 A CN103954707 A CN 103954707A
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Abstract
The invention relates to a method for analyzing the speciation of arsenic elements in smoke of cigarettes. The method is characterized by comprising the steps of capturing arsenic in particulate matter of smoke by virtue of a rotary disc smoking machine with an electrostatic capturing device, extracting arsenic compounds of different speciation in the particulate matter by virtue of a diammonium hydrogen phosphate solution, and quantitatively analyzing the release amount of arsenic elements of different speciation by virtue of an HPLC-ICP-MS (High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometry) technique so as to realize the quantitative analysis on the speciation of the arsenic elements in main stream smoke of the cigarettes. The method has the advantages that a sample pretreatment process is simple, convenient and rapid, the consumption amount of an extraction reagent is little, a separating effect of the speciation of As elements is good, the analytical interference is less, the sensitivity is high, the linearity range is wide, the precision is high, and a technical support is provided for accurately estimating the security risk of the As elements in the main stream smoke of the cigarettes.
Description
Technical field
The present invention relates to tobacco heavy metal objectionable constituent detection technique, specifically the method for arsenic element form in cigarette smoke is measured in a kind of HPLC-ICP-MS coupling, utilizes the burst size that the method can quantitative test different shape arsenic element.
Background technology
Heavy metal is important class objectionable constituent in cigarette mainstream flue gas, because heavy metal element harm exists form closely related with it, its Difference In Toxicity of different shape is very large, as As element, there is number of chemical form, common are As (V), As (III), monomethyl arsenic acid (MMA), dimethyl arsenate (DMA) etc., wherein trivalent arsenic is larger than pentavalent arsenic toxicity, and inorganic arsenic toxicity is greater than organo-arsenic.Therefore, in research cigarette mainstream flue gas, the chemical form of arsenic element aligns that to confirm to know in flue gas arsenic element significant to harm.
Arsenic element morphological analysis adopts liquid chromatography (HPLC) that different shape is separated more, and then adopt atomic fluorescence method (AFS), graphite oven atomic absorption (AAS) or inductively coupled plasma mass spectrometry (ICP-MS) to measure, the morphological analysis of arsenic element at present adopts HPLC-ICP-MS coupling technique more, make full use of exactly the high separating power of HPLC and the high sensitivity of ICP-MS ultimate analysis, the conventional separating column of arsenic element morphological analysis mainly contains anion-exchange column, cation-exchange chromatography post etc.Due to HPLC-ICP-MS for the morphological analysis method of arsenic element have interference less, sensitive height, the feature such as the range of linearity is wide, precision is high and sample pre-treatments is easy and simple to handle, at present in industry widespread uses such as food, water quality, environment, atmosphere, but the morphological analysis of As not yet has correlative study in cigarette smoke.
Summary of the invention
The present invention on the basis of existing analytical approach, has set up As in a kind of cigarette mainstream flue gas (V), As (III), monomethyl arsenic acid (MMA), 4 kinds of morphological analysis assay methods of dimethyl arsenate (DMA) just.For the security risk assessment of As element in accurate evaluation cigarette mainstream flue gas provides technical support.
Fundamental purpose of the present invention is different shape arsenic compound burst size in analysis of cigarette flue gas, thus the harmfulness of arsenic in correct evaluation of flue gas, and set up the method for arsenic element form in a kind of HPLC-ICP-MS coupling technique analysis of cigarette flue gas.The rotating disk smoking machine trapping Smoke Particulate of the present invention with Electrostatic device, in Smoke Particulate, different shape arsenic compound extracts through ammonium dibasic phosphate solution, anion-exchange column for extract (Hamilton PRP-X100) carries out HPLC with ammonium dibasic phosphate solution (pH=6.0) and separates, then carry out arsenic element somatometry of physique with ICP-MS, thereby realize the quantitative test of arsenic element form burst size in cigarette mainstream flue gas.
