CN103698454B - A kind of measure the detection method of epimedium active constituent in cigarette shreds and main flume thereof - Google Patents
A kind of measure the detection method of epimedium active constituent in cigarette shreds and main flume thereof Download PDFInfo
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Abstract
A kind of measure the detection method of epimedium active constituent in cigarette shreds and main flume thereof, the method utilizes high performance liquid chromatography LC-MS spectrometry combination method (HPLC ESI MS), the content of Herba Epimedii principle active component icariin and epimidin c in cigarette shreds and cigarette mainstream flue gas is detected, comprises the following steps successively: the selecting and balancing of (1) Cigarette；(2) reference substance solution is prepared；(3) cigarette shreds sample solution is prepared；(4) sample solution in cigarette mainstream flue gas is prepared；(5) sample to be analyzed to gained carries out High Performance Liquid Chromatography Coupled with Electrospray Ionization Mass method (HPLC ESI MS) analysis.Epimedium active constituent in cigarette shreds and cigarette mainstream flue gas can be carried out effectively extracting completely by the present invention, and can the content of epimedium active constituent in Accurate Determining cigarette shreds and cigarette mainstream flue gas.The method is reproducible, analyzes detection sensitivity high.
Description
Technical field
The present invention relates to the detection method of content of epimedium active constituent, particularly measure epimedium active constituent content assaying method in cigarette shreds and main flume thereof, belong to Nicotiana tabacum L. detection technique field.
Background technology
Herba Epimedii is Berberidaceae plant Herba Epimedii Epimedium brevicornum Maxim., Epimedium sagittatum Epimedium sagittatum (Sieb.et Zucc.) Maxim., E. Pubescens Epimedium pubescens Maxim. or the dry aerial parts of Herba Epimedii Epimedium koreanum Nakai, there is kidney-replenishing, bone and muscle strengthening, effect of wind-damp dispelling.For impotence and seminal emission, muscles and bones flaccidity is soft, rheumatic arthralgia, numbness contracture.
Continuous propelling along with global Tobacco Control campaign, the public is for smoking and health problem growing interest, viewpoint is had to think, in Medicated cigarette, add the beneficiating ingredient of natural plants to reduce cigarette smoke and attempt to reduce the harm that smoking causes by adding Herba Epimedii extract at Medicated cigarette to harm, Some Domestic research.Chinese patent " a kind of moist-keeping flavouring additive agent for Medicated cigarette and its preparation method and application " (CN201210227599.3) and " a kind of natural plants cigarette harm reduction additive and its preparation method and application " (CN201210227591.7) display, natural plant extraction liquid containing Herba Epimedii composition can be effectively increased the perfume quantity of Medicated cigarette after making an addition to Medicated cigarette, improve aroma quality and harmony, reduce miscellaneous QI and zest, increase sweet sense, making pleasant impression cleaner, comfortable, entirety improves the interior quality of Medicated cigarette；Can alleviate compared with comparison Medicated cigarette cigarette smoke to the damage of human respiratory epithelial cell, reverse the hemoglobin caused for 30 days in animal fume exposure and decline, platelet counts increases situation, reverses the animal cough latent period reduction that cigarette smoke causes, the animal phenols contents that symptom, the reverse cigarette smokes such as cough number of times increase cause reduces symptom, embodies and necessarily alleviates cigarette smoke damaging effect.
Herba Epimedii effect effective ingredient main with it is closely related, Herba Epimedii principle active component is icariin (Icariin) and epimidin c(Epmedin C), icariin has multiple pharmacotoxicological effects such as improving cardio and vascular function, endocrine regulation and gonad function, the osteoblastic propagation of promotion and growth, enhancing immunologic function, antitumor；Epimidin c has significant anti-inflammatory and analgesic effect, and two kinds of compositions are the principle active component of Herba Epimedii, is also its main Quality Control composition.And the content of these effective ingredient is relatively low, the most after being combusted, possible hot cracked, the chemical reaction of these effective ingredient etc. produces change, and the content in cigarette mainstream flue gas is lower.In natural medicinal formulations, the detection method of epimedium active constituent is mainly high performance liquid chromatography at present, also have document report to use the detection of HPLC method to add the icariin in Herba Epimedii extract cigarette mainstream flue gas at tobacco business, and in flue gas the detection of epimidin c there is not been reported.Liquid chromatography can realize two kinds of active constituent content measurings, but sensitivity is relatively low, self capacity of resisting disturbance is more weak, when analyzing low content sample, easily occurs the most inaccurate or cannot be quantitative.High performance liquid chromatography-electro-spray ionization-MS (HPLC-ESI-MS) is that current Drugs studies strong instrument, have highly sensitive, specificity is good, sample treatment is simple, analyze the advantages such as quick, active ingredient of natural plant in detection cigarette smoke is had suitable advantage.
