CN103399118B - Method used for detecting caffeic acid content in cigarette sidestream smoke by high performance liquid chromatography-tandem mass spectrum - Google Patents
Method used for detecting caffeic acid content in cigarette sidestream smoke by high performance liquid chromatography-tandem mass spectrum Download PDFInfo
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Abstract
The invention discloses a method used for detecting caffeic acid content in cigarette sidestream smoke by high performance liquid chromatography-tandem mass spectrum. The method comprises following steps: (1) total particulate matters in smoke are collected by a fishtail cover and a filter disc; (2) the filter disc is placed in a methanol solution containing internal standard substances for extraction so as to obtain an extract; (3) the extract is filtered, and then is detected by a high performance liquid chromatography-tandem mass spectrometer; and (4) the content of caffeic acid is quantitatively analyzed by internal standard method. According to the method used for detecting caffeic acid content in cigarette sidestream smoke by high performance liquid chromatography-tandem mass spectrum, pre-treatment is simple, separating effect is excellent, qualitative analysis is accurate, sample analysis time is short, and detection sensitivity is high.
Description
Technical field
The present invention relates to tobacco and technical field of chemistry, particularly relate to the assay method of caffeinic high performance liquid chromatography-tandem mass in a kind of cigarette side-stream smoke.
Background technology
Caffeic acid on a molecular scale, this compound can cause the fracture of DNA double chain structure in testing in vitro, on a cellular level, this compound is found also may cause chromosome aberration and sister chromatid exchange, international cancer research institution of the World Health Organization (WHO) (IARC) is classified as 2B class carcinogen, is subject to extensive concern about the impact of this compound on health always.Calendar year 2001 Hoffmann and its researcher have carried out amendment and supplement to the objectionable constituent inventory of 1991, one of 69 kinds of objectionable constituent caffeic acid being classified as cigarette smoke, within 2002, Rodgman and Green sums up the objectionable constituent reported in flue gas, also caffeic acid is classified as one of 149 kinds of cigarette smoke objectionable constituent.
In the traditional Chinese medicine materials such as dandelion, caulis lonicerae, the achene of Siberian cocklebur, the report of the assay method of caffeic acid content is more, main employing be high performance liquid chromatography, UV-detector carries out quantitative test, and the detection method of high performance liquid chromatography-tandem mass also has a small amount of report.(the Journal of Analytical Science such as Xu Gaoyan, 2006,22 (5): 567-569.) by the ultrasonic extraction of water-soluble Rosmarinus officinalis extract methyl alcohol, directly adopt high performance liquid chromatography-tandem mass to measure wherein caffeinic content after extracting liquid filtering film, detecting of method for building up is limited to 5ng/mL.Caffeic acid is also the one of tobacco leaf polyphenol substance, in tobacco leaf, also have certain content distribution.Peng Youyuan etc. (assay laboratory, 2006,25 (2): 92-96.) are by tobacco leaf drying, and pulverize, adopts capillary electrophoresis with electrochemical detection Simultaneously test containing the content of caffeic acid at interior several polyhydric phenol after the ultrasonic extraction of ethanol water.Zhu Ruizhi etc. (assay laboratory, 2009,28 (10): 108-112.) also report the method adopting high performance liquid chromatography-tandem mass to measure caffeic acid content in tobacco leaf.
Mensuration about phenolic compounds in cigarette smoke mainly concentrates on several phenolic compounds of showing great attention to such as o-benzenediol, p-benzenediol, phenol, o-cresols, m-cresol.As Chinese patent 200910066382.7 discloses a kind of method measuring several major phenolic compound such as o-benzenediol in cigarette mainstream flue gas, p-benzenediol, phenol, o-cresols, m-cresol, this assay method utilizes the major phenolic compound in glass fiber filter trapping cigarette mainstream flue gas, filter with after acetic acid aqueous solution extraction, adopt two-dimensional HPLC separation Cascade System fluorescence detector to detect, measure the content of this several phenolic compound in cigarette mainstream flue gas.(the tobacco science and technology such as Xie Fuwei, 2004,5:6-10.) adopt 1% acetum extraction smoke's total particulate matter, extract directly carries out HPLC analysis after filtering with microporous membrane, fluorescence detector is adopted to detect, to establish in cigarette main flow and side-stream smoke adjacent, p-benzenediol, phenol, adjacent, the detection method of 7 kinds of phenols components such as p-Cresol.