The object of the invention is to realize by following steps:
The analytical approach of arsenic element form in a kind of cigarette smoke, adopt with the arsenic in the rotating disk smoking machine trapping Smoke Particulate of Electrostatic device, with the arsenic compound of different shape in ammonium dibasic phosphate solution extraction granule phase substance, the burst size of using again HPLC-ICP-MS coupling technique quantitative test different shape arsenic element, concrete steps are as follows:
(1) flue gas trapping: test cigarette is prior to (22 ± 1) DEG C, relative humidity is balance 48h in the environment of (60 ± 5) %, prop up with average resistance to suction ± 49Pa/ and prop up sorting by average quality ± 0.02g/, then according to GB/T16450-2004(or ISO 3308:2000) suction method suction test cigarette, use the rotating disk smoking machine suction 20 test cigarette with Electrostatic device, with Electrostatic device trapping Smoke Particulate;
(2) sample preparation: the Smoke Particulate in Electrostatic device trap tube is rinsed in 50mL triangular flask with 30mL 15mmol/L ammonium dibasic phosphate solution (pH=6.0), vibration 30min, get 5mL extract centrifugal 10min under 10000rpm rotating speed, pipette again supernatant and cross after 0.45 μ m mocromembrane, be stored in brown chromatogram bottle for analyzing;
(3) HPLC-ICP-MS analyzes: it is tuning first to carry out ICP-MS, to ensure that it has higher sensitivity; 50cmPEEK is managed to one end to be connected with HPLC chromatography column outflow end; the other end is connected with the atomizer of ICP-MS; then taking 15 mmoL/L (NH4) 2HPO4(pH=6.0) as mobile phase; its flow velocity is 1.0 mL/min, carries out As (V), As (III), monomethyl arsenic acid (MMA), the 4 kinds of morphological analyses of dimethyl arsenate (DMA) of arsenic element in cigarette mainstream flue gas;
The groundwork condition of HPLC-ICP-MS analytical instrument is as table 1:
Table 1. ICP-MS and HPLC Instrument working parameter
The invention has the advantages that: adopt different As element morphologies in rotating disk smoking machine-Electrostatic method trapping cigarette mainstream flue gas, extraction solvent consumption is few, and sample pre-treatments is easy fast, with 15 mmoL/L (NH4)
2hPO
4mobile phase can be by different As element morphology baseline separation, sample analysis disturbs less, sensitive height, the range of linearity is wide, precision is high, in 10min, can realize whole sample analysis, for the security risk assessment of As element in accurate evaluation cigarette mainstream flue gas provides technical support.
Brief description of the drawings
Fig. 1 is As (V), As (III), monomethyl arsenic acid (MMA), dimethyl arsenate (DMA) chromatogram.
Embodiment
example 1
Pipette respectively a certain amount of As (V), As (III), monomethyl arsenic acid (MMA), dimethyl arsenate (DMA) standard solution is configured to 0.5,1.0,2.0,5.0,10.0 and 20.0 μ g/L and mixes serial standard operation solution (all in As), and then measure with HPLC-ICP-MS, carry out linear regression with concentration and CPS counting, obtain linear equation and related coefficient, carrying out 10 times with least concentration hybrid standard working solution measures, calculate the standard deviation of 4 kinds of form content, using 3 times of standard deviations as detection limit.Result shows method good linearity, detection limit low (the results are shown in Table 1).
4 kinds of arsenic compound working stamndard curves of table 1. and linearly dependent coefficient
| The form of arsenic | Retention time/min | Linear equation | Related coefficient R 2 | Detection limit |
| As（Ⅲ） | 2.25 | y=24773x+2034.4 | 0.9980 | 0.16 |
| DMA | 2.95 | y=27973x+2677.7 | 0.9994 | 0.25 |
| MMA | 4.54 | y=27465x+1275.8 | 0.9998 | 0.24 |
| As（Ⅴ） | 7.22 | y=27373x+3238.0 | 0.9978 | 0.15 |
example 2
According to step (1) screening test cigarette in foregoing invention content, then use with the smoking machine of Electrostatic device and test cigarette according to 20 of GB/T 16450-2004 suctions, with Electrostatic device trapping Smoke Particulate, do mensuration 6 times simultaneously.With 30mL15 mmoL/L (NH
4)
2hPO
4(pH=6.0) granule phase substance in Electrostatic pipe is rinsed in 50mL triangular flask, vibration 30min, get 5mL extract centrifugal 10min under 10000rpm rotating speed, pipetting supernatant crosses after 0.45 μ m mocromembrane again, be stored in brown chromatogram bottle and use in order to analyzing, and then measure with HPLC-ICP-MS, obtain 4 kinds of form burst sizes of As element in cigarette mainstream flue gas, result shows that method precision is all less than 15%(and the results are shown in Table 2).
