CN109725098A - A kind of flue gas rhynchophyllin rate of transform and filter tip rhynchophyllin rejection measuring method - Google Patents

A kind of flue gas rhynchophyllin rate of transform and filter tip rhynchophyllin rejection measuring method Download PDF

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CN109725098A
CN109725098A CN201910165684.3A CN201910165684A CN109725098A CN 109725098 A CN109725098 A CN 109725098A CN 201910165684 A CN201910165684 A CN 201910165684A CN 109725098 A CN109725098 A CN 109725098A
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rhynchophyllin
cigarette
rate
flue gas
filter
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CN109725098B (en
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樊亚玲
彭军仓
何育萍
何媛
曹永艳
王瑶
康世萍
张萌萌
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China Tobacco Shaanxi Industrial Co Ltd
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China Tobacco Shaanxi Industrial Co Ltd
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Abstract

The invention discloses a kind of flue gas rhynchophyllin rate of transform and filter tip rhynchophyllin rejection measuring method, by being balanced processing to the cigarette containing rhynchophyllin feed liquid, then respectively to pipe tobacco and filter disc, cigarette holder carries out that extract liquor is obtained by extraction, using the rhynchophyllin in gas chromatography mass spectrometry choice ion pattern measurement cigarette smoke, improve the sensitivity and accuracy of detection, the area ratio of rhynchophyllin calculates the rate of transform and rejection of the rhynchophyllin in cigarette smoke in cigarette shreds shared by area by rhynchophyllin in filter disc and filter tip, important reference frame is provided for effect research of the new type natural tobacco aromaticss in cigarette, research and development simultaneously for functional form or drug cigarette are of great significance, the present invention is added in pipe tobacco from rhynchophyllin, it is transferred to cigarette smoke after to cigarette burning and neutralizes the amount being trapped in cigarette filter, make rhynchophyllin in cigarette Effect in sensory evaluating smoking obtains specific quantitatively evaluating, while providing for the quantitatively evaluating of other function cigarette a kind of with reference to method.

Description

A kind of flue gas rhynchophyllin rate of transform and filter tip rhynchophyllin rejection measuring method
Technical field
The invention belongs to chemical analysis detection technique fields, and in particular to a kind of flue gas rhynchophyllin rate of transform and filter tip uncaria Alkali rejection measuring method.
Background technique
Rhynchophyllin is the extracted alkaloid of buckle branch of madder wort uncaria, is had for traditional Chinese medicine Uncaria genus plant One of the main component for imitating ingredient has cardiovascular system of human body, central nervous system and hematological system etc. specific raw Object active function is the common medicine source for treating hypertension prescription.In recent years, with the nutritive value of uncaria, medicinal function by Gradually recognized by people, using relatively more in terms of Chinese medicine, but it is less to compare in terms of the research of cigarette, opens third of the twelve Earthly Branches etc. within 2011 years New natural tobacco Flavour resources are artificially developed, " constituent analysis of uncaria sonicated extract and the application in cigarette " is had studied, And the research about the rhynchophyllin rate of transform in flue gas rarely has people's report.
Summary of the invention
The purpose of the present invention is to provide a kind of flue gas rhynchophyllin rate of transform and filter tip rhynchophyllin rejection measuring method, with Overcome the deficiencies in the prior art.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of flue gas rhynchophyllin rate of transform and filter tip rhynchophyllin rejection measuring method, comprising the following steps:
Step 1) will add the cigarette containing rhynchophyllin feed liquid at 21-23 DEG C, and RH is balanced at least in 58-62% environment 48 hours, then it is divided into two groups;
Step 2) separates the pipe tobacco in cigarette to first group of cigarette after Balance Treatment, then to the pipe tobacco separated Filtrate is removed after first extracting alkane derivative with petroleum ether, it is molten that ammonium hydroxide then is added to the pipe tobacco after extraction alkane derivative Liquid complete wetting pipe tobacco adds dichloromethane solution concussion extraction pipe tobacco not less than 1 hour and obtains extract liquor, to extract liquor into Row GC/MS analysis, obtains the area of rhynchophyllin in cigarette shreds;
Step 3) aspirates second group of cigarette after Balance Treatment, using flue gas trapping filter disc to drawing smoke mistake Filter, then by the flue gas trapping filter disc after cigarette filter and filtering flue gas, concussion extraction obtains at least 1 hour in methyl alcohol respectively Then extract liquor carries out GC/MS analysis to extract liquor respectively, respectively obtain in filter tip rhynchophyllin in the area and filter disc of rhynchophyllin Area;
Step 4), in flue gas the rhynchophyllin rate of transform use calculation of area, i.e., the transfer of rhynchophyllin in cigarette smoke Rate is equal to the area of rhynchophyllin in filter disc divided by the area of rhynchophyllin in cigarette shreds, the rate of transform etc. of rhynchophyllin in cigarette filter In filter tip the area of rhynchophyllin divided by the rhynchophyllin in cigarette shreds area.
Further, use ammonia spirit concentration for 5-10%.
Further, GC/MS analyzes detailed process are as follows: sample to be tested is through 7890B gas chromatograph autosampler sample introduction Afterwards, the transient evaporation under 280 DEG C of injector temperature, then brings gasifying gas into gas chromatography-mass spectrography by carrier gas Instrument carries out separation detection using the capillary chromatographic column in gas chromatograph-mass spectrometer (GC-MS), rhynchophyllin component content can be obtained As a result.
Further, gas chromatograph-mass spectrometer (GC-MS) (GC/MS) uses 7890B-5977A gas chromatography-mass spectrography Instrument.
Further, capillary chromatographic column uses HP-5MS capillary column.
Further, use GC/MS analyze in carrier gas for He, carrier gas flux: 1.2mL/min.
Further, the initial temperature of gas chromatograph column oven is risen to since 80 DEG C with 5 DEG C/min heating rate 290 DEG C, 30min is kept at 290 DEG C.
Further, using GC/MS analysis condition are as follows: transmission line temperature: 280 DEG C;Ionization mode: the source EI;Ionizing energy: 70eV;Ion source temperature: 230 DEG C;Level four bars temperature: 150 DEG C;Solvent delay: 3.5min;Scanning range: 35~500amu;Inspection Survey mode: full scan mode is qualitative, and SIM mode is quantitative;The characteristic ion (m/z) of rhynchophyllin: 384.
Compared with prior art, the invention has the following beneficial technical effects:
A kind of flue gas rhynchophyllin rate of transform of this method and filter tip rhynchophyllin rejection measuring method, by containing rhynchophyllin The cigarette of feed liquid is balanced processing, then carries out that extract liquor is obtained by extraction to pipe tobacco and filter disc, cigarette holder respectively, is added a certain amount of Dilute alkaline soln, rhynchophyllin separate out can be made, drifting alkaloids are easier to extract than reference state alkaloid, improve the effect of extraction Fruit, then using gas chromatography mass spectrometry choice ion pattern measurement extract liquor in rhynchophyllin area, improve detection sensitivity and Accuracy, the area ratio of rhynchophyllin calculates rhynchophyllin and is rolling up in cigarette shreds shared by the area by rhynchophyllin in filter disc and filter tip The rate of transform and rejection in cigarette flue gas, algorithm is simple, and accuracy is high, for the effect of new type natural tobacco aromaticss in cigarette Research provides important reference frame, and the research and development simultaneously for functional form or drug cigarette are of great significance, and the present invention is from uncaria Alkali is added in pipe tobacco, to cigarette burning after be transferred to cigarette smoke and neutralize the amount that is trapped in cigarette filter, so that rhynchophyllin is existed Effect in cigarette sensory evaluating smoking obtains specific quantitatively evaluating, while the quantitatively evaluating for other function cigarette provides one kind With reference to method.
Detailed description of the invention
Fig. 1 is the selection ion scan SIM figure of rhynchophyllin in cigarette shreds.
Fig. 2 is the SIM figure that cigarette smoke traps rhynchophyllin in filter disc and cigarette filter.
Fig. 3 is the SIM figure of rhynchophyllin in embodiment different number cigarette.
Specific embodiment
The invention will be described in further detail with reference to the accompanying drawing:
The purpose of the present invention is to provide a kind of flue gas rhynchophyllin rate of transform and filter tip rhynchophyllin rejection measuring method, adopt With gas chromatography mass spectrometry, selects ion scan detection method to improve the detection sensitivity and accuracy of rhynchophyllin, make the transfer of rhynchophyllin The calculating of rate and rejection is easier, and rhynchophyllin is made to obtain quantitatively evaluating in cigarette smoke.
A kind of flue gas rhynchophyllin rate of transform and filter tip rhynchophyllin rejection measuring method, comprising the following steps:
Step 1) will add the cigarette containing rhynchophyllin feed liquid at 21-23 DEG C, and RH is balanced at least in 58-62% environment 48 hours, two groups are then divided into, keeps the water tariff collection of cigarette consistent;
Step 2) separates the pipe tobacco in cigarette to first group of cigarette after Balance Treatment, then to the pipe tobacco separated After first extracting alkane derivative with petroleum ether, filtrate is removed, ammonia spirit complete wetting pipe tobacco is then added, then use dichloromethane Alkane solution concussion extraction pipe tobacco is not less than 1 hour, carries out GC/MS analysis to extract liquor, analyzes the amount of rhynchophyllin in cigarette shreds, It obtains;
Use ammonia spirit concentration for 5-10%;
Step 3) aspirates second group of cigarette after Balance Treatment, using flue gas trapping filter disc to drawing smoke mistake Filter, then by filter flue gas after flue gas trapping filter disc and cigarette filter respectively in methyl alcohol concussion extraction at least 1 hour, then GC/MS analysis is carried out to extract liquor respectively, respectively obtains the area of rhynchophyllin in the area and filter tip of rhynchophyllin in filter disc, is detected The rate of transform of rhynchophyllin in cigarette smoke condensates;
Step 4), in flue gas the rhynchophyllin rate of transform use calculation of area, i.e., the transfer of rhynchophyllin in cigarette smoke Rate is equal to the area of rhynchophyllin in filter disc divided by the area of rhynchophyllin in cigarette shreds, the rate of transform etc. of rhynchophyllin in cigarette filter In filter tip the area of rhynchophyllin divided by the rhynchophyllin in cigarette shreds area.
GC/MS analyzes detailed process are as follows: sample to be tested is after 7890B gas chromatograph autosampler sample introduction, at 280 DEG C Injector temperature under transient evaporation, gas chromatograph-mass spectrometer (GC-MS) then into is brought gasifying gas by carrier gas, utilizes gas phase Capillary chromatographic column in chromatograph-mas spectrometer carries out separation detection, and rhynchophyllin component content result can be obtained.
Gas chromatograph-mass spectrometer (GC-MS) (GC/MS) uses 7890B-5977A gas chromatograph-mass spectrometer (GC-MS);
Capillary chromatographic column uses HP-5MS capillary column;
Using GC/MS analysis condition: chromatographic column: HP-5MS capillary column (30m × 0.25mm × 0.25 μm);Carrier gas: He; Carrier gas flux: 1.2mL/min;Injector temperature: 280 DEG C;Split ratio: 10:1;Sample volume: 1 μ L;Temperature programming: initial temperature 290 DEG C are risen to from 80 with 5 DEG C/min heating rate, keeps 30min at 290 DEG C;Transmission line temperature: 280 DEG C;Ionization mode: The source EI;Ionizing energy: 70eV;Ion source temperature: 230 DEG C;Level four bars temperature: 150 DEG C;Solvent delay: 3.5min;Scan model It encloses: 35~500amu;Detection mode: full scan mode is qualitative, and SIM mode is quantitative;The characteristic ion (m/z) of rhynchophyllin: 384.
Experiment chooses two kinds of methanol, methylene chloride organic solvents respectively to cigarette shreds, flue gas trapping filter disc, cigarette filter In rhynchophyllin extracted, the experimental results showed that, methylene chloride when extracting filter tip, filter tip dissolution, be unsuitable for hook in filter tip The extraction of rattan alkali, therefore final choice cigarette shreds are extracted with dichloromethane, filter disc and filter tip methanol extraction.
Experiment is compared two kinds of extraction modes of ultrasonic extraction and oscillation extraction, the results showed that, ultrasonic extraction process water Temperature can be increased with extraction time, and impact analysis is as a result, event slective extraction mode is oscillation extraction, so as to guarantee test condition Consistency.
Rhynchophyllin is a kind of vegetable soda, in order to make the better separate out of rhynchophyllin, test rhynchophyllin in cigarette shreds Extraction process in, done the test of a certain amount of 5% ammonium hydroxide of addition with being not added compared with ammonium hydroxide tests, the results showed that, do not ammoniate Rhynchophyllin is not detected in the cigarette shreds extract liquor of water, and is added in the cigarette shreds extract liquor of a certain amount of 5% ammonium hydroxide and is detected Rhynchophyllin out, therefore suitable 5% ammonium hydroxide is added in the processing selection of cigarette shreds, rhynchophyllin belongs to alkaloid, is added a certain amount of Dilute alkaline soln, rhynchophyllin separate out can be made, drifting alkaloids are easier to extract than reference state alkaloid, improve the effect of extraction Fruit;
In specific implementation process: methanol concussion extraction 1 hour of the cigarette smoke aspirated trapping filter disc 50mL extracts GC/MS analysis is carried out after taking liquid to be concentrated to 0.5mL;The cigarette filter aspirated is added methanol concussion extraction 1 hour of 50mL, Extract liquor carries out GC/MS analysis after being concentrated to 0.5mL;
Containing for rhynchophyllin in the cigarette shreds, flue gas trapping filter disc and cigarette filter of 5,10,20 cigarette has been investigated in experiment Measurement is pledged love condition, and test result shows that the rhynchophyllin effect of extracting of 20 cigarette is relatively good, as shown in Figure 1 to Figure 3.
The effect of extracting of rhynchophyllin compares in 1 different number Cigarette of table, and area refers to rhynchophyllin characteristic ion 384 The area at peak:
The calculating of the rhynchophyllin rate of transform
It tests and calculation of area is used to the rhynchophyllin rate of transform, i.e., the rate of transform of rhynchophyllin is equal to filter disc in cigarette smoke The area of middle rhynchophyllin is divided by the area of rhynchophyllin in cigarette shreds, and the rate of transform of rhynchophyllin is equal to hook in filter tip in cigarette filter The area of rattan alkali divided by the rhynchophyllin in cigarette shreds area.
In flue gas in the rate of transform=filter disc of rhynchophyllin in area/cigarette shreds of rhynchophyllin rhynchophyllin area
In filter tip in rejection=filter tip of rhynchophyllin in area/cigarette shreds of rhynchophyllin rhynchophyllin area
The measurement result of the rhynchophyllin rate of transform and rejection in cigarette smoke
The rate of transform and rejection measurement result of rhynchophyllin in 2 cigarette smoke of table
The middle area of pipe tobacco Area in filter disc Area in filter tip The rate of transform (%) Rejection (%)
187941 11507 10200 6.12 5.43
This method passes through to rhynchophyllin in rhynchophyllin in rhynchophyllin in cigarette shreds, flue gas trapping filter disc, cigarette filter Measurement calculates the rate of transform and rejection of the rhynchophyllin in cigarette smoke using calculation of area, and this method has certain Novelty provides important reference frame to effect research of the new type natural tobacco aromaticss in cigarette, simultaneously for functional form Or the research and development of drug cigarette are of great significance.

Claims (8)

1. a kind of flue gas rhynchophyllin rate of transform and filter tip rhynchophyllin rejection measuring method, which comprises the following steps:
Step 1) will add the cigarette containing rhynchophyllin feed liquid at 21-23 DEG C, and it is small that RH balances at least 48 in 58-62% environment When, then it is divided into two groups;
Step 2) separates the pipe tobacco in cigarette to first group of cigarette after Balance Treatment, then first uses the pipe tobacco separated Petroleum ether removes filtrate after extracting alkane derivative, and it is complete that ammonia spirit then is added to the pipe tobacco after extraction alkane derivative Full infiltration pipe tobacco adds dichloromethane solution concussion extraction pipe tobacco not less than 1 hour and obtains extract liquor, carries out to extract liquor GC/MS analysis, obtains the area of rhynchophyllin in cigarette shreds;
Step 3) aspirates second group of cigarette after Balance Treatment, is filtered using flue gas trapping filter disc to drawing smoke, so By the flue gas trapping filter disc after cigarette filter and filtering flue gas, concussion extraction is extracted at least 1 hour in methyl alcohol respectively afterwards Then liquid carries out GC/MS analysis to extract liquor respectively, respectively obtain the face of rhynchophyllin in the area and filter disc of rhynchophyllin in filter tip Product;
Step 4), in flue gas the rhynchophyllin rate of transform use calculation of area, i.e., the rate of transform etc. of rhynchophyllin in cigarette smoke The area of rhynchophyllin is divided by the area of rhynchophyllin in cigarette shreds in filter disc, and the rate of transform of rhynchophyllin is equal to filter in cigarette filter In mouth the area of rhynchophyllin divided by the rhynchophyllin in cigarette shreds area.
2. a kind of flue gas rhynchophyllin rate of transform according to claim 1 and filter tip rhynchophyllin rejection measuring method, special Sign is, uses ammonia spirit concentration for 5-10%.
3. a kind of flue gas rhynchophyllin rate of transform according to claim 1 and filter tip rhynchophyllin rejection measuring method, special Sign is that GC/MS analyzes detailed process are as follows: sample to be tested is after 7890B gas chromatograph autosampler sample introduction, at 280 DEG C Injector temperature under transient evaporation, gas chromatograph-mass spectrometer (GC-MS) then into is brought gasifying gas by carrier gas, utilizes gas phase Capillary chromatographic column in chromatograph-mas spectrometer carries out separation detection, and rhynchophyllin component content result can be obtained.
4. a kind of flue gas rhynchophyllin rate of transform according to claim 3 and filter tip rhynchophyllin rejection measuring method, special Sign is that gas chromatograph-mass spectrometer (GC-MS) uses 7890B-5977A gas chromatograph-mass spectrometer (GC-MS).
5. a kind of flue gas rhynchophyllin rate of transform according to claim 3 and filter tip rhynchophyllin rejection measuring method, special Sign is that capillary chromatographic column uses HP-5MS capillary column.
6. a kind of flue gas rhynchophyllin rate of transform according to claim 3 and filter tip rhynchophyllin rejection measuring method, special Sign is, use GC/MS analyze in carrier gas for He, carrier gas flux: 1.2mL/min.
7. a kind of flue gas rhynchophyllin rate of transform according to claim 3 and filter tip rhynchophyllin rejection measuring method, special Sign is that the initial temperature of gas chromatograph column oven rises to 290 DEG C since 80 DEG C with 5 DEG C/min heating rate, at 290 DEG C Lower holding 30min.
8. a kind of flue gas rhynchophyllin rate of transform according to claim 3 and filter tip rhynchophyllin rejection measuring method, special Sign is, using GC/MS analysis condition are as follows: transmission line temperature: 280 DEG C;Ionization mode: the source EI;Ionizing energy: 70eV;Ion Source temperature: 230 DEG C;Level four bars temperature: 150 DEG C;Solvent delay: 3.5min;Scanning range: 35~500amu;The spy of rhynchophyllin Levy ion m/z:384.
CN201910165684.3A 2019-03-04 2019-03-04 Method for measuring rhynchophylline transfer rate and rhynchophylline retention rate of filter tip of smoke Active CN109725098B (en)

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