But, cigarette in combustion, there occurs the multiple physical and chemical reactions such as distillation, destructive distillation, pyrolysis, synthesis, condensation, form a large amount of Xinshenghua compound, and whether distribute in cigarette side-stream smoke about caffeic acid, the pertinent literature report how to measure is less, so far, not yet finds to have any patent and the bibliographical information that adopt high performance liquid chromatography-tandem mass instrument to measure caffeic acid content in cigarette side-stream smoke both at home and abroad.And smoke components is very complicated, matrix interference is serious, and the content of caffeic acid in flue gas is lower again, and it is on the knees of the gods that can the detection method of the phenolic compound in smoke set up be applicable to caffeinic mensuration in flue gas.
Environmental tobacco smoke (ETS) is important indoor pollutant, and what involuntary smoker experienced is exactly this kind of material, and the side-stream smoke of cigarette is the main source of environmental tobacco smoke, accounts for 85% of environmental tobacco smoke.Along with the public is to the growing interest of smoking and health problem, in cigarette, objectionable constituent burst size becomes the focus that people pay close attention to gradually, at present, relevant law has been formulated in some countries and regions such as Canada, requires that production of cigarettes business provides the burst size of harmful constituents in cigarette flue gas.In view of this, set up the detection method of caffeic acid content in a kind of cigarette side-stream smoke, in research cigarette smoking process, the regularity of distribution important in inhibiting of caffeic acid in cigarette main flow and side-stream smoke, is also conducive to the size of objective evaluation cigarette harmfulness.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of method that high performance liquid chromatography-tandem mass measures caffeic acid content in cigarette side-stream smoke, namely provide that a kind of pre-treatment is simple, good separating effect, qualitative accurately, the assay method of caffeinic high performance liquid chromatography-tandem mass in sample analysis time is short, detection sensitivity is high cigarette side-stream smoke.
The technical solution used in the present invention is to provide a kind of method that high performance liquid chromatography-tandem mass measures caffeic acid content in cigarette side-stream smoke, and the method comprises the steps:
(1) with the TPM in fish tail cover and filter disc trapping flue gas;
(2) filter disc is placed in methanol solution to carry out extracting to obtain extract;
(3) extracted by filtration liquid, measures filtrate with high performance liquid chromatography/mass spectrometer;
(4) inner mark method ration analysis is adopted to draw caffeic acid content.
Preferably, the trapping described in step (1) refer to by cigarette to be measured GB/T16447-2004 tobacco and tobacco product regulate and test Atmospheric Condition in the environmental baseline balance 48h that specifies; Determine and mark the stub length of smoking cigarette, the side-stream smoke suction method specified in mensuration according to T/N in cigarette side-stream smoke in YC/T185, the suction flow regulating effluent smoking machine is 3000mL/min, aspirate 5 cigarette, with fish tail cover and glass fiber filter trapping side-stream smoke TPM.
Preferably, step (2) described methanol solution contains internal standard compound.
Preferably, described internal standard compound is salicylic acid.
Preferably, step (3) described filtration refers to that extract is through organic phase membrane filtration.
Preferably, the described high performance liquid chromatograph condition of step (3) is: C18 reversed-phase column, detected temperatures 30 DEG C, sample size 1 μ L ~ 10 μ L, flow velocity 0.2 ~ 0.4mL/min, gradient elution; Mobile phase A is deionized water, and Mobile phase B is methyl alcohol; Described mass spectrometer condition is: ionization mode is electron spray, and scan pattern is negative ion, atomization gas 25 ~ 35psi, gas curtain gas 10psi, auxiliary heating gas 20 ~ 30psi, collision gas 5psi, ion gun injection electric 5000 ~ 5800V, ion source temperature 350 ~ 400 DEG C.
