CN105136931A - Method for determining polyaromatic hydrocarbons in smokeless tobacco product by utilization of on-line solid phase extraction high performance liquid chromatography - Google Patents
Method for determining polyaromatic hydrocarbons in smokeless tobacco product by utilization of on-line solid phase extraction high performance liquid chromatography Download PDFInfo
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Abstract
Provided is a method for determining polyaromatic hydrocarbons in a smokeless tobacco product by utilization of on-line solid phase extraction high performance liquid chromatography. Polyaromatic hydrocarbons comprise the following 13 species: naphthalene, 1-methylnaphthalene, 2-methylnaphthalene, fluorene, phenanthrene, anthracene, fluoranthene, benzo(a)anthracene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, dibenzo(a,h)anthracene, and benzo(g,h,i)perylene. The method is characterized in that a triangular flask loaded with cyclohexane is employed to extract polyaromatic hydrocarbons in a smokeless tobacco product, and the content of polyaromatic hydrocarbons in the smokeless tobacco product is analyzed and determined by utilization of on-line solid phase extraction high performance liquid chromatography. The method is advantageous in that the method is employed to detect a content of polyaromatic hydrocarbons in a smokeless tobacco product, the method is rapid and effective, the pre-treatment is simple, the average relative standard deviation is less than 5%, and the average recovery rate of each index is from 83.6%-104.1%. The method has characteristics of rapidness, accuracy, high sensitivity and good repeatability.
Description
Technical field
The invention belongs to the physical and chemical inspection technical field of smoke-free tobacco product, relate to the determination techniques of palycyclic aromatic in smoke-free tobacco product specifically.
Background technology
Along with the enforcement of all the more strict smoking-control, smoke-free tobacco product is becoming a kind of important tobacco consumption product.But it is also less to the research of the objectionable constituent wherein contained.Palycyclic aromatic cigarette smoke research in by extensive concern, and thought human carcinogen's material (l class) by international cancer research institution (IARC) or for questionable person's body carcinogenic components (2B class), be therefore necessary to analyze and research to the palycyclic aromatic in smoke-free tobacco product.Benzo [a] pyrene (BaP) is the composition that in palycyclic aromatic (PAHs), carcinogenic activity is the strongest, and Accurate Determining BaP is significant for cigarette Evaluation of Harmfulness.At present, the BaP analytical approach of report has fluorescence spectrophotometry, vapor-phase chromatography, gas chromatography/mass spectrometry (GC/MS) coupling method, paper chromatography and high performance liquid chromatography etc. both at home and abroad.Domestic tobacco business generally adopts the GC/MS method of the exploitations such as the summer skilful tinkling of pieces of jade to detect BaP in cigarette mainstream flue gas.But, the method be sample after solvent extraction, also need solid phase extraction column to purify, concentrated, just can carry out GC/MS analysis, both expend comparatively multi-solvent, easily caused environmental pollution again; The ethanol that Zhang Junsong etc. set up and ether mixed extractant solvent, neutral alumina column chromatography purifies, and the method for high effective liquid chromatography for measuring is also comparatively loaded down with trivial details.
summary of the invention:
Object of the present invention is intended to overcome prior art defect, a kind of method using palycyclic aromatic in on-line solid phase extraction high-performance liquid chromatogram determination smoke-free tobacco product is provided, the present invention adopts on-line solid phase extraction purification efficient liquid phase chromatographic analysis to establish the analytical approach of the palycyclic aromatic in smoke-free tobacco product, while improving detection efficiency, greatly reduce the use of pre-treatment organic reagent, reduce the pollution to environment.
