CN105699305A - Method for measuring transfer rate of cigarette saponins additive in main stream smoke - Google Patents
Method for measuring transfer rate of cigarette saponins additive in main stream smoke Download PDFInfo
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- CN105699305A CN105699305A CN201610065090.1A CN201610065090A CN105699305A CN 105699305 A CN105699305 A CN 105699305A CN 201610065090 A CN201610065090 A CN 201610065090A CN 105699305 A CN105699305 A CN 105699305A
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
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Abstract
The invention discloses a method for measuring a transfer rate of a cigarette saponins additive in main stream smoke. The method comprises the following steps: selecting a saponins additive in a cigarette as a measured object, wherein the saponins additive can be natural plant powder, a plant extract and residues obtained by plant extraction. The method for adding the additive is that the additive is sprayed into a reconstituted tobacco (liquid or solid) in the form of material liquid (liquid) or added into the reconstituted tobacco in the form of a raw material; after a turntable type range hood is used for suction, a Cambridge filter captures particle phase substances in the main stream smoke, to measure the content of saponins in the collected particle phase substances, so that quantitative detection of the transfer rate of the added saponins in the cigarette in the main stream smoke is realized; therefore, the possibility that the saponins added into the cigarette escape along with gas flow and are inhaled into a human body is judged. The method is accurate, reliable, simple and convenient, and has an important instruction value for development of Chinese herbal cigarettes.
Description
Technical field
The present invention relates to a kind of assay method, particularly to a kind of Medicated cigarette soaping agents additive assay method of the rate of transform in main flume。
Background technology
Saponin (saponins), also known as Saponin, is distributed mainly in the higher plant of land, is also present in the marine organisms such as Asterias amurensis Lutken and Stichopus japonicus on a small quantity。The principle active component of many Chinese herbal medicine such as Radix Ginseng, Herb Gynostemmae Pentaphylli, Radix Polygalae, Radix Platycodonis, Radix Glycyrrhizae, the Rhizoma Anemarrhenae and Radix Bupleuri etc. all contains saponin。Lasting saponiform foam can be produced after its aqueous solution jolting, thus gain the name。
Generate the structure of ruscogenin after being hydrolyzed according to Saponin, triterpenoid saponin (triterpenoidalsaponins) and the big class of steroid saponin (steroidalsaponins) two can be divided into。The sugar of composition Saponin common are glucose, galactose, rhamnose, arabinose, xylose and glucuronic acid, galacturonic acid etc., and normal and ruscogenin C3 position-OH connects into glycoside。
Saponin is one of the important composition in natural product chemistry storehouse, has multiple biological activity, such as antitumor, antiinflammatory, immunomodulating, antiviral, antifungal, spermicide, liver-protecting activity etc.。
The pharmacological action of Saponin mainly has:
(1) two-ways regulation immunization；
(2) anti-hypoxia and antifatigue effect；
(3) low-temperature resistance stress effect；
(4) lipid peroxidation inhibition effect；
(5) the effect to central nervous system；
(6) Antimutagenesis。
Smoking has become society and the medical problem of people's most attention, and Medicated cigarette can produce the harmful substances such as harmful phenol, crotonic aldehyde, benzopyrene, nitrosamine in combustion。For harmful components in minimizing Medicated cigarette to human body associated injury, a lot of Nicotiana tabacum L. workers begin attempt to add in Medicated cigarette by some to the Chinese herbal medicine active component that human body is useful, Saponin in natural plants, and verify that its effective ingredient can enter oral cavity or respiratory tract with main flume, the generation of harmful substance can be reduced, thus playing effect locally or systemically, what reduction caused because of smoking does not accommodate harm。
So, investigate the soaping agents rate of transform in cigarette mainstream flue gas, namely its effective ingredient Saponin of Chinese herbal medicine cigarette is measured at tobacco shred to the rate of transform in its combustion product gases, can check whether effective ingredient in the process of burning and sucking is transferred in flue gas, for providing the effective ingredient adding draft Chinese medicine Medicated cigarette to the evidence of transfer in flue gas, and this type of effect manufacturing experimently medicated cigarette can be carried out entry evaluation。
Summary of the invention
It is an object of the invention to provide a kind of simple and convenient, Medicated cigarette soaping agents additive assay method of the rate of transform in main flume accurately and reliably。
For reaching above-mentioned purpose, the technical solution used in the present invention is:
1) cigarette selects: choose the cigarette that with the addition of soaping agents additive as cigarette laboratory sample；
2) trial-production cigarette shreds pre-treatment: taking the tobacco shred that with the addition of soaping agents additive and as tobacco shred laboratory sample and be placed in 250ml conical flask, add 100ml water, ultrasonic extraction 30-60min obtains tobacco shred laboratory sample extract；
3) trapping of trial-production cigarette smoke and pre-treatment:
Utilize 92mm specification cambridge filter that main flume is trapped after smoking machine burns and sucks by GB/T19609-2004 standard cigarette laboratory sample, reclaim filter disc, it is placed in 250ml conical flask, adds 100ml water, after ultrasonic extraction 30-60min, obtain cigarette laboratory sample treatment fluid；
4) chromatographic column separates:
With the syringe of 10ml as chromatography pipe, insert the D101 macroporous resin of 2-4cm and the neutral alumina of 0.5-1.5cm, first wash post with volumetric concentration 75% alcoholic solution, discard eluent, then wash post with deionized water, discard eluent and obtain chromatographic column；
The cigarette laboratory sample treatment fluid of 1.0ml, tobacco shred laboratory sample extract is accurately added respectively in each chromatographic column, again respectively with the water elution of 20-30ml, discard eluent, again with the volumetric concentration 75% alcoholic solution eluting Saponin of 20-30ml, effluent is collected in evaporating dish, be placed in the water-bath of 60 DEG C volatilize cigarette laboratory sample volatilizes solvent, tobacco shred laboratory sample volatilizes solvent；
5) drafting of standard curve:
The standard solution of preparation Saponin, detects each standard solution spectrophotography, and draws the standard curve of this Saponin according to testing result；
6) colour developing:
Volatilize solvent at cigarette laboratory sample respectively, tobacco shred laboratory sample volatilizes and accurately adds the vanillin glacial acetic acid solution that 0.2ml mass concentration is 5% in the evaporating dish of solvent, rotate evaporating dish, residue is dissolved, add 0.8ml perchloric acid, move in tool plug test tube after mixing, 60 DEG C of heating in water bath 5-15min take out, after ice-water bath cooling, add 5ml glacial acetic acid, shake up, measure its absorbance under 560nm respectively, by comparison standard curve, obtain the content of Total saponin in cigarette laboratory sample, tobacco shred laboratory sample；
7) rate of transform calculates: be calculated as follows the gypenoside rate of transform in main flume in trial-production Medicated cigarette:
The present invention is by selecting addition soaping agents additive Medicated cigarette, trap the granule phase substance matter in cigarette mainstream flue gas through cambridge filter after utilizing the suction of rotating disc type smoking machine, realized the quantitative assay of the Saponin rate of transform in main flume in trial-production Medicated cigarette by spectrophotography。Measure the content of Saponin in collected granule phase substance matter, thus realizing, to the Saponin detection by quantitative of the rate of transform in main flume added in Medicated cigarette, judging that the Saponin added in Medicated cigarette is overflowed with air-flow and sucks the probability into human body according to this。The method is accurately and reliably, simple and convenient, and the exploitation of Chinese herbal medicine cigarette is had important guiding value
Detailed description of the invention
Embodiment:
1) cigarette selects: choose the cigarette that with the addition of soaping agents additive as cigarette laboratory sample, and to choose the Cigarette being not added with soaping agents additive be cigarette control sample；
2) trial-production cigarette shreds pre-treatment: take the tobacco shred that with the addition of soaping agents additive respectively and be not added with the tobacco shred of soaping agents additive as tobacco shred laboratory sample, tobacco shred control sample, and tobacco shred laboratory sample, tobacco shred control sample are respectively placed in 250ml conical flask, adding 100ml water, ultrasonic extraction 30-60min obtains tobacco shred laboratory sample extract and tobacco shred control sample extract；
3) trapping of trial-production cigarette smoke and pre-treatment:
Utilize 92mm specification cambridge filter that main flume is trapped after smoking machine burns and sucks by GB/T19609-2004 standard cigarette laboratory sample, cigarette control sample respectively, reclaim filter disc, it is placed in 250ml conical flask, add 100ml water, cigarette laboratory sample treatment fluid, cigarette control sample treatment fluid is obtained after ultrasonic extraction 30-60min；
4) chromatographic column separates:
With the syringe of 10ml as chromatography pipe, insert the D101 macroporous resin of 2-4cm and the neutral alumina of 0.5-1.5cm, first wash post with the alcoholic solution that volumetric concentration is 75%, discard eluent, then wash post with deionized water, discard eluent and obtain chromatographic column；
The cigarette laboratory sample treatment fluid of 1.0ml, cigarette control sample treatment fluid, tobacco shred laboratory sample extract and tobacco shred control sample extract is added respectively in each chromatographic column, again respectively with the water elution of 20-30ml, discard eluent, again with the alcoholic solution eluting Saponin that the volumetric concentration of 20-30ml is 75%, effluent is collected in evaporating dish, be placed in the water-bath of 60 DEG C volatilize cigarette laboratory sample volatilizes solvent, cigarette control sample volatilizes solvent, tobacco shred laboratory sample volatilizes solvent, tobacco shred control sample volatilizes solvent；
5) drafting of standard curve:
The standard solution of preparation Saponin, detects each standard solution spectrophotography, and draws the standard curve of this Saponin according to testing result；
Detailed process, for accurately to weigh 0.0125gRe Saponin standard substance in 5ml volumetric flask, methanol constant volume, does the standard solution storing solution that concentration is 2.5mg/ml。Pipette standard reserving solution 20 μ l, 40 μ l, 60 μ l, 80 μ l, 100 μ l, 120 μ l, 140 μ l to 10ml tool plug test tubes respectively, dry solvent in 60 DEG C of hot baths, add vanillin glacial acetic acid solution and 0.8ml perchloric acid that 0.2ml mass concentration is 5%, mix rear 60 DEG C of heating in water bath 10min to take out, after ice-water bath cooling, accurately add 5ml glacial acetic acid, shake up, measure its absorbance under 560nm respectively。
Making abscissa (X) with absorbance, concentration makes vertical coordinate (Y), obtains standard curve equation。
Y=0.419X+0.039 (coefficient R is 0.9970)。
6) colour developing:
Solvent is volatilized respectively at cigarette laboratory sample, cigarette control sample volatilizes solvent, tobacco shred laboratory sample volatilizes solvent, tobacco shred control sample volatilizes and adds the vanillin glacial acetic acid solution that 0.2ml mass concentration is 5% in the evaporating dish of solvent, rotate evaporating dish, residue is dissolved, add 0.8ml perchloric acid, move in 5ml tool plug test tube after mixing, 60 DEG C of heating in water bath 5-15min take out, after ice-water bath cooling, accurately add 5ml glacial acetic acid, shake up, measure its absorbance under 560nm respectively, by comparison standard curve, obtain cigarette laboratory sample, cigarette control sample, tobacco shred laboratory sample, the content of Total saponin in tobacco shred control sample；
7) rate of transform calculates: be calculated as follows the gypenoside rate of transform in main flume in trial-production Medicated cigarette:
Testing result is as shown in the table:
More than detection parallel testing 6 times, result above is meansigma methods。
Claims (1)
1. Medicated cigarette soaping agents additive assay method of the rate of transform in main flume, it is characterised in that:
1) cigarette selects: choose the cigarette that with the addition of soaping agents additive as cigarette laboratory sample；
2) trial-production cigarette shreds pre-treatment: taking the tobacco shred that with the addition of soaping agents additive and as tobacco shred laboratory sample and be placed in 250ml conical flask, add 100ml water, ultrasonic extraction 30-60min obtains tobacco shred laboratory sample extract；
3) trapping of trial-production cigarette smoke and pre-treatment:
Utilize 92mm specification cambridge filter that main flume is trapped after smoking machine burns and sucks by GB/T19609-2004 standard cigarette laboratory sample, reclaim filter disc, it is placed in 250ml conical flask, adds 100ml water, after ultrasonic extraction 30-60min, obtain cigarette laboratory sample treatment fluid；
4) chromatographic column separates:
With the syringe of 10ml as chromatography pipe, insert the D101 macroporous resin of 2-4cm and the neutral alumina of 0.5-1.5cm, first wash post with volumetric concentration 75% alcoholic solution, discard eluent, then wash post with deionized water, discard eluent and obtain chromatographic column；
The cigarette laboratory sample treatment fluid of 1.0ml, tobacco shred laboratory sample extract is added respectively in each chromatographic column, again respectively with the water elution of 20-30ml, discard eluent, again with the volumetric concentration 75% alcoholic solution eluting Saponin of 20-30ml, effluent is collected in evaporating dish, be placed in the water-bath of 60 DEG C volatilize cigarette laboratory sample volatilizes solvent, tobacco shred laboratory sample volatilizes solvent；
5) drafting of standard curve:
The standard solution of preparation Saponin, detects each standard solution spectrophotography, and draws the standard curve of this Saponin according to testing result；
6) colour developing:
Volatilize solvent at cigarette laboratory sample respectively, tobacco shred laboratory sample volatilizes and adds the vanillin glacial acetic acid solution that 0.2ml mass concentration is 5% in the evaporating dish of solvent, rotate evaporating dish, residue is dissolved, add 0.8ml perchloric acid, move in tool plug test tube after mixing, 60 DEG C of heating in water bath 5-15min take out, after ice-water bath cooling, add 5ml glacial acetic acid, shake up, measure its absorbance under 560nm respectively, by comparison standard curve, obtain the content of Total saponin in cigarette laboratory sample, tobacco shred laboratory sample；
7) rate of transform calculates: be calculated as follows the gypenoside rate of transform in main flume in trial-production Medicated cigarette:
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Cited By (5)
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| CN108535141A (en) * | 2018-05-16 | 2018-09-14 | 云南中烟工业有限责任公司 | The detection device and detection method of Rosa Damascana ingredient the amount of migration in a kind of filter stick |
| CN108535142A (en) * | 2018-05-16 | 2018-09-14 | 云南中烟工业有限责任公司 | A kind of detection method of the Peppermint essential oil ingredient the amount of migration of special flavoring filter stick |
| CN109725098A (en) * | 2019-03-04 | 2019-05-07 | 陕西中烟工业有限责任公司 | A kind of flue gas rhynchophyllin rate of transform and filter tip rhynchophyllin rejection measuring method |
| CN112119305A (en) * | 2018-07-13 | 2020-12-22 | 日本电气硝子株式会社 | Gas detection material |
| CN114088582A (en) * | 2021-11-01 | 2022-02-25 | 河南中烟工业有限责任公司 | Method for stabilizing diffusion rate of feed liquid applied in heating cigarette |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108535141A (en) * | 2018-05-16 | 2018-09-14 | 云南中烟工业有限责任公司 | The detection device and detection method of Rosa Damascana ingredient the amount of migration in a kind of filter stick |
| CN108535142A (en) * | 2018-05-16 | 2018-09-14 | 云南中烟工业有限责任公司 | A kind of detection method of the Peppermint essential oil ingredient the amount of migration of special flavoring filter stick |
| CN112119305A (en) * | 2018-07-13 | 2020-12-22 | 日本电气硝子株式会社 | Gas detection material |
| CN112119305B (en) * | 2018-07-13 | 2022-10-28 | 日本电气硝子株式会社 | Gas detection material |
| CN109725098A (en) * | 2019-03-04 | 2019-05-07 | 陕西中烟工业有限责任公司 | A kind of flue gas rhynchophyllin rate of transform and filter tip rhynchophyllin rejection measuring method |
| CN114088582A (en) * | 2021-11-01 | 2022-02-25 | 河南中烟工业有限责任公司 | Method for stabilizing diffusion rate of feed liquid applied in heating cigarette |
| CN114088582B (en) * | 2021-11-01 | 2024-04-09 | 河南中烟工业有限责任公司 | Method for stabilizing diffusion rate of applied feed liquid in heating cigarette |
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