Preferably, the condition of described gradient elution is as follows:
| Time/min | Flow velocity/mL ﹒ min-1 | Mobile phase A % | Mobile phase B % |
| 0 | 0.2 | 80 | 20 |
| 5 | 0.2 | 80 | 20 |
| 6 | 0.4 | 0 | 100 |
| 16 | 0.2 | 0 | 100 |
| 17 | 0.2 | 80 | 20 |
| 27 | 0.2 | 80 | 20 |
Preferably, described mass spectrometer detects caffeinic detected parameters and is: quota ion is 179.0/134.9 to m/z, and qualitative ion pair m/z is 179.0/106.8, and residence time is 200ms, and impact energy is-22.0V.
Preferably, described mass spectrometer detects salicylic detected parameters and is: quota ion is 136.9/93.1 to m/z, and qualitative ion pair m/z is 136.9/64.5, and residence time is 200ms, and impact energy is-25.0V.
Preferably, the described quantitative test of step (4) adopts external standard method, the caffeic acid series standard working solution of preparation 10ng/mL ~ 300ng/mL, concentration gradient more than 5 and being uniformly distributed, contained by standard solution at different levels, the concentration of internal standard compound is 90-110ng/mL, high performance liquid chromatography-tandem mass instrument is utilized to detect standard solution, using the ratio of the caffeic acid peak area that obtains and interior mark peak area as ordinate, caffeic acid concentration and internal standard compound concentration ratio are as horizontal ordinate, drawing standard curve also obtains regression equation, then under the same conditions sample is detected, the peak area ratio of the caffeic acid obtained and internal standard compound is substituted in equation, caffeinic content can be calculated.
The invention has the beneficial effects as follows to propose first adopts high performance liquid chromatography-tandem mass to measure caffeinic method in cigarette side-stream smoke.Method of the present invention adopts multiple-reaction monitoring pattern (MRM) to carry out quantitative and qualitative analysis, effectively can improve the sensitivity of qualitative accuracy and method, the recovery of standard addition of sample is between 91.42 ~ 103.75%, repeatability is not more than 5%, the quantitative limit of cigarette sample can reach 1.17ng/mL, is applicable to caffeinic batch in all kinds of cigarette side-stream smoke and measures.
Accompanying drawing explanation
Fig. 1 is the chromatogram of standard solution;
Fig. 2 is caffeinic chromatogram in embodiment 1 side-stream smoke.
Embodiment
Below in conjunction with drawings and Examples, the present invention is illustrated further.
Instrument, reagent and material:
The triple quadrupole rods tandem mass spectrometry instrument of U.S.'s Applied Biosystems company API3200 type, be furnished with electric spray ion source and Analyst system software, Agilent company 1200 of U.S. type high performance liquid chromatograph, band automatic sampler, Germany Borgwaldt RM20H type smoking machine, electronic balance (sensibility reciprocal 0.1mg), convolution adjustable mechanical oscillator.
Methyl alcohol is chromatographically pure, deionized water; Caffeic acid standard items, Chun Du≤98%.
Reagent and solution preparation:
The preparation of standard reserving solution: accurately take the urethanes of about 25mg in 25mL beaker, be accurate to 0.0001g, add about 10mL methyl alcohol, be transferred in 25mL volumetric flask after dissolving completely, swing with a small amount of methyl alcohol and wash beaker 3 ~ 5 times, cleansing solution is transferred in volumetric flask in the lump, then by methanol constant volume to scale.
The preparation of primary standard solution: the Standard Stock solutions accurately pipetting 1.0mL with transfer pipet in 50mL volumetric flask, by methanol constant volume to scale.
The preparation of interior mark storing solution: accurately take the salicylic acid of about 20mg in 50mL beaker, be accurate to 0.0001g, adding after about 20mL methyl alcohol dissolves completely is transferred in 100mL volumetric flask, swing with a small amount of methyl alcohol and wash beaker 3 ~ 5 times, cleansing solution is transferred in volumetric flask in the lump, is then settled to scale with acetonitrile.
The preparation of one-level inner mark solution: accurately pipette in 2.00mL with transfer pipet and mark stock solution in 100mL volumetric flask, by methanol constant volume to scale.
The preparation of secondary inner mark solution: the Standard Stock solutions accurately pipetting 5.00mL with transfer pipet in 250mL volumetric flask, by methanol constant volume to scale.