The object of the invention is to be achieved through the following technical solutions:
A kind of method of palycyclic aromatic in on-line solid phase extraction high-performance liquid chromatogram determination smoke-free tobacco product, described palycyclic aromatic is following 13 kinds: naphthalene, 1-methylnaphthalene, 2-methylnaphthalene, fluorenes, phenanthrene, anthracene, fluoranthene, benzo (a) anthracene, benzo (b) fluoranthene, benzo (k) fluoranthene, benzo (a) pyrene, dibenzo (a, h) anthracene, benzo (g, h, i) perylene, comprises following concrete determination step
The preparation of a, sample: take 1g smoke-free tobacco product and put into 100mL conical flask, then 10-15mL cyclohexane is added, ultrasonic extraction 40min, then leave standstill to room temperature, getting supernatant 0.22 μm of polyethersulfone millipore filter is filtered in 2mL chromatogram bottle, carries out on-line solid phase extraction efficient liquid phase chromatographic analysis;
B, prepared by standard working solution: preparation has the methanol solution containing 13 kinds of palycyclic aromatics of concentration gradient as hybrid standard working solution, concrete compound method is as follows: accurately take the 1-methylnaphthalene of 10mg and 2-methylnaphthalene respectively in the volumetric flask of 10mL, be accurate to 0.1mg, use methanol constant volume as one-level storing solution respectively, get 1-methylnaphthalene, 2-methylnaphthalene methanol solution and 11 Polycyclic Aromatic Hydrocarbon Mixtures are mixed with mixed sample solution, with methanol dilution, be mixed with the hybrid standard stock solution that 13 palycyclic aromatic components are 1 μ g/mL, get appropriate hybrid standard stock solution respectively, with methyl alcohol and constant volume, obtain palycyclic aromatic concentration of component and be respectively 0.0001, 0.001, 0.005, 0.01, 6 hybrid standard working solutions of 0.05 and 0.1 μ g/mL, the term of validity is 30 days.Standard solution is placed in Refrigerator store, under being placed in normal temperature, can use after reaching normal temperature when taking.
C, on-line solid phase extraction high-performance liquid chromatogram determination: on-line solid phase extraction high performance liquid chromatography is joined fluorescence detector and detected standard working solution and sample treatment liquid, in-line purification and the separation condition of on-line solid phase extraction high performance liquid chromatography are as follows:
On-line solid phase extraction (OnlineSPE) enriching column: AcclaimPA2 (50mm × 4.6mm, 3 μm);
Mobile phase: pure water and acetonitrile, sampling volume 100 μ L;
Compartment analysis post: HypersilGreenPAH (150mm × 3mm, 3 μm);
Mobile phase is pure water and acetonitrile; On-line preconcentration post and analytical column gradient as shown in table 1;
Column temperature: 30 DEG C;
Detecting device: fluorescence detector, fluorescence excitation and emission wavelength as shown in table 2.
Table 1 is for on-line solid phase extraction and the gradient be separated
Fluoroscopic examination maximum excitation/the emission wavelength of each polycyclic aromatic hydrocarbon compounds of table 2
Compared with prior art instant invention overcomes the deficiency of prior art sample treatment, optimize instrument testing conditions, the present invention has following effect:
(1) sample pre-treatments is simple: adopting the present invention to measure palycyclic aromatic in smoke-free tobacco product does not need pre-treatment to purify, and directly goes up high performance liquid chromatography in-line purification;
(2) object is detected many: adopt the present invention can measure 13 kinds of palycyclic aromatics in smoke-free tobacco product;
(3) the present invention has accurate, the highly sensitive and reproducible advantage of operation, and the content that energy is quick, efficient, environmental protection ground detects palycyclic aromatic in smoke-free tobacco product.
1. the typical curve of the inventive method and detectability:
With naphthalene, 1-methylnaphthalene, 2-methylnaphthalene, fluorenes, phenanthrene, anthracene, fluoranthene, benzo (a) anthracene, benzo (b) fluoranthene, benzo (k) fluoranthene, benzo (a) pyrene, dibenzo (a; H) anthracene and benzo (g; H; I) perylene is Testing index, the Working Standard Solution of preparation 13 kinds of palycyclic aromatics, analyze through on-line solid phase extraction high liquid chromatography, with object chromatographic peak area, regretional analysis is carried out to its respective concentration, obtain typical curve and regression equation, related coefficient, utilize least concentration mark liquid signal to noise ratio (S/N ratio) for calculate during S/N=3 detectability (
lOD) (table 3).As shown in Table 3, the chromatographic condition adopted makes 13 kinds of palycyclic aromatic chromatographic peaks all be separated better, and all have good correlativity (
r>0.98), detection limit is between 0.13 ~ 2.56ng/g.