Summary of the invention
Present invention is generally directed to the weak point in terms of liquid chromatography measures epimedium active constituent in the case of content is low, especially for not yet there being the situation of epimidin c content report in detection cigarette smoke, it is provided that a kind of measure the method for Herba Epimedii principle active component content in Medicated cigarette and main flume.The method can realize quick, the accurate quantitative analysis of Herba Epimedii principle active component in Medicated cigarette and main flume.
It is an object of the invention to be achieved through the following technical solutions.
A kind of measure the detection method of epimedium active constituent in cigarette shreds and main flume thereof, described epimedium active constituent includes icariin and epimidin c, it is characterized in that: the method utilizes high performance liquid chromatography-electro-spray ionization-MS (HPLC-ESI-MS), respectively the content of icariin and epimidin c in cigarette shreds and cigarette mainstream flue gas is detected, comprises the following steps successively:
(1) the selecting and balancing of Cigarette: Cigarette is balanced 48h in 22 DEG C ± 1 DEG C and RH60% ± 2% time；
(2) reference substance solution is prepared: take icariin reference substance appropriate, accurately weighed, add 35-75% alcoholic solution and make every 1ml solution containing 0.1mg, to obtain final product；Take epimedin C reference substance appropriate, accurately weighed, add 35-75% alcoholic solution and make every 1ml solution containing 0.1mg, to obtain final product；
(3) cigarette shreds sample solution is prepared: take 10-20 and prop up the tobacco shred of sample cigarette after balance, accurately weighed, the accurate alcoholic solution 100-200ml adding 35-75%, extracts 20-60min, supplies weight with 35-75% alcoholic solution, shake up, cross 0.22um microporous filter membrane, to obtain final product；
(4) sample solution in cigarette mainstream flue gas is prepared: the Medicated cigarette after weighing apparatus of making even, in 22 DEG C ± 2 DEG C environment with RH60% ± 5% and under standard conditions, with smoking machine smoking cigarette sample, trap Smoke Particulate, the flue gas of every filter disc 20 cigarettes of trapping with cambridge filter；Inhaling and finish, take out sample cigarette filter disc a, precision adds 35-75% alcoholic solution 30-100ml, extracts 20-60min, supplies weight with 35-75% alcoholic solution, shake up, and crosses 0.22um microporous filter membrane, to obtain final product；
(5) sample to be analyzed to gained carries out high performance liquid chromatography-electro-spray ionization-MS (HPLC-ESI-MS) and analyzes:
Chromatographic condition: with octadecylsilane chemically bonded silica as filler；Flowing phase: acetonitrile/water=30/70；Flow velocity: 0.5ml/min；Column temperature: 30 DEG C；
Mass Spectrometry Conditions: use electron spray (ESI) ion source, negative ion mode；Spray voltage: 3kV；Sheath atmospheric pressure: 30mTorr；Auxiliary gas pressure: 0；Heated capillary temperature: 350 DEG C；Collision energy: 15V；Collision-induced parsing voltage in source: 0；Collision air pressure: 1.1mTorr；Collision energy: 30V；
Algoscopy: precision draws reference substance solution and need testing solution 5-10ul respectively, injects HPLC-MS instrument, measures, to obtain final product.
Of the present invention a kind of measure the detection method of epimedium active constituent in cigarette shreds and main flume thereof, it is characterised in that above-mentioned (3rd) and (4) step described in extract process, can be ultrasonic extraction, it is possible to extract for concussion, or soak extraction.
Of the present invention a kind of measure the detection method of epimedium active constituent in cigarette shreds and main flume thereof, it is characterized in that, above-mentioned (2nd), (3) and dissolve and alcohol used by extraction process described in (4) step, can be to include one, the monohydric alcohol of two or three carbon atoms or polyhydric alcohol, preferably methanol, ethanol, propylene glycol, normal propyl alcohol, isopropanol or glycerol.
Of the present invention a kind of measure the detection method of Herba Epimedii main effect component in cigarette shreds and main flume thereof, it is characterised in that dissolving described in above-mentioned (2nd), (3) and (4) step and alcoholic solution concentration used by extraction process is preferably 40-60%, optimum is 50%.
Of the present invention a kind of measure the detection method of Herba Epimedii main effect component in cigarette shreds and main flume thereof, it is characterised in that adding alcoholic solution described in above-mentioned (3rd) step and be preferably 130-160mL, optimum is 150mL；Adding alcoholic solution described in above-mentioned (4) step and be preferably 40-60mL, optimum is 50mL.