The preparation of series standard working solution: accurately pipette the primary standard solution of 0.025mL, 0.05mL, 0.25mL, 0.5mL, 1.0mL and 1.50mL secondary inner mark solution respectively in 50mL volumetric flask, by methanol constant volume to scale, obtain the standard solution of 5 different series concentration, high performance liquid chromatography-tandem mass is adopted to be measured by this series standard working solution successively, production standard curve.Regression equation is obtained according to typical curve.
Embodiment 1
High performance liquid chromatography-tandem mass measures a method for caffeic acid content in cigarette side-stream smoke, and the method comprises the steps:
1. the collection of sample: by certain brand cigarette to be measured balance 48 hours under (22 ± 1) DEG C, relative humidity (60 ± 3) % condition, then determine and mark the stub length of smoking cigarette, according to side-stream smoke suction method in YC/T185, the suction flow regulating effluent smoking machine is 3000mL/min, aspirate 5 cigarette, with fish tail cover and glass fiber filter trapping side-stream smoke TPM.
2. filter disc extraction and sample determination: filter disc is placed in 100mL conical flask, add the methanol solution of 10mL containing 120 nanograms (ng) internal standard compound of having an appointment wherein, and divide 2 ~ 3 clean fish hoods with 10mL methyl alcohol, cleaning fluid is transferred in conical flask in the lump, and conical flask is placed in 30min that oscillator vibrates; Extract adopts high performance liquid chromatography/mass spectrometer (LC-MS/MS) to measure after organic phase membrane filtration.
3. adopt high performance liquid chromatography-tandem mass to measure:
High performance liquid chromatograph condition is: C18 reversed-phase column, detected temperatures 30 DEG C, sample size 1 μ L ~ 10 μ L, flow velocity 0.2 ~ 0.4mL/min, and first alcohol and water carries out gradient elution as mobile phase; Mobile phase A is deionized water, and Mobile phase B is methyl alcohol; Condition of gradient elution is as shown in table 1:
Table 1 condition of gradient elution
| Time/min | Flow velocity/mL ﹒ min -1 | Mobile phase A % | Mobile phase B % |
| 0 | 0.2 | 80 | 20 |
| 5 | 0.2 | 80 | 20 |
| 6 | 0.4 | 0 | 100 |
| 16 | 0.2 | 0 | 100 |
| 17 | 0.2 | 80 | 20 |
| 27 | 0.2 | 80 | 20 |
Mass spectrometer condition is: ionization mode is electron spray; Scan pattern is negative ion; Atomization gas 25 ~ 35psi; Gas curtain gas 10psi; Auxiliary heating gas 20 ~ 30psi; Collision gas 5psi; Ion gun injection electric 5000 ~ 5800V; Ion source temperature 350 ~ 450 DEG C; Detecting caffeinic detected parameters is: quota ion is 179.0/134.9 to m/z, and qualitative ion pair m/z is 179.0/106.8, and residence time is 200ms, and impact energy is-22.0V; Detecting salicylic detected parameters is: quota ion is 136.9/93.1 to m/z, and qualitative ion pair m/z is 136.9/64.5, and residence time is 200ms, and impact energy is-25.0V.
4. calculate caffeinic content in cigarette smoke:
Be calculated as follows and often propped up caffeinic content in cigarette side-stream smoke:
In formula:
M-often prop up the caffeinic content of cigarette, unit is nanogram/(ng/cig);
A-caffeic acid peak area;
As-salicylic peak area;
B-drawn by equation of linear regression;
Mark content in ms-sample solution, unit is nanogram (ng);
A-drawn by equation of linear regression;
N-cigarette quantity, unit is for propping up.
Twice mensuration is carried out to sample, then using the mean value of twice mensuration as final measurement result, result is accurate to 0.01ng/cig.Relative deviation between twice measurement result is within 10%, and the mean value of mensuration is in table 2.