The typical curve of table 3 smoke-free tobacco product carbonyls and detection limit
Note: 1. detection limit calculates with 3 times of signal to noise ratio (S/N ratio)s (S/N=3).
2. the repeatability of the inventive method and recovery of standard addition:
The recovery of table 4 method and repeatability (
n=5)
| Sequence number | Palycyclic aromatic | The recovery (%) | RSD（%） |
| 1 | Naphthalene | 104.1 | 2.6 |
| 2 | 1-methylnaphthalene | 88.3 | 3.6 |
| 3 | 2-methylnaphthalene | 100.1 | 4.9 |
| 4 | Fluorenes | 98.1 | 3.5 |
| 5 | Luxuriant and rich with fragrance | 89.8 | 2.3 |
| 6 | Anthracene | 94.4 | 2.6 |
| 7 | Fluoranthene | 96.8 | 2.8 |
| 8 | Benzo (a) anthracene | 83.6 | 3.8 |
| 9 | Benzo (b) fluoranthene | 95.5 | 2.8 |
| 10 | Benzo (k) fluoranthene | 95.5 | 2.2 |
| 11 | Benzo (a) pyrene | 99.3 | 2.5 |
| 12 | Dibenzo (a, h) anthracene | 95.3 | 3.3 |
| 13 | Benzo (g, h, i) perylene | 95.0 | 2.6 |
Sample is carried out to the standard solution recovery of standard addition test of high, medium and low variable concentrations level, each sample measures 5 times respectively, calculate average relative standard's deviation of measured value after the average recovery rate of palycyclic aromatic in this method various smoke-free tobacco product and mark-on, the results are shown in Table 4.As can be seen from Table 4, in 3 mark-on levels, the method is utilized to detect the average recovery rate of palycyclic aromatic in smoke-free tobacco product between 83.6% ~ 104.1%.The mean relative deviation of sample tests is less than 5%; Illustrate that the recovery of this law is higher, repeatability better.
Accompanying drawing explanation
Fig. 1 assay method process flow diagram of the present invention,
Fig. 2 on-line solid phase extraction schematic diagram.
Embodiment
The present invention is described further below in conjunction with specific embodiment:
example 1:
1. reagent and instrument:
Standard items: the mixed sample (concentration of 11 palycyclic aromatics is 2.0mg/ml) of 11 palycyclic aromatics, is dissolved in methylene chloride, comprises: naphthalene; fluorenes, luxuriant and rich with fragrance, anthracene; fluoranthene, benzo (a) anthracene, benzo (b) fluoranthene; benzo (k) fluoranthene, benzo (a) pyrene, dibenzo (a; h) anthracene, benzo (g, h; i) perylene, An Pu company); 1-methylnaphthalene, 2-methylnaphthalene, all purchased from AccuStandard company;
Reagent: acetonitrile (chromatographically pure, Duksanpurechemicals company of Korea S), cyclohexane (chromatographically pure, JTBaker company of the U.S.).Experimental water is the made deionized water of Milli-Q pure water system.
Instrument: ThermoUltiMate3000 high performance liquid chromatograph, the online degasser of configuration Hexamermis spp, two ternary gradient pump, automatic sampler (band large volume sample injection assembly), column oven (are with a 2p-6p transfer valve, i.e. 2 six-way valves), fluorescence detector (FLD), chameleon Chromatography Manager software Chromeleon7.2 (U.S. match Mo Feishier company).
2. sample preparation:
Take 1g smoke-free tobacco product and put into 100mL conical flask, then add 11mL cyclohexane, ultrasonic extraction 40min, then leave standstill to room temperature, getting supernatant 0.22 μm of polyethersulfone millipore filter is filtered in 2mL chromatogram bottle, carries out on-line solid phase extraction efficient liquid phase chromatographic analysis.