Of the present invention a kind of measure the detection method of Herba Epimedii main effect component in cigarette shreds and main flume thereof, it is characterised in that extraction time described in above-mentioned (3rd) step is preferably 25-40 minute, and optimum is 30 minutes.
It is an advantage of the current invention that: use this method, it is possible to carry out epimedium active constituent in cigarette shreds and cigarette mainstream flue gas effectively extracting completely, and the content of epimedium active constituent in energy Accurate Determining cigarette shreds and cigarette mainstream flue gas.The method is reproducible, analysis detection sensitivity is high, it is capable of effective analysis of Herba Epimedii chemical composition in cigarette shreds and cigarette mainstream flue gas, effectively can add the uniformity of flavouring harm reduction additive and accuracy by evaluating cigarette tobacco shred, thering is provided technical support for cigarette primary processing technique, to improving, cigarette product quality is significant.
Accompanying drawing illustrates:
Fig. 1 icariin standard substance chromatogram；
Fig. 2 epimidin c standard substance chromatogram；
Fig. 3 compares the detection chromatogram of icariin in cigarette shreds；
Fig. 4 compares the detection chromatogram of epimidin c in cigarette shreds；
The detection chromatogram of icariin in Fig. 5 sample cigarette shreds；
The detection chromatogram of epimidin c in Fig. 6 sample cigarette shreds；
Fig. 7 compares the detection chromatogram of icariin in cigarette mainstream flue gas；
Fig. 8 compares the detection chromatogram of epimidin c in cigarette mainstream flue gas；
The detection chromatogram of icariin in Fig. 9 sample cigarette mainstream flue gas；
The detection chromatogram of epimidin c in Figure 10 sample cigarette mainstream flue gas.
Detailed description of the invention:
The present invention is further described below with reference to embodiment, but does not limit the practical range of the present invention.
Embodiment:
Materials and methods
1.1 experimental apparatus
Finnigan TSQ Quantum Discovery Max liquid chromatograph-mass spectrometer (Thermo Finnigan company of the U.S.), is equipped with electron spray (ESI) ion source detector；Sai Duolisi BP110s type electronic balance；RM200 smoking machine (BORGWALDT company of Germany).
1.2 standard substance and sample
Icariin and epimedin C are purchased from Phytomarker Co., Ltd.；Certain trade mark Medicated cigarette blank tobacco shred and add the comparison Medicated cigarette and sample Medicated cigarette made containing the sample tobacco cartridge of Herba Epimedii composite natral plant extracting solution；Acetonitrile is chromatographically pure (Merck)；Water is high purity water；Remaining reagent is analytical pure.
Flue gas filter disc: take the comparison Medicated cigarette after selecting and sample Medicated cigarette, 48h is balanced in 22 DEG C ± 1 DEG C and RH60% ± 2% time, use RM200 smoking machine to press GB/T19609 smoking cigarette sample, trap Smoke Particulate, every filter disc 20 Medicated cigarette of trapping with φ 92mm cambridge filter.
1.3 test method
1.3.1 chromatographic condition
Agilent Eclipse XDB C18 (150mm × 2.1mm, 5um)；Flowing phase: acetonitrile/water=30/70；Flow velocity: 0.5ml/min；Column temperature: 30 DEG C
1.3.2 Mass Spectrometry Conditions
Electron spray (ESI) ion source, negative ion mode, spray voltage: 3kV；Sheath atmospheric pressure: 30mTorr；Auxiliary gas pressure: 0；Heated capillary temperature: 350 DEG C；Collision energy: 15V；Collision-induced parsing voltage in source: 0；Collision air pressure: 1.1mTorr；Collision energy: 30V.
Icariin: 721.01(m/z)--513.26(m/z)；Therefore optionally detecting mass-to-charge ratio (m/z) is the daughter ion of 513.26；Epimedin C: 867.15(m/z)--659.31(m/z), therefore optionally detecting mass-to-charge ratio (m/z) is the daughter ion of 659.31.
1.3.3 solution preparation
1.3.3.1 reference substance solution preparation
The most accurately weigh icariin reference substance 8.99mg, epimedin C reference substance 8.57mg, it is placed in volumetric flask, adds 50% methanol solution, be configured to the reference substance solution that mass concentration is 35.96ng/ml and 171.4ng/ml respectively.