Table 2. replicate determination result (ng/20 props up)
example 3
According to step (1) sorting Virginian-type cigarette and blended type cigarette in foregoing invention content, then use with the smoking machine of Electrostatic device and test cigarette according to 20 of GB/T 16450-2004 suctions, with Electrostatic device trapping Smoke Particulate, do replicate determination simultaneously.With containing the mixed target 30mL15 mmoL/L (NH of a certain amount of 4 kinds of forms
4)
2hPO
4(pH=6.0) granule phase substance in Electrostatic pipe is rinsed in 50mL triangular flask, vibration 30min, get 5mL extract centrifugal 10min under 10000rpm rotating speed, pipetting supernatant crosses after 0.45 μ m mocromembrane again, be stored in brown chromatogram bottle and use in order to analyzing, and then measure with HPLC-ICP-MS, calculating recovery of standard addition, result shows method sample recovery of standard addition good (the results are shown in Table 3).
Table 3. recovery of standard addition
example 4
According to 6 kinds of domestic and international cigarette samples of step (1) sorting in foregoing invention content, then use with the smoking machine of Electrostatic device and test cigarette according to 20 of GB/T 16450-2004 suctions, with Electrostatic device trapping Smoke Particulate, do mensuration 6 times simultaneously.With 30mL15 mmoL/L (NH
4)
2hPO
4(pH=6.0) granule phase substance in Electrostatic pipe is rinsed in 50mL triangular flask, vibration 30min, get 5mL extract centrifugal 10min under 10000rpm rotating speed, pipetting supernatant crosses after 0.45 μ m mocromembrane again, be stored in brown chromatogram bottle and use in order to analyzing, and then measure with HPLC-ICP-MS, obtain 4 kinds of form burst sizes of As element in cigarette mainstream flue gas, the results are shown in Table 4.
Different shape As Element release amount (ng/20cig) in 6 kinds of domestic and international cigarette smokes of table 4.
Claims (3)
1. the analytical approach of arsenic element form in a cigarette smoke, it is characterized in that: adopt with the arsenic in the rotating disk smoking machine trapping Smoke Particulate of Electrostatic device, with the arsenic compound of different shape in ammonium dibasic phosphate solution extraction granule phase substance, the burst size of using again HPLC-ICP-MS coupling technique quantitative test different shape arsenic element, concrete steps are as follows:
(1) flue gas trapping: use the rotating disk smoking machine suction 20 test cigarette with Electrostatic device, with Electrostatic device trapping Smoke Particulate;
(2) sample preparation: the Smoke Particulate in Electrostatic device trap tube is rinsed in 50mL triangular flask with 30mL 15mmol/L ammonium dibasic phosphate solution (pH=6.0), vibration 30min, get 5mL extract centrifugal 10min under 10000rpm rotating speed, pipette again supernatant and cross after 0.45 μ m mocromembrane, be stored in brown chromatogram bottle for analyzing;
(3) HPLC-ICP-MS analyzes: it is tuning first to carry out ICP-MS, to ensure that it has higher sensitivity; 50cmPEEK is managed to one end to be connected with HPLC chromatography column outflow end, the other end is connected with the atomizer of ICP-MS, then taking 15 mmoL/L (NH4) 2HPO4(pH=6.0) as mobile phase, its flow velocity is 1.0 mL/min, carries out As (V), As (III), monomethyl arsenic acid (MMA), the 4 kinds of morphological analyses of dimethyl arsenate (DMA) of arsenic element in cigarette mainstream flue gas.