3. standard working solution preparation:
Accurately take the 1-methylnaphthalene of 10mg and 2-methylnaphthalene respectively in the volumetric flask of 10mL, be accurate to 0.1mg, use methanol constant volume as one-level storing solution respectively, get appropriate 1-methylnaphthalene, 2-methylnaphthalene methanol solution and 11 Polycyclic Aromatic Hydrocarbon Mixtures and be mixed with mixed sample solution, with methanol dilution, be mixed with the hybrid standard stock solution that 13 palycyclic aromatic components are 1ug/mL.Get appropriate hybrid standard stock solution respectively, with methyl alcohol and constant volume, obtain 6 hybrid standard working solutions that palycyclic aromatic concentration of component is respectively 0.0001,0.001,0.005,0.01,0.05 and 0.1 μ g/mL, the term of validity is 30 days.Standard solution is placed in Refrigerator store, under being placed in normal temperature, can use after reaching normal temperature when taking.
4. assay method:
With the chromatographic peak area of target palycyclic aromatic, regretional analysis is carried out to its respective concentration, obtain typical curve.The sample prepared is measured; record the chromatographic peak area detecting target palycyclic aromatic; substitute into typical curve, obtain the naphthalene in sample, 1-methylnaphthalene, 2-methylnaphthalene, fluorenes, phenanthrene, anthracene, fluoranthene, benzo (a) anthracene, benzo (b) fluoranthene, benzo (k) fluoranthene, benzo (a) pyrene, dibenzo (a respectively; H) anthracene and benzo (g; H; I) the content of perylene, the results are shown in Table 5.
Palycyclic aromatic testing result in table 5 smoke-free tobacco product
| Compound | Content (ng/g) |
| Naphthalene | 19.8 |
| 1-methylnaphthalene | 8.0 |
| 2-methylnaphthalene | 4.2 |
| Fluorenes | 7.8 |
| Luxuriant and rich with fragrance | 15.6 |
| Anthracene | 66.0 |
| Fluoranthene | 32.0 |
| Benzo (a) anthracene | N.D. |
| Benzo (b) fluoranthene | N.D. |
| Benzo (k) fluoranthene | N.D. |
| Benzo (a) pyrene | N.D. |
| Dibenzo (a, h) anthracene | N.D. |
| Benzo (g, h, i) perylene | 11.9 |
Note: N.D. represents and does not detect.
The in-line purification of on-line solid phase extraction high performance liquid chromatography be separated testing conditions as listed by summary of the invention above.
Example 2:
Concrete steps as described in Example 1, select another sample B, record the content of palycyclic aromatic in smoke-free tobacco product in table 6.
Palycyclic aromatic testing result in table 6 smoke-free tobacco product
| Compound | Content (ng/g) |
| Naphthalene | 17.8 |
| 1-methylnaphthalene | 48.2 |
| 2-methylnaphthalene | 71.0 |
| Fluorenes | 11.8 |
| Luxuriant and rich with fragrance | N.D. |
| Anthracene | 143.9 |
| Fluoranthene | N.D. |
| Benzo (a) anthracene | 33.7 |
| Benzo (b) fluoranthene | N.D. |
| Benzo (k) fluoranthene | 877.9 |
| Benzo (a) pyrene | N.D. |
| Dibenzo (a, h) anthracene | N.D. |
| Benzo (g, h, i) perylene | N.D. |
Note: N.D. represents and does not detect.
Example 3:
Concrete steps as described in Example 1, select another sample C, record the content of palycyclic aromatic in smoke-free tobacco product in table 7.
Palycyclic aromatic testing result in table 7 smoke-free tobacco product
| Compound | Content (ng/g) |
| Naphthalene | 22.5 |
| 1-methylnaphthalene | 158.9 |
| 2-methylnaphthalene | 0.3 |
| Fluorenes | 20.8 |
| Luxuriant and rich with fragrance | N.D. |
| Anthracene | 210.5 |
| Fluoranthene | 3.8 |
| Benzo (a) anthracene | 38.9 |
| Benzo (b) fluoranthene | 9.0 |
| Benzo (k) fluoranthene | 814.5 |
| Benzo (a) pyrene | N.D. |
| Dibenzo (a, h) anthracene | N.D. |
| Benzo (g, h, i) perylene | 4.9 |
Note: N.D. represents and does not detect.
example 4:
Concrete steps as described in Example 1, select another sample D, record the content of palycyclic aromatic in smoke-free tobacco product in table 8.