1.3.3.2 the preparation of need testing solution:
The preparation of tobacco shred need testing solution: take comparison cigarette shreds and each about 10.0g of sample cigarette shreds, accurately weighed, accurate addition 50% methanol solution 150ml, supersound extraction 30min, supply weight with 50% methanol, shake up, cross 0.22um microporous filter membrane, to obtain final product.
The preparation of filter disc need testing solution: take filter disc sample, accurate addition 50% methanol solution 50ml, supersound extraction 30min, supply weight with 50% methanol, shake up, cross 0.22um microporous filter membrane, to obtain final product.
2. result and analysis
2.1 specificity experiments
Accurate measuring comparison cigarette shreds need testing solution, sample cigarette shreds need testing solution, comparison cigarette smoke filter disc need testing solution, the sample cigarette smoke each 10ul of filter disc need testing solution, inject liquid chromatograph/mass spectrometer, detection 513.26 and 659.31 daughter ions respectively, and compare with icariin and epimedin C standard substance collection of illustrative plates, result is shown in Fig. 1-Figure 10, and result shows to compare cigarette shreds and the mensuration of sample cigarette shreds and main flume thereof is not interfered with by flue gas filter disc.
2.2 standard curves and the range of linearity
Respectively reference substance is diluted to series concentration, precision draws 10ul injection liquid chromatograph/mass spectrometer respectively, it is analyzed, record chromatogram, respectively with sample size (ng) as abscissa, with peak area as vertical coordinate, draw standard curve, obtain the equation of linear regression of icariin: y=367.39x-249.49(r=0.9991), the range of linearity is 0.0072-0.539ng；The equation of linear regression y=12282x-1161.5(r=0.9992 of epimedin C), the range of linearity is 0.0857-1.714ng.
2.3 Precision Experiment
Taking icariin and each portion of epimedin C reference substance solution, continuous sample introduction measures 6 times respectively, and the RSD of the peak area recording icariin and epimedin C is respectively 2.5% and 3.4%, shows that precision is preferable, the results are shown in Table 1.
Table 1 Precision Experiment
2.4 stability experiment
Take sample tobacco shred about 10.0g, accurately weighed, prepare according to need testing solution preparation method, respectively 0,1,2,4,6, within 8 hours, measuring, the RSD of the peak area of result icariin and epimedin C is respectively 2.8% and 3.8%, and result shows that need testing solution is stable in 8 hours, the results are shown in Table 2.
Table 2 sample solution stability experiment
2.5 repeated experiment
Take 6 parts of sample tobacco shred about 10.0g, accurately weighed, prepare 6 parts of need testing solutions according to need testing solution preparation method, and be measured, the RSD of the content recording icariin and epimedin C is respectively 3.6% and 3.7%, and result shows that the repeatability of method is preferable, the results are shown in Table 3.
Table 3 repeated experiment
2.6 response rate experiments
Take 6 parts of sample tobacco shred, every part of about 5.0g, accurately weighed, and precision adds icariin reference substance solution 20.0ml that concentration is 71.92ng/ml or epimedin C reference substance solution 15.0ml that concentration is 171.4ng/ml respectively, precision is supplied 50% methanol and is prepared need testing solution to after 150ml according to need testing solution preparation method and be measured again, the average recovery rate (n=6) of result icariin and epimedin C is respectively 95.1% and 97.3%, and RSD is respectively 3.6% and 3.7%, the results are shown in Table 4-5.
The table 4 icariin response rate is tested
The table 5 epimedin C response rate is tested
Icariin and epimidin c assay in 2.7 sample cigarette shreds and main flume
Comparison Medicated cigarette and sample cigarette smoke and main flume filter disc carry out the assay of icariin and epimedin C according to the method described above, and Fig. 3-10 are shown in by detection collection of illustrative plates, do not detect icariin and epimidin c in result comparison cigarette shreds and main flume；Icariin and epimedin C content in sample tobacco shred is respectively 443.68ng/ and props up and prop up with 844.65ng/, in main flume filter disc, respectively 15.61ng/ props up and props up with 60.14ng/, and the rate of transform calculating epimedin C and icariin is respectively 3.52% and 7.12%.
2.8 solvent compatibility tests
The solvent adaptability of method is analyzed for the checking present invention, according to above-mentioned detection method, solvent made by the different alcohol of replacing and extractant is tested, it is respectively ethanol, propylene glycol, normal propyl alcohol, isopropanol or glycerol, result shows, selected solvent on result of the test without impact, consistent with Methanol result.
Claims (8)
1. measuring a detection method for epimedium active constituent in cigarette shreds and main flume thereof, described epimedium active constituent includes
Icariin and epimidin c, it is characterised in that: the method utilizes high performance liquid chromatography-electro-spray ionization-MS
(HPLC-ESI-MS), the content of icariin and epimidin c in cigarette shreds and cigarette mainstream flue gas is detected, depends on
Secondary comprise the following steps:
(1) the selecting and balancing of Cigarette: Cigarette is balanced 48h in 22 DEG C ± 1 DEG C and RH60% ± 2% time；
(2) reference substance solution is prepared: take icariin reference substance appropriate, accurately weighed, add 35-75% alcoholic solution and make every 1ml and contain
The solution of 0.1mg, to obtain final product；Take epimedin C reference substance appropriate, add 35-75% alcoholic solution and make molten containing 0.1mg of every 1ml
Liquid, to obtain final product；
(3) cigarette shreds sample solution is prepared: take 10-20 and prop up the tobacco shred of sample cigarette after balance, accurately weighed, accurate add 35-75%
Alcoholic solution 100-200ml, accurately weighed, extract 20-60min, supply weight with 35-75% alcoholic solution, shake up, cross 0.22
μm microporous filter membrane, to obtain final product；
(4) sample solution in cigarette mainstream flue gas is prepared: the Medicated cigarette after weighing apparatus of making even, in the environment of 22 DEG C ± 2 DEG C and RH60% ± 5%
With under standard conditions, with smoking machine smoking cigarette sample, trap Smoke Particulate, every filter disc 20 cigarettes of trapping with cambridge filter
Flue gas；Inhaling and finish, take out sample cigarette filter disc a, precision adds 35-75% alcoholic solution 30-100ml, extracts 20-60min,
Supply weight with 35-75% alcoholic solution, shake up, cross 0.22 μm microporous filter membrane, to obtain final product；
(5) sample to be analyzed to gained carries out high performance liquid chromatography-electro-spray ionization-MS (HPLC-ESI-MS) and analyzes:
Chromatographic condition: with octadecylsilane chemically bonded silica as filler；Flowing phase: acetonitrile/water=30/70；Flow velocity: 0.5ml/min；
Column temperature: 30 DEG C；
Mass Spectrometry Conditions: use electron spray (ESI) ion source, negative ion mode；Spray voltage: 3kV；Sheath atmospheric pressure: 30mTorr；
Auxiliary gas pressure: 0；Heated capillary temperature: 350 DEG C；Collision energy: 15V；Collision-induced parsing voltage in source: 0；
Collision air pressure: 1.1mTorr；Collision energy: 30V；
Algoscopy: precision draws reference substance solution and need testing solution 5-10 μ l respectively, injects HPLC-MS instrument,
Measure, to obtain final product；
Above-mentioned (3rd) and (4) step described in extract process, for ultrasonic extraction, or concussion is extracted, or soak extraction；
Alcohol used by above-mentioned (2nd), (3) and (4) step, is monohydric alcohol or the polyhydric alcohol including one, two or three carbon atom.
The most according to claim 1 a kind of measure the detection method of epimedium active constituent in cigarette shreds and main flume thereof, its
Being characterised by, alcoholic solution concentration used by described (2nd), (3) and (4) step is 40-60%.
3. described a kind of measure the inspection of epimedium active constituent in cigarette shreds and main flume thereof according to arbitrary in claim 1 or 2
Survey method, it is characterised in that alcohol used by above-mentioned (2nd), (3) and (4) step, for methanol, ethanol, propylene glycol, normal propyl alcohol,
Isopropanol or glycerol.
The most according to claim 3 a kind of measure the detection method of epimedium active constituent in cigarette shreds and main flume thereof, its
Being characterised by, alcoholic solution concentration used by above-mentioned (2nd), (3) and (4) step is 50%.
5. described a kind of measure the detection side of epimedium active constituent in cigarette shreds and main flume thereof according to claim 1-2 is arbitrary
Method, it is characterised in that it is 130-160mL that (3rd) step adds alcoholic solution, it is 40-60mL that (4th) step adds alcoholic solution volume.
The most according to claim 5 a kind of measure the detection method of epimedium active constituent in cigarette shreds and main flume thereof, its
Being characterised by, it is 150mL that above-mentioned (3rd) step adds alcoholic solution, and it is 50mL that above-mentioned (4) step adds alcoholic solution volume.
The most according to claim 6 a kind of measure the detection method of epimedium active constituent in cigarette shreds and main flume thereof, its
Being characterised by, extraction time described in above-mentioned (3rd) step is 25-40 minute.
The most according to claim 7 a kind of measure the detection method of epimedium active constituent in cigarette shreds and main flume thereof, its
Being characterised by, extraction time described in above-mentioned (3rd) step is 30 minutes.
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