2. according to the analytical approach of arsenic element form in the cigarette smoke described in claim 1, it is characterized in that: in flue gas trapping process, test cigarette is prior to (22 ± 1) DEG C, relative humidity is balance 48h in the environment of (60 ± 5) %, prop up with average resistance to suction ± 49Pa/ and prop up sorting by average quality ± 0.02g/, then according to GB/T16450-2004(or ISO 3308:2000) suction method suction test cigarette.
3. according to the analytical approach of arsenic element form in the cigarette smoke described in claim 1, it is characterized in that: the groundwork condition of HPLC-ICP-MS analytical instrument is as table 1:
Table 1. ICP-MS and HPLC Instrument working parameter
。
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104237369A (en) * | 2014-09-25 | 2014-12-24 | 上海烟草集团有限责任公司 | Method for separation and determination of arsenic elements in different forms in tobacco and tobacco products |
| CN104266888A (en) * | 2014-09-25 | 2015-01-07 | 上海烟草集团有限责任公司 | Method for separating and measuring arsenic elements with different forms in main stream smoke of cigarettes |
| CN104614436A (en) * | 2015-01-21 | 2015-05-13 | 上海烟草集团有限责任公司 | Method for detecting content of arsenic in main stream smoke of cigarette |
| CN105606721A (en) * | 2015-12-11 | 2016-05-25 | 济南市环境保护科学研究院 | Method for separation and determination of arsenic in PM2.5 |
| CN105866231A (en) * | 2015-01-19 | 2016-08-17 | 上海市食品药品检验所 | Methods for determining total amount arsenic and valence arsenic content in biological tissues and organs |
| CN108120785A (en) * | 2018-01-03 | 2018-06-05 | 江苏中宜金大分析检测有限公司 | The method of abio-arsenic residues and resolution centrifugal device in a kind of measure rice flour |
| CN110007036A (en) * | 2019-05-17 | 2019-07-12 | 河北省地质环境监测院 | The detection of different arsenic morphologies in environment water based on HPLC-ICP-MS joint technology |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104237369A (en) * | 2014-09-25 | 2014-12-24 | 上海烟草集团有限责任公司 | Method for separation and determination of arsenic elements in different forms in tobacco and tobacco products |
| CN104266888A (en) * | 2014-09-25 | 2015-01-07 | 上海烟草集团有限责任公司 | Method for separating and measuring arsenic elements with different forms in main stream smoke of cigarettes |
| CN105866231A (en) * | 2015-01-19 | 2016-08-17 | 上海市食品药品检验所 | Methods for determining total amount arsenic and valence arsenic content in biological tissues and organs |
| CN105866231B (en) * | 2015-01-19 | 2019-07-30 | 上海市食品药品检验所 | The method for measuring total amount arsenic and valence state arsenic content in living organism tissue and internal organs |
| CN104614436A (en) * | 2015-01-21 | 2015-05-13 | 上海烟草集团有限责任公司 | Method for detecting content of arsenic in main stream smoke of cigarette |
| CN105606721A (en) * | 2015-12-11 | 2016-05-25 | 济南市环境保护科学研究院 | Method for separation and determination of arsenic in PM2.5 |
| CN108120785A (en) * | 2018-01-03 | 2018-06-05 | 江苏中宜金大分析检测有限公司 | The method of abio-arsenic residues and resolution centrifugal device in a kind of measure rice flour |
| CN108120785B (en) * | 2018-01-03 | 2020-05-12 | 江苏中宜金大分析检测有限公司 | Method for determining inorganic arsenic content in rice flour and digestion centrifugal device |
| CN110007036A (en) * | 2019-05-17 | 2019-07-12 | 河北省地质环境监测院 | The detection of different arsenic morphologies in environment water based on HPLC-ICP-MS joint technology |
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Application publication date: 20140730 |