Palycyclic aromatic testing result in table 8 smoke-free tobacco product
| Compound | Content (ng/g) |
| Naphthalene | 20.1 |
| 1-methylnaphthalene | N.D. |
| 2-methylnaphthalene | 4.2 |
| Fluorenes | 6.8 |
| Luxuriant and rich with fragrance | 0.2 |
| Anthracene | 173.5 |
| Fluoranthene | N.D. |
| Benzo (a) anthracene | N.D. |
| Benzo (b) fluoranthene | N.D. |
| Benzo (k) fluoranthene | N.D. |
| Benzo (a) pyrene | N.D. |
| Dibenzo (a, h) anthracene | N.D. |
| Benzo (g, h, i) perylene | N.D. |
Note: N.D. represents and does not detect.
Claims (3)
1. the method for palycyclic aromatic in an on-line solid phase extraction high-performance liquid chromatogram determination smoke-free tobacco product, described palycyclic aromatic is following 13 kinds: naphthalene, 1-methylnaphthalene, 2-methylnaphthalene, fluorenes, phenanthrene, anthracene, fluoranthene, benzo (a) anthracene, benzo (b) fluoranthene, benzo (k) fluoranthene, benzo (a) pyrene, dibenzo (a, h) anthracene, benzo (g, h, i) perylene, is characterized in that: comprise following concrete determination step
The preparation of a, sample: take 1g smoke-free tobacco product and put into 100mL conical flask, then 10-15mL cyclohexane is added, ultrasonic extraction 40min, then leave standstill to room temperature, getting supernatant 0.22 μm of polyethersulfone millipore filter is filtered in 2mL chromatogram bottle, carries out on-line solid phase extraction efficient liquid phase chromatographic analysis;
Prepared by b, standard working solution: preparation has the methanol solution containing 13 kinds of palycyclic aromatics of concentration gradient as hybrid standard working solution;
C, on-line solid phase extraction high-performance liquid chromatogram determination: on-line solid phase extraction high performance liquid chromatography is joined fluorescence detector and detected standard working solution and sample treatment liquid, and the condition of on-line solid phase extraction high performance liquid chromatography is as follows:
On-line preconcentration post: AcclaimPA2, specification 50mm × 4.6mm, 3 μm,
Mobile phase: pure water and acetonitrile, sampling volume 100 μ L;
Compartment analysis post: HypersilGreenPAH, specification 150mm × 3mm, 3 μm;
Mobile phase is pure water and acetonitrile, gradient elution.
2. the method for palycyclic aromatic in on-line solid phase extraction high-performance liquid chromatogram determination smoke-free tobacco product according to claim 1, it is characterized in that: the concrete compound method of standard working solution is as follows: accurately take the 1-methylnaphthalene of 10mg and 2-methylnaphthalene respectively in the volumetric flask of 10mL, be accurate to 0.1mg, use methanol constant volume as one-level storing solution respectively, get 1-methylnaphthalene, 2-methylnaphthalene methanol solution and 11 Polycyclic Aromatic Hydrocarbon Mixtures are mixed with mixed sample solution, with methanol dilution, be mixed with the hybrid standard stock solution that 13 palycyclic aromatic components are 1 μ g/mL, get appropriate hybrid standard stock solution respectively, with methyl alcohol and constant volume, obtain palycyclic aromatic concentration of component and be respectively 0.0001, 0.001, 0.005, 0.01, 6 hybrid standard working solutions of 0.05 and 0.1 μ g/mL.
3. the method for palycyclic aromatic in on-line solid phase extraction high-performance liquid chromatogram determination smoke-free tobacco product according to claim 1, is characterized in that: on-line preconcentration post and analytical column gradient as shown in the table;
Table 1 is for on-line solid phase extraction and the gradient be separated
。
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