Embodiment 2
High performance liquid chromatography-tandem mass measures a method for caffeic acid content in cigarette side-stream smoke, and the method comprises the steps:
1. the collection of sample: by certain brand cigarette balance 48 hours under (22 ± 1) DEG C, relative humidity (60 ± 3) % condition, then determine and mark the stub length of smoking cigarette, according to side-stream smoke suction method in YC/T185, the suction flow regulating effluent smoking machine is 3000mL/min, aspirate 5 cigarette, with fish tail cover and glass fiber filter trapping side-stream smoke TPM.
2. filter disc extraction and sample determination: filter disc is placed in 100mL conical flask, add the methanol solution of 10mL containing 120 nanograms (ng) internal standard compound of having an appointment wherein, and divide 2 ~ 3 clean fish hoods with 10mL methyl alcohol, cleaning fluid is transferred in conical flask in the lump, and conical flask is placed in 30min that oscillator vibrates; Extract adopts high performance liquid chromatography/mass spectrometer (LC-MS/MS) to measure after organic phase membrane filtration.
3. adopt high performance liquid chromatography-tandem mass to measure:
High performance liquid chromatograph condition is: C18 reversed-phase column, detected temperatures 30 DEG C, sample size 1 μ L ~ 10 μ L, flow velocity 0.2 ~ 0.4mL/min, and first alcohol and water carries out gradient elution as mobile phase; Mobile phase A is deionized water, and Mobile phase B is methyl alcohol; Condition of gradient elution is as shown in table 1:
Table 1 condition of gradient elution
| Time/min | Flow velocity/mL ﹒ min -1 | Mobile phase A % | Mobile phase B % |
| 0 | 0.2 | 80 | 20 |
| 5 | 0.2 | 80 | 20 |
| 6 | 0.4 | 0 | 100 |
| 16 | 0.2 | 0 | 100 |
| 17 | 0.2 | 80 | 20 |
| 27 | 0.2 | 80 | 20 |
Mass spectrometer condition is: ionization mode is electron spray; Scan pattern is negative ion; Atomization gas 25 ~ 35psi; Gas curtain gas 10psi; Auxiliary heating gas 20 ~ 30psi; Collision gas 5psi; Ion gun injection electric 5000 ~ 5800V; Ion source temperature 350 ~ 450 DEG C; Detecting caffeinic detected parameters is: quota ion is 179.0/134.9 to m/z, and qualitative ion pair m/z is 179.0/106.8, and residence time is 200ms, and impact energy is-22.0V; Detecting salicylic detected parameters is: quota ion is 136.9/93.1 to m/z, and qualitative ion pair m/z is 136.9/64.5, and residence time is 200ms, and impact energy is-25.0V.
4. calculate caffeinic content in cigarette smoke:
Be calculated as follows and often propped up caffeinic content in cigarette side-stream smoke:
In formula:
M-often prop up the caffeinic content of cigarette, unit is nanogram/(ng/cig);
A-caffeic acid peak area;
As-salicylic peak area;
B-drawn by equation of linear regression;
Mark content in ms-sample solution, unit is nanogram (ng);
A-drawn by equation of linear regression;
N-cigarette quantity, unit is for propping up.
Twice mensuration is carried out to sample, then using the mean value of twice mensuration as final measurement result, result is accurate to 0.01ng/cig.Relative deviation between twice measurement result is within 10%, and the mean value of mensuration is in table 2.
Caffeic acid content in the cigarette flow measurement flue gas that table 2 embodiment 1,2 measures
| Cigarette sample | Caffeic acid (ng/cig) |
| Embodiment 1 | 17.39 |
| Embodiment 2 | 14.81 |
Measure 6 times to the sample parallel of embodiment 1, the repeated result obtaining sample is as shown in table 3:
The repeatability of table 3 embodiment 1 measurement result
| Parallel | 1# | 2# | 3# | 4# | 5# | 6# | Mean value | RSD(%) |
| Content (ng/cig) | 16.36 | 17.28 | 15.41 | 15.87 | 16.4 | 17.54 | 16.48 | 4.93 |
Result display in table 3, the relative standard deviation of measurement result is less than 5%, and showing can caffeinic content in Accurate Measurement cigarette side-stream smoke.
Repeat sample introduction 10 times with the standard specimen of least concentration (10.0ng/mL), count standard deviation by the concentration value recorded, detectability (LOD) is tried to achieve with 3 times of standard deviations, this method be quantitatively limited to 1.17ng/mL, show that the sensitivity of method is higher.
The recovery
On the cigarette filter disc of embodiment 1, add the caffeic acid reference material of 66ng, 132ng and 198ng respectively, record the caffeic acid content value under basic, normal, high mark-on three levels, each horizontal parallel measures three times, and mean value is in table 4.The recovery of result presentation method is 91.42 ~ 103.75%, shows that the inventive method has the higher recovery.
Table 4 recovery of standard addition
| Caffeic acid addition ng/cig | Yield ng/cig | Average recovery rate % |
| 22.00 | 20.11 | 91.42 |
| 44.00 | 41.91 | 95.24 |
| 66.00 | 68.47 | 103.75 |
The above embodiment of the present invention is only for example of the present invention is clearly described, the restriction not to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here cannot give exhaustive to all embodiments.Every belong to technical scheme of the present invention the apparent change of extending out or variation be still in the row of protection scope of the present invention.
Claims (4)
1. high performance liquid chromatography-tandem mass measures a method for caffeic acid content in cigarette side-stream smoke, it is characterized in that: comprise the steps:
(1) with the TPM in fish tail cover and filter disc trapping flue gas;
(2) filter disc is placed in methanol solution to carry out extracting to obtain extract;
(3) extracted by filtration liquid, measures filtrate with high performance liquid chromatography/tandem mass spectrometer;
(4) inner mark method ration analysis is adopted to draw caffeic acid content,
Wherein, the described high performance liquid chromatograph condition of step (3) is: C18 reversed-phase column, detected temperatures 30 DEG C, sample size 1 μ L ~ 10 μ L, flow velocity 0.2 ~ 0.4mL/min, gradient elution; Mobile phase A is deionized water, and Mobile phase B is methyl alcohol; Described mass spectrometer condition is: ionization mode is electron spray, and scan pattern is negative ion, atomization gas 25 ~ 35psi, gas curtain gas 10psi, auxiliary heating gas 20 ~ 30psi, collision gas 5psi, ion gun injection electric 5000 ~ 5800V, ion source temperature 350 ~ 400 DEG C;
The condition of described gradient elution is as follows:
Described mass spectrometer detects caffeinic condition: quota ion is 179.0/134.9 to m/z, and qualitative ion pair m/z is 179.0/106.8, and residence time is 200ms, and impact energy is-22.0V;
Described mass spectrometer detects salicylic testing conditions: quota ion is 136.9/93.1 to m/z, and qualitative ion pair m/z is 136.9/64.5, and residence time is 200ms, and impact energy is-25.0V;
Step (2) described methanol solution contains internal standard compound;
Described internal standard compound is salicylic acid.
2. method according to claim 1, is characterized in that: the trapping described in step (1) refer to by cigarette to be measured GB/T 16447-2004 tobacco and tobacco product regulate and test Atmospheric Condition in the environmental baseline balance 48h that specifies; Determine and mark the stub length of smoking cigarette, the side-stream smoke suction method specified in mensuration according to T/N in cigarette side-stream smoke in YC/T 185-2004, the suction flow regulating effluent smoking machine is 3000mL/min, aspirate 5 cigarette, with fish tail cover and glass fiber filter trapping side-stream smoke TPM.
3. method according to claim 1, is characterized in that: step (3) described filtration refers to that extract is through organic phase membrane filtration.
4. method according to claim 1, it is characterized in that: the described quantitative test of step (4) adopts internal standard method, the caffeic acid series standard working solution of preparation 10ng/mL ~ 300ng/mL, concentration gradient more than 5 and being uniformly distributed, contained by standard solution at different levels, the concentration of internal standard compound is 90-110ng/mL, high performance liquid chromatography-tandem mass instrument is utilized to detect standard solution, using the ratio of the caffeic acid peak area that obtains and interior mark peak area as ordinate, caffeic acid concentration and internal standard compound concentration ratio are as horizontal ordinate, drawing standard curve also obtains regression equation, then under the same conditions sample is detected, the peak area ratio of the caffeic acid obtained and internal standard compound is substituted in the regression equation obtained, caffeinic content can be calculated.
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