CN102788858B - Method for LC-MS/MS (Liquid Chromatography-Mass Spectrometry/ Mass Spectrometry) jointly detecting ethyl carbamate content in cigarette main stream smoke - Google Patents
Method for LC-MS/MS (Liquid Chromatography-Mass Spectrometry/ Mass Spectrometry) jointly detecting ethyl carbamate content in cigarette main stream smoke Download PDFInfo
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Abstract
The invention discloses a method for LC-MS/MS (Liquid Chromatography-Mass Spectrometry/ Mass Spectrometry) jointly detecting ethyl carbamate content in cigarette main stream smoke. The method comprises: utilizing a Cambridge filter sheet to collect the ethyl carbamate in the cigarette main stream smoke; using ethanol to extract the filter sheet; concentrating and diluting the extract liquor, carrying out solid phase extraction and columella purification, eluting by using dichloromethane; using a high efficient liquid chromatography/tandem mass spectrometer to detect the eluant; and adopting an internal standard method to obtain the ethyl carbamate content in the cigarette main stream smoke. The method has simple preliminary treatment, good separation effect, accurate nature determination, short sample analysis time and high detection sensitivity.
Description
Technical field
The invention belongs to tobacco and technical field of chemistry, relate to particularly a kind of method that high performance liquid chromatography-tandem mass coupling detects ammonia of main stream smoke of cigarette base ethyl formate content.
Background technology
Urethanes (Ethyl carbamate, EC claims again urethane) be extensively present in various fermented foods, it is a kind of potential carcinogen, can cause lung cancer, lymph cancer, the various diseases such as liver cancer and cutaneum carcinoma, international cancer research institution of the World Health Organization (WHO) (IARC) is classified as 2A class carcinogenic substance, " have reason expect cause cancer material " list is also listed urethanes in the plan of American National toxicity, the food additives joint specialist council of FAO (Food and Agriculture Organization of the United Nation)/World Health Organization (WHO) (FAO/WHO) (JECFA) the 64th meeting suggestion, healthy in order to ensure human body, should reduce as far as possible the content of urethanes in fermented beverage and food.
1991, in 43 kinds of harmful ingredients in flue gas inventories that Hoffmann announces, urethanes is listed, calendar year 2001 Hoffmann and its researcher have carried out amendment and supplement to the objectionable constituent inventory of 1991, will classify one of 69 kinds of objectionable constituent as by urethanes, Rodgman in 2002 and Green sum up the objectionable constituent of having reported in flue gas, also urethanes is classified as to one of 149 kinds of cigarette smoke objectionable constituent, U.S. food and FAD (FDA) are classified the urethanes in tobacco as carcinogen (CA) and reproductive system/growth Toxic (RDT), but so far, not yet find to have any patent and the bibliographical information that adopt high performance liquid chromatography-tandem mass instrument to measure ammonia of main stream smoke of cigarette base ethyl formate content both at home and abroad.
Chinese patent 200910099554.0 open " a kind of method that detects ethyl carbamate in yellow wine ", to carry out derivative reaction-utilize colleges and universities' liquid chromatograph to carry out component separated by decompression distillation-mix with hydrochloric acid and 9-hydroxyl ton solution for the method, then adopts external standard method to calculate the content of urethanes.The method can effectively detect ethyl carbamate in yellow wine.In addition Chinese patent 201110339615.3 and Chinese patent 201110288339.2 disclose respectively a kind of in Spirit and beverage the detection method of urethanes.
Along with the growing interest of the public to smoking and health problem, the content of urethanes of cigarette smoke objectionable constituent-especially-the become focal issue that people pay close attention to, but, drinks composition is comparatively simple, and matrix interference is less, and the complicated component of flue gas, that identifies out just has nearly 5000 kinds, and urethanes is trace components in flue gas, and the interference of all the other compositions is comparatively serious, above-mentioned patented method is not also suitable for the content that detects ammonia in flue gas base ethyl formate.Therefore, set up a kind of detection method of ammonia of main stream smoke of cigarette base ethyl formate content, and the method also needs fast, accurately, good separating effect, highly sensitive be a current urgent task of tobacco business, for research with evaluate smoking and health problem also has very important and urgent meaning.
Summary of the invention
The object of this invention is to provide that a kind of pre-treatment is simple, good separating effect, qualitative accurately, sample analysis time is short, detection sensitivity is high high performance liquid chromatography-tandem mass coupling detects the method for ammonia of main stream smoke of cigarette base ethyl formate content.
A kind of LC-MS/MS coupling detects the method for ammonia of main stream smoke of cigarette base ethyl formate content, comprise the following steps: utilize the urethanes in cambridge filter trapping cigarette mainstream flue gas, use ethanol extraction filter disc, extract is concentrated, dilution purifies by solid phase extraction column, use methylene chloride wash-out, eluent detects with high performance liquid chromatography/tandem mass spectrometer, adopts internal standard method to obtain the content of ammonia of main stream smoke of cigarette base ethyl formate.
Further, the internal standard compound adopting in described internal standard method is deuterated urethanes.
Further, described solid phase extraction column is fixing is hydrophilic-lipophilic balance resin mutually.For example, HLB pillar (the SDVB multipolymer of modification).
Further, described high performance liquid chromatograph condition is: C18 reversed-phase column, and 30 ℃ of detected temperatures, sample size 1 μ L～10 μ L, flow velocity 0.2～0.4mL/min, acetonitrile and water carry out gradient elution as mobile phase; Described mass spectrometer condition is: ionization mode is electron spray; Scan pattern is positive ion; Atomization gas 35～45psi; Gas curtain gas 10psi; Auxiliary heating gas 45～55psi; Collision gas 5psi; Ion gun injection electric 5000～5800V; 350～400 ℃ of ion source temperatures.
Further, described high performance liquid chromatograph mobile phase A is the mixed solution of the acetonitrile/water containing 0.1% acetic acid with V:V=90:10, and Mobile phase B is acetonitrile; Gradient elution program is:
| Time/min | Flow velocity/mL ﹒ min -1 | Mobile phase A | Mobile phase B |
| 0 | 0.2 | 100 | 0 |
| 6 | 0.2 | 100 | 0 |
| 12 | 0.4 | 0 | 100 |
| 27 | 0.2 | 100 | 0 |
| 40 | 0.2 | 100 | 0 |
LC-MS/MS coupling detects a method for ammonia of main stream smoke of cigarette base ethyl formate content, comprises the following steps:
1) by cigarette to be measured balance 48h under the tobacco of GB/T16447-2004 regulation and the Atmospheric Condition of tobacco product adjusting and test;
2) adopt smoking machine to aspirate under standard aspiration condition, utilize the urethanes in cambridge filter trapping cigarette mainstream flue gas, the ethanolic solution extraction filter disc that adopts 40mL to contain 320 nanograms (ng) internal standard compound,, be extracted liquid;
3) pipette 10～20ml extract in concentrated bottle, evaporation and concentration, to 0.5mL left and right, adds 10mL distilled water in concentrate, the percent by volume of ethanol is down to below 10%, dilution is transferred on solid phase extraction column and is purified, adopt methylene chloride to carry out wash-out, collect eluent;
4) eluent is concentrated into dry rear with adopting high performance liquid chromatography/mass spectrometer to measure after about 1ml mobile phase dissolving:
Described high performance liquid chromatograph condition is: C18 reversed-phase column, and 30 ℃ of detected temperatures, sample size 1 μ L～10 μ L, flow velocity 0.2～0.4mL/min, acetonitrile and water carry out gradient elution as mobile phase;
Described mass spectrometer condition is: ionization mode is electron spray; Scan pattern is positive ion; Atomization gas 35～45psi; Gas curtain gas 10psi; Auxiliary heating gas 45～55psi; Collision gas 5psi; Ion gun injection electric 5000～5800V; 350～400 ℃ of ion source temperatures; Described atomization gas, gas curtain gas, auxiliary heating gas, collision gas are high pure nitrogen;
5) the urethanes series standard working solution of preparation 10ng/mL～600ng/mL, 5 of concentration gradients are above and be uniformly distributed, and the concentration of the internal standard compound that standard solution at different levels contain is 300ng/mL left and right; Utilize high performance liquid chromatography-tandem mass instrument to detect standard solution, using the ratio of the urethanes peak area obtaining and interior mark peak area as ordinate, urethane ester concentration and interior mark concentration ratio are as horizontal ordinate, drawing standard curve also obtains regression equation, then under the same conditions sample is detected, by in the urethanes obtaining and interior target peak area ratio substitution equation, can calculate the content of urethanes.
Further, step 2), internal standard compound is deuterated urethanes.
Further, concentrated in step 3) is extract to be adopted under 50 ℃ of conditions nitrogen blow concentrating instrument to be concentrated into dry.
Further, in step 3) solid phase extraction column fixing be hydrophilic-lipophilic balance resin mutually.
Described C18 reversed-phase column specification is 150mm * 2.1mm, 5 μ m.
Further, described high performance liquid chromatograph mobile phase A is the mixed solution of the acetonitrile/water containing 0.1% acetic acid with V:V=90:10, and Mobile phase B is acetonitrile; Gradient elution program is:
| Time/min | Flow velocity/mL ﹒ min-1 | Mobile phase A | Mobile phase B |
| 0 | 0.2 | 100 | 0 |
| 6 | 0.2 | 100 | 0 |
| 12 | 0.4 | 0 | 100 |
| 27 | 0.2 | 100 | 0 |
| 40 | 0.2 | 100 | 0 |
Further, the quota ion of described urethanes is 90.0/62.1 to m/z, and qualitative ion pair m/z is 90.0/44.0, and residence time is 200ms, and impact energy is 14.0V.
Further, the quota ion of described deuterated urethanes is 95.0/63.2 to m/z, and qualitative ion pair m/z is 95.0/44.2, and residence time is 200ms, and impact energy is 25.0.
The invention has the advantages that:
The present invention has proposed to adopt high performance liquid chromatography-tandem mass to measure the method for ammonia of main stream smoke of cigarette base ethyl formate first; Method of the present invention is quick, accurate, highly sensitive, the recovery of standard addition of sample is between 93.71%～99.83%, sample repeatability is not more than 5%, and the qualitative limit of cigarette sample can reach 0.39ng/mL, is applicable to the mensuration of all kinds of ammonia of main stream smoke of cigarette base ethyl formates.
Accompanying drawing explanation
Fig. 1 is the chromatogram of standard solution;
Fig. 2 is the chromatogram that standard solution contains internal standard compound;
Fig. 3 is the chromatogram of certain ammonia of main stream smoke of cigarette base ethyl formate (containing internal standard compound).
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is further described.
Instrument of the present invention and reagent, material
The triple quadrupole rods tandem mass spectrometry instrument of the U.S.'s API3200 of Applied Biosystems company type, be furnished with electric spray ion source and Analyst system software, U.S. Agilent company 1200 type high performance liquid chromatographs, band automatic sampler, Germany Borgwaldt RM20H type smoking machine, the RapidVap N2 of U.S. Labconco company concentrating instrument, electronic balance (sensibility reciprocal 0.1mg), convolution adjustable mechanical oscillator U.S. Supelco solid-phase extraction device (VISPREPTM DL), the hydrophilic lipophilic solid phase extraction column of the HLB of U.S. Waters company (500mg/6mL).
Acetonitrile, acetic acid are chromatographically pure, and ethanol, methylene chloride are that analysis is pure, deionized water; Urethanes standard items, Chun Du≤98%, deuterated urethanes internal standard compound standard items, Chun Du≤99%.
Reagent and solution preparation
The preparation of standard reserving solution: accurately take the urethanes of about 10mg in 50mL beaker, be accurate to 0.0001g, after adding about 20mL acetonitrile to dissolve completely, be transferred in 100mL volumetric flask, with a small amount of acetonitrile, swing and wash beaker 3～5 times, cleansing solution is transferred in volumetric flask in the lump, then with acetonitrile, is settled to scale.
The preparation of primary standard solution: the standard inventory solution that accurately pipettes 2.50mL with transfer pipet, in 250mL volumetric flask, is settled to scale with acetonitrile.
The preparation of interior mark storing solution: accurately take the deuterated urethanes of about 20mg in 50mL beaker, be accurate to 0.0001g, after adding about 20mL acetonitrile to dissolve completely, be transferred in 100mL volumetric flask, with a small amount of acetonitrile, swing and wash beaker 3～5 times, cleansing solution is transferred in volumetric flask in the lump, then with acetonitrile, is settled to scale.
The preparation of one-level inner mark solution: the interior mark stock solution that accurately pipettes 4.00mL with transfer pipet, in 100mL volumetric flask, is settled to scale with acetonitrile.
The preparation of secondary inner mark solution: the standard inventory solution that accurately pipettes 10.00mL with transfer pipet, in 250mL volumetric flask, is settled to scale with acetonitrile.
The preparation of series standard working solution: accurately pipette respectively the primary standard solution of 0.25mL, 0.50mL, 1.00mL, 3.75mL, 7.50mL, 15.00mL, 30.00mL and 1.00 secondary inner mark solutions in 50mL volumetric flask, with acetonitrile, be settled to scale, obtain the standard solution of 7 different series concentration, adopt high performance liquid chromatography-tandem mass successively this series standard working solution to be measured, production standard curve.
Fig. 1 is the chromatogram of standard solution; Fig. 2 is the chromatogram that standard solution contains internal standard compound; Fig. 3 is the chromatogram of certain ammonia of main stream smoke of cigarette base ethyl formate (containing internal standard compound).
Embodiment 1
LC-MS/MS coupling detects a method for ammonia of main stream smoke of cigarette base ethyl formate content, comprises the following steps:
Sample collection: by cigarette balance 48 hours under (22 ± 1) ℃, relative humidity (60 ± 3) % condition, then according to tobacco business YC/T29-1996 standard defined terms, carry out cigarette smoking, adopt glass fiber filter trapping main flume, 20 cigarette of every group of suction.
Filter disc extraction: have the filter disc of 20 cigarette smoke granule phase substances to put into 150mL conical flask trapping, add 40mL ethanol and 1.00mL secondary inner mark solution, be placed on velocity-modulated oscillator and vibrate 30 minutes.
Sample pre-treatments: measure the above-mentioned extract of about 10mL in concentrated bottle, adopt nitrogen to blow concentrating instrument and be concentrated into 0.5mL left and right, add the dilution of 10mL deionized water in concentrate, mix rear to be clean.Above-mentioned dilution is transferred on hydrophilic lipophilic solid phase extraction column (HLB) pillar that activation, balance are good, efflux discards and drains pillar 3min, then use 4mL methylene chloride wash-out, after collection eluent is concentrated into and does, adopt 1.0ml mobile phase to dissolve post analysis.
High performance liquid chromatograph condition is:
Liquid-phase chromatographic column: Waters X-Bridge C182.1 * 150mm, 5 μ m; Sample size: 10 μ L; Flow velocity: 0.2～0.4mL/min; Column temperature: 30 ℃; Mobile phase A: the acetonitrile/water that contains 0.1% acetic acid (V:V=90:10) mixed solution; Mobile phase B: acetonitrile; Gradient elution program is as shown in table 1:
Table 1 gradient elution program
| Time/min | Flow velocity/mL ﹒ min-1 | Mobile phase A | Mobile phase B |
| 0 | 0.2 | 100 | 0 |
| 6 | 0.2 | 100 | 0 |
| 12 | 0.4 | 0 | 100 |
| 27 | 0.2 | 100 | 0 |
| 40 | 0.2 | 100 | 0 |
The conditional parameter of tandem mass spectrometer is:
Ionization mode: electron spray (ESI); Scan pattern: positive ion; Atomizer: 40psi; Gas curtain gas: 10psi; Auxiliary heating gas: 45psi; Collision gas: 5psi; Ion injection electric: 5500v; Ion source temperature: 350 ℃; The mass spectrophotometry parameter of urethanes and internal standard compound thereof is as shown in table 2:
The mass spectrophotometry parameter of table 2 compound
| Compound | Quota ion is to m/z | Qualitative ion pair m/z | Residence time ms | Impact energy V |
| Urethanes | 90.0/62.1 | 90.0/44.0 | 200 | 14.0 |
| Deuterated-urethanes | 95.0/63.2 | 95.0/44.2 | 200 | 25.0 |
Utilize high performance liquid chromatography-tandem mass instrument to detect series standard solution, using the ratio of the urethanes peak area obtaining and interior mark peak area as horizontal ordinate, urethane ester concentration and interior mark concentration ratio are as ordinate, drawing standard curve also obtains regression equation, regression equation is that y=0.967x+0.00408(linearly dependent coefficient is 1.0), then under the same conditions sample is detected, by in the urethanes obtaining and interior target peak area ratio substitution equation, calculate according to the following formula the content of urethanes.
In formula:
The content of m-every cigarette urethanes, unit is nanogram/(ng/cig);
A-urethanes peak area;
A
s-deuterated urethanes peak area;
B-drawn by equation of linear regression;
M
smark content in-sample solution, unit is nanogram (ng);
A-drawn by equation of linear regression;
N-cigarette quantity, unit is for propping up.
The precision of the inventive method and detectability
A certain standard model is carried out to 6 times continuously and measure, the peak area ratio precision of urethanes is investigated, result is as shown in table 3:
The precision of table 3 method
| Sample introduction number of times 1 | Retention time min3.06 | Peak area 9128.4 |
| 2 | 3.09 | 8915.7 |
| 3 | 3.07 | 9108.3 |
| 4 | 3.08 | 9194.9 |
| 5 | 3.06 | 9118.5 |
| 6 | 3.02 | 9034.7 |
| Mean value | 3.06 | 9083.42 |
| RSD | 0.74% | 1.07 |
In table, result shows, no matter is retention time or peak area, and relative standard deviation is all less than 5%, show can Accurate Measurement ammonia of main stream smoke of cigarette base ethyl formate content.
Standard specimen with least concentration (5.0ng/mL) repeats sample introduction 10 times, by the concentration value recording, counts standard deviation, and detectability (LOD) is tried to achieve with 3 times of standard deviations, and the detection of this method is limited to 0.39ng/mL, shows that the sensitivity of method is higher.
The recovery of the inventive method
Urethanes reference material to adding respectively 232ng, 464ng and 696ng on certain brand cigarette filter disc, records the sodium cyclohexylsulfamate content value under three levels of basic, normal, high mark-on, and each horizontal parallel is measured three times, and mean value is in Table 4.The recovery of result presentation method is 93.71%～99.83%, shows that method has the higher recovery.
The recovery of standard addition of table 4 method
| EC addition ng/cig | Yield ng/cig | Average recovery rate % |
| 11.6 | 10.87 | 93.71 |
| 23.2 | 23.15 | 99.78 |
| 46.4 | 46.32 | 99.83 |
Sample determination
Adopt the inventive method to measure the content of the urethanes in two cigarette sample main flumes, measurement result is as shown in the table:
| Cigarette sample | Urethanes (ng/cig) |
| 1 | 11.25 |
| 2 | 22.17 |
The above embodiment of the present invention is only for example of the present invention is clearly described, not the restriction 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 all embodiments exhaustive.Every still row in protection scope of the present invention of apparent variation that technical scheme of the present invention extends out or change that belong to.
Claims (4)
1. a LC-MS/MS coupling detects the method for ammonia of main stream smoke of cigarette base ethyl formate content, it is characterized in that, comprise the following steps: utilize the urethanes in cambridge filter trapping cigarette mainstream flue gas, use ethanol extraction filter disc, extract is concentrated, dilution purifies by solid phase extraction column, use methylene chloride wash-out, eluent detects with high performance liquid chromatography/tandem mass spectrometer, adopts internal standard method to obtain the content of ammonia of main stream smoke of cigarette base ethyl formate;
The internal standard compound adopting in described internal standard method is deuterated urethanes;
Described solid phase extraction column is fixing is hydrophilic-lipophilic balance resin mutually;
Described high performance liquid chromatograph condition is: C18 reversed-phase column, and 30 ℃ of detected temperatures, sample size 1 μ L～10 μ L, flow velocity 0.2～0.4mL/min, acetonitrile and water carry out gradient elution as mobile phase; Described mass spectrometer condition is: ionization mode is electron spray; Scan pattern is positive ion; Atomization gas 35～45psi; Gas curtain gas 10psi; Auxiliary heating gas 45～55psi; Collision gas 5psi; Ion gun injection electric 5000～5800V; 350～400 ℃ of ion source temperatures;
Described high performance liquid chromatograph mobile phase A is the mixed solution of the acetonitrile/water containing 0.1% acetic acid with V:V=90:10, and Mobile phase B is acetonitrile; Gradient elution program is:
。
2. according to the LC-MS/MS coupling of claim 1, detect the method for ammonia of main stream smoke of cigarette base ethyl formate content, it is characterized in that, comprise the following steps:
1) by cigarette to be measured balance 48h under the tobacco of GB/T16447-2004 regulation and the Atmospheric Condition of tobacco product adjusting and test;
2) adopt smoking machine to aspirate under standard aspiration condition, utilize the urethanes in cambridge filter trapping cigarette mainstream flue gas, adopt 40mL containing the ethanolic solution extraction filter disc of the 320 nanogram internal standard compounds of having an appointment, be extracted liquid;
3) pipette 10～20ml extract in concentrated bottle, evaporation and concentration, to 0.5mL left and right, adds 10mL distilled water in concentrate, the percent by volume of ethanol is down to below 10%, dilution is transferred on solid phase extraction column and is purified, adopt methylene chloride to carry out wash-out, collect eluent;
4) eluent is concentrated into dry rear with adopting high performance liquid chromatography/tandem mass spectrometer to measure after about 1ml mobile phase dissolving:
Described high performance liquid chromatograph condition is: C18 reversed-phase column, and 30 ℃ of detected temperatures, sample size 1 μ L～10 μ L, flow velocity 0.2～0.4mL/min, acetonitrile and water carry out gradient elution as mobile phase;
Described mass spectrometer condition is: ionization mode is electron spray; Scan pattern is positive ion; Atomization gas 35～45psi; Gas curtain gas 10psi; Auxiliary heating gas 45～55psi; Collision gas 5psi; Ion gun injection electric 5000～5800V; 350～400 ℃ of ion source temperatures;
5) the urethanes series standard working solution of preparation 10ng/mL～600ng/mL, 5 of concentration gradients are above and be uniformly distributed, and the concentration of the internal standard compound that standard solution at different levels contain is 300ng/mL left and right; Utilize high performance liquid chromatography-tandem mass instrument to detect standard solution, using the ratio of the urethanes peak area obtaining and interior mark peak area as ordinate, urethane ester concentration and interior mark concentration ratio are as horizontal ordinate, drawing standard curve also obtains regression equation, then under the same conditions sample is detected, by in the urethanes obtaining and interior target peak area ratio substitution equation, can calculate the content of urethanes.
3. according to the LC-MS/MS coupling of claim 2, detect the method for ammonia of main stream smoke of cigarette base ethyl formate content, it is characterized in that, the quota ion of described urethanes is 90.0/62.1 to m/z, qualitative ion pair m/z is 90.0/44.0, residence time is 200ms, and impact energy is 14.0V.
4. according to the LC-MS/MS coupling of claim 1, detect the method for ammonia of main stream smoke of cigarette base ethyl formate content, it is characterized in that, the quota ion of described deuterated urethanes is 95.0/63.2 to m/z, qualitative ion pair m/z is 95.0/44.2, residence time is 200ms, and impact energy is 25.0V.
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| CN101620206A (en) * | 2009-06-18 | 2010-01-06 | 浙江大学 | Method for detecting ethyl carbamate in yellow wine |
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| CN101692075A (en) * | 2009-09-10 | 2010-04-07 | 广东中烟工业有限责任公司 | Method for analyzing main stream smoke of cigarette |
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