CN104132895B - The buffer system of total alkaloid tobacco and tobacco product is determined suitable for continuous flow method - Google Patents
The buffer system of total alkaloid tobacco and tobacco product is determined suitable for continuous flow method Download PDFInfo
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Abstract
The present invention provides a kind of buffer system that total alkaloid tobacco and tobacco product is determined suitable for continuous flow method, and the buffer system includes cushioning liquid A and buffering solution B；Wherein, cushioning liquid A is formulated as：Disodium hydrogen phosphate 60.5 83.0g, preferably 71.6g, tertiary sodium phosphate 10.1 20.2g are weighed, preferably 15.2g is dissolved with water into beaker, is then transferred in 1L volumetric flasks, scale is settled to water；Cushioning liquid B's is formulated as：Weigh the 8.0g of p-aminobenzene sulfonic acid 5.5, preferably 7.0g, the 83.0g of disodium hydrogen phosphate 60.5, preferably 71.6g, the 7.0g of sodium dihydrogen phosphate 5.0, the preferably 6.2g and 12.1g of sodium citrate 10.0, preferably 11.8g is into beaker, dissolved with water, be then transferred in 1L volumetric flasks, scale is settled to water.
Description
Technical field
The invention belongs to tobacco components detection technique field, and in particular to suitable for continuous flow method determine tobacco and
The buffer system of total alkaloid in tobacco product.
Background technology
Nicotine is the important component of tobacco, and no nicotine does not also just claim tobacco.In tobacco conventional analysis, generally by surveying
Determine the content of total alkaloid in tobacco to know the content information of nicotine.Tobacco business issue at present on total plant in tobacco
The standard that alkali is determined has：GB/T23225-2008 " the measure photometry of tobacco and tobacco product total alkaloid ", YC/T160-
" tobacco and tobacco product are total by 2002 " the measure continuous flow methods of tