CN102788858A - 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 the method that a kind of high performance liquid chromatography-tandem mass coupling detects urethane ester content in the cigarette mainstream flue gas particularly.
Background technology
Urethanes (Ethyl carbamate; EC claims urethane again) extensively be present in the various fermented foods; It is a kind of potential carcinogen; Can cause multiple diseases such as lung cancer, lymph cancer, liver cancer and cutaneum carcinoma; International cancer research institution of the World Health Organization (WHO) (IARC) is classified as 2A class carcinogenic substance with it, and " 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; In order to ensure human body health, should reduce the content of urethanes in fermented beverage and the food as far as possible.
1991; In 43 kinds of harmful ingredients in flue gas inventories that Hoffmann announces; Urethanes is listed; Calendar year 2001 Hoffmann and its researcher revise and replenish objectionable constituent inventory in 1991, will classify one of 69 kinds of objectionable constituent as by urethanes, and Rodgman in 2002 and Green sum up the objectionable constituent of having reported in the flue gas; Also classify urethanes one of as 149 kinds of cigarette smoke objectionable constituent; U.S. food and FAD (FDA) are classified the urethanes in the tobacco as carcinogen (CA) and reproductive system/growth Toxic (RDT), but so far, do not find to have any patent and the bibliographical information that adopts the high performance liquid chromatography-tandem mass appearance to measure urethane ester content in the cigarette mainstream flue gas as yet both at home and abroad.
Chinese patent 200910099554.0 open " a kind of method that detects urethanes in the yellow rice wine "; This method is mixed through decompression distillation-with hydrochloric acid and 9-hydroxyl ton solution and is carried out derivative reaction-utilize colleges and universities' liquid chromatograph that component is separated, and adopts external standard method to calculate the content of urethanes then.This method can effectively detect urethanes in the yellow rice 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-become the focal issue that people pay close attention to, still; The 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, and above-mentioned patented method also is not suitable for the content that detects urethanes in the flue gas.Therefore; Set up urethanes content detecting method in a kind of cigarette mainstream flue gas; And this method also needs fast, accurately, good separating effect, highly sensitive be a current urgent task of tobacco business, for research with estimate smoking and also have the important and urgent meaning of ten minutes with health problem.
Summary of the invention
The purpose 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 urethane ester content in the cigarette mainstream flue gas.
A kind of LC-MS/MS coupling detects the method for urethane ester content in the cigarette mainstream flue gas; May further comprise the steps: utilize cambridge filter to capture the urethanes in the cigarette mainstream flue gas; Use the ethanol extraction filter disc, extract concentrates, dilution is after solid phase extraction column purifies, and uses the methylene chloride wash-out; Eluent detects with high performance liquid chromatography/tandem mass spectrometer, adopts internal standard method to obtain the content of urethanes in the cigarette mainstream flue gas.
Further, the internal standard compound that adopts in the said internal standard method is that deuterium is for urethanes.
Further, said solid phase extraction column stationary phase is the hydrophilic-lipophilic balance resin.For example, HLB pillar (the SDVB multipolymer of modification).
Further, said high performance liquid chromatograph condition is: the 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 moving phase; Said mass spectrometer condition is: ionization mode is an electron spray; Scan pattern is a positive ion; Atomization gas 35～45L/min; Gas curtain gas 10L/min; Auxiliary heating gas 45～55L/min; Collision gas 5L/min; Ion gun injection electric 5000～5800V; 350～400 ℃ of ion source temperatures.
Further, said high performance liquid chromatograph mobile phase A is to contain the mixed solution of the acetonitrile/water of 0.1% acetate with V:V=90:10, and Mobile phase B is an acetonitrile; The gradient elution program is:
| Time/min | Flow velocity/mL ﹒ min-1 | Mobile phase A | |
| 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 |
A kind of LC-MS/MS coupling detects the method for urethane ester content in the cigarette mainstream flue gas, may further comprise the steps:
1) with cigarette to be measured balance 48h under the atmospheric environment condition that the tobacco and the tobacco product of GB/T16447-2004 regulation are regulated and tested;
2) adopt smoking machine under the standard aspiration condition, to aspirate, utilize cambridge filter to capture the urethanes in the cigarette mainstream flue gas, the ethanolic solution that adopts 40mL to contain 320 nanograms (ng) internal standard compound extracts filter disc,, obtain extract;
3) pipette 10～20ml extract in concentrating bottle, evaporation and concentration adds 10mL distilled water to the 0.5mL in concentrate; The percent by volume of ethanol is reduced to below 10%; Dilution is transferred on the solid phase extraction column purifies, adopt methylene chloride to carry out wash-out, collect eluent;
4) eluent is concentrated into to do and adopts high performance liquid chromatography/mass spectrometer to measure after dissolve with about 1ml moving phase the back:
Said high performance liquid chromatograph condition is: the 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 moving phase;
Said mass spectrometer condition is: ionization mode is an electron spray; Scan pattern is a 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; Said 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, concentration gradient distributes more than 5 and evenly, and the concentration of the internal standard compound that standard solution at different levels contain is about 300ng/mL; Utilize the high performance liquid chromatography-tandem mass appearance that standard solution is detected; With the ratio of urethanes peak area that obtains and interior mark peak area as ordinate; Urethane ester concentration and interior mark concentration ratio are as horizontal ordinate, and the drawing standard curve also obtains regression equation, under the same conditions sample is detected then; In urethanes that obtains and interior target peak area ratio substitution equation, can calculate the content of urethanes.
Further, internal standard compound is that deuterium is for urethanes step 2).
Further, concentrating in the step 3) is under 50 ℃ of conditions, to adopt nitrogen to blow concentrating instrument extract to be concentrated into dried.
Further, the solid phase extraction column stationary phase is the hydrophilic-lipophilic balance resin in the step 3).
Said C18 reversed-phase column specification is 150mm * 2.1mm, 5 μ m.
Further, said high performance liquid chromatograph mobile phase A is to contain the mixed solution of the acetonitrile/water of 0.1% acetate with V:V=90:10, and Mobile phase B is an acetonitrile; The 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 said 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, said deuterium is 95.0/63.2 for the quota ion of urethanes 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 urethanes in the cigarette mainstream flue gas 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 urethanes in all kinds of cigarette mainstream flue gas.
Description of drawings
Fig. 1 is the chromatogram of standard solution;
Fig. 2 contains the chromatogram of internal standard compound for standard solution;
Fig. 3 is the chromatogram of urethanes (containing internal standard compound) in certain cigarette mainstream flue gas.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is further specified.
Instrument of the present invention and reagent, material
The triple level Four bar of the U.S. API3200 of Applied Biosystems company type tandem mass spectrometer; Be furnished with electric spray ion source and Analyst system software; U.S. Agilent company 1200 type high performance liquid chromatographs, band automatic sampler, German Borgwaldt RM20H type smoking machine; The U.S. RapidVapN2 of Labconco company concentrating instrument; Electronic balance (sensibility reciprocal 0.1mg), the adjustable mechnical oscillator U.S. Supelco solid-phase extraction device (VISPREPTM DL) that circles round, the hydrophilic lipophilic solid phase extraction column of the HLB of U.S. Waters company (500mg/6mL).
Acetonitrile, acetate are chromatographically pure, and ethanol, methylene chloride are that analysis is pure, deionized water; The urethanes standard items, Chun Du ≧ 98%, deuterium is for urethanes internal standard compound standard items, Chun Du ≧ 99%.
Reagent and solution preparation
The preparation of standard reserving solution: the urethanes that accurately takes by weighing about 10mg is in the 50mL beaker; Be accurate to 0.0001g; Add and be transferred in the 100mL volumetric flask after about 20mL acetonitrile dissolves fully; Swing with minor amounts of acetonitrile and to wash beaker 3～5 times, cleansing solution is transferred in the volumetric flask in the lump, is settled to scale with acetonitrile then.
The preparation of primary standard solution: the standard inventory solution that accurately pipettes 2.50mL with transfer pipet is settled to scale with acetonitrile in the 250mL volumetric flask.
In the preparation of mark storing solution: the deuterium that accurately takes by weighing about 20mg for urethanes in the 50mL beaker; Be accurate to 0.0001g; Add and be transferred in the 100mL volumetric flask after about 20mL acetonitrile dissolves fully; Swing with minor amounts of acetonitrile and to wash beaker 3～5 times, cleansing solution is transferred in the volumetric flask in the lump, is settled to scale with acetonitrile then.
The preparation of one-level inner mark solution: the interior mark stock solution that accurately pipettes 4.00mL with transfer pipet is settled to scale with acetonitrile in the 100mL volumetric flask.
The preparation of secondary inner mark solution: the standard inventory solution that accurately pipettes 10.00mL with transfer pipet is settled to scale with acetonitrile in the 250mL volumetric flask.
The preparation of series standard working solution: the primary standard solution and the 1.00 secondary inner mark solutions that accurately pipette 0.25mL, 0.50mL, 1.00mL, 3.75mL, 7.50mL, 15.00mL, 30.00mL respectively are in the 50mL volumetric flask; Be settled to scale with acetonitrile; 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 the production standard curve.
Fig. 1 is the chromatogram of standard solution; Fig. 2 contains the chromatogram of internal standard compound for standard solution; Fig. 3 is the chromatogram of urethanes (containing internal standard compound) in certain cigarette mainstream flue gas.
Embodiment 1
A kind of LC-MS/MS coupling detects the method for urethane ester content in the cigarette mainstream flue gas, may further comprise the steps:
Sample collection: with cigarette balance 48 hours under (22 ± 1) ℃, relative humidity (60 ± 3) % condition; Carry out cigarette smoking according to the condition of tobacco business YC/T29-1996 standard code then; Adopt the spun glass filter disc to capture 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 the 150mL conical flask capture, add 40mL ethanol and 1.00mL secondary inner mark solution, place on the velocity-modulated oscillator and vibrated 30 minutes.
Sample pre-treatments: measure the above-mentioned extract of about 10mL in concentrating bottle, adopt nitrogen to blow concentrating instrument and be concentrated into about 0.5mL, in concentrate, add the dilution of 10mL deionized water, to be clean behind the mixing.Above-mentioned dilution is transferred on good hydrophilic lipophilic solid phase extraction column (HLB) pillar of activation, balance; Effluent discards and drains pillar 3min; Use 4mL methylene chloride wash-out then, after the collection eluent is concentrated into and does, adopt 1.0ml moving phase dissolving post analysis.
The 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: acetonitrile/water (V:V=90:10) mixed solution that contains 0.1% acetate; Mobile phase B: acetonitrile; The gradient elution program is as shown in table 1:
Table 1 gradient elution program
| Time/min | Flow velocity/mL ﹒ min-1 | Mobile phase A | |
| 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: 50psi; 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 |
| Deuterium generation-urethanes | 95.0/63.2 | 95.0/44.2 | 200 | 25.0 |
Utilize the high performance liquid chromatography-tandem mass appearance that series standard solution is detected; With the ratio of urethanes peak area that obtains and interior mark peak area as horizontal ordinate; Urethane ester concentration and interior mark concentration ratio are as ordinate; The drawing standard curve also obtains regression equation, and regression equation is y=0.967x+0.00408 (linearly dependent coefficient is 1.0), under the same conditions sample is detected then; In urethanes that obtains and interior target peak area ratio substitution equation, draw the content of urethanes according to computes.
In the formula:
The content of m-every cigarette urethanes, unit are nanogram/(ng/cig);
A-urethanes peak area;
A
s-deuterium is for the urethanes peak area;
B-draw by equation of linear regression;
m
sMark content in-the sample solution, unit is nanogram (ng);
A-draw by equation of linear regression;
N-cigarette number, unit is for propping up.
Precision of the inventive method and detectability
A certain standard model is carried out 6 times continuously measure, the peak area ratio precision of urethanes is investigated, the result is as shown in table 3:
The precision of table 3 method
| The sample introduction number of times | Retention time min | Peak area |
| 1 | 3.06 | 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 |
The result shows in the table, no matter is retention time or peak area, and relative standard deviation shows the content that can accurately measure urethanes in the cigarette mainstream flue gas all less than 5%.
Standard specimen with least concentration (5.0ng/mL) repeats sample introduction 10 times, counts standard deviation by the concentration value that records, 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
On certain brand cigarette filter disc, add the urethanes reference material of 232ng, 464ng and 696ng respectively, record the sodium cyclohexylsulfamate content value under three levels of basic, normal, high mark-on, each horizontal parallel is measured three times, and mean value is seen 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 that the content of the urethanes in two cigarette sample main flumes is measured, it is as shown in the table to measure the result:
| Cigarette sample | Urethanes (ng/cig) |
| 1 | 11.25 |
| 2 | 22.17 |
The above embodiment of the present invention only be for clearly the present invention is described and is done for example, be not qualification to embodiment of the present invention.For the those of ordinary skill in affiliated field, on the basis of above-mentioned explanation, can also make other multi-form variation or change.Here can't give exhaustive to all embodiments.Everyly belong to the row that conspicuous variation that technical scheme of the present invention extends out or change still are in protection scope of the present invention.
Claims (8)
1. a LC-MS/MS coupling detects the method for urethane ester content in the cigarette mainstream flue gas; It is characterized in that, may further comprise the steps: utilize cambridge filter to capture the urethanes in the cigarette mainstream flue gas, use the ethanol extraction filter disc; Extract concentrates, dilution after solid phase extraction column purify; Use the methylene chloride wash-out, eluent detects with high performance liquid chromatography/tandem mass spectrometer, adopts internal standard method to obtain the content of urethanes in the cigarette mainstream flue gas.
2. detect the method for urethane ester content in the cigarette mainstream flue gas according to the LC-MS/MS coupling of claim 1, it is characterized in that the internal standard compound that adopts in the said internal standard method is that deuterium is for urethanes.
3. detect the method for urethane ester content in the cigarette mainstream flue gas according to the LC-MS/MS coupling of claim 1, it is characterized in that said solid phase extraction column stationary phase is the hydrophilic-lipophilic balance resin.
4. detect the method for urethane ester content in the cigarette mainstream flue gas according to the LC-MS/MS coupling of claim 1; It is characterized in that; Said high performance liquid chromatograph condition is: C18 reversed-phase column, 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 moving phase; Said mass spectrometer condition is: ionization mode is an electron spray; Scan pattern is a 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. detect the method for urethane ester content in the cigarette mainstream flue gas according to the LC-MS/MS coupling of claim 4; It is characterized in that; Said high performance liquid chromatograph mobile phase A is to contain the mixed solution of the acetonitrile/water of 0.1% acetate with V:V=90:10, and Mobile phase B is an acetonitrile; The gradient elution program is:
6. detect the method for urethane ester content in the cigarette mainstream flue gas according to the LC-MS/MS coupling of claim 1, it is characterized in that, may further comprise the steps:
1) with cigarette to be measured balance 48h under the atmospheric environment condition that the tobacco and the tobacco product of GB/T 16447-2004 regulation are regulated and tested;
2) adopt smoking machine under the standard aspiration condition, to aspirate, utilize cambridge filter to capture the urethanes in the cigarette mainstream flue gas, adopt 40mL to contain the ethanolic solution extraction filter disc of 320 nanograms (ng) internal standard compound of having an appointment, obtain extract;
3) pipette 10～20ml extract in concentrating bottle, evaporation and concentration adds 10mL distilled water to the 0.5mL in concentrate; The percent by volume of ethanol is reduced to below 10%; Dilution is transferred on the solid phase extraction column purifies, adopt methylene chloride to carry out wash-out, collect eluent;
4) eluent is concentrated into to do and adopts high performance liquid chromatography/mass spectrometer to measure after dissolve with about 1ml moving phase the back:
Said high performance liquid chromatograph condition is: the 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 moving phase;
Said mass spectrometer condition is: ionization mode is an electron spray; Scan pattern is a 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, concentration gradient distributes more than 5 and evenly, and the concentration of the internal standard compound that standard solution at different levels contain is about 300ng/mL; Utilize the high performance liquid chromatography-tandem mass appearance that standard solution is detected; With the ratio of urethanes peak area that obtains and interior mark peak area as ordinate; Urethane ester concentration and interior mark concentration ratio are as horizontal ordinate, and the drawing standard curve also obtains regression equation, under the same conditions sample is detected then; In urethanes that obtains and interior target peak area ratio substitution equation, can calculate the content of urethanes.
7. detect the method for urethane ester content in the cigarette mainstream flue gas according to the LC-MS/MS coupling of claim 6; It is characterized in that; The quota ion of said urethanes is 90.0/62.1 to m/z; Qualitative ion pair m/z is 90.0/44.0, and residence time is 200ms, and impact energy is 14.0V.
8. detect the method for urethane ester content in the cigarette mainstream flue gas according to the LC-MS/MS coupling of claim 2; It is characterized in that; Said deuterium is 95.0/63.2 for the quota ion of urethanes to m/z; Qualitative ion pair m/z is 95.0/44.2, and residence time is 200ms, and impact energy is 25.0.
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| CN105758973A (en) * | 2014-12-18 | 2016-07-13 | 中粮集团有限公司 | Solid support liquid-liquid extraction pretreatment method of urethane in wine |
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| CN105758973A (en) * | 2014-12-18 | 2016-07-13 | 中粮集团有限公司 | Solid support liquid-liquid extraction pretreatment method of urethane in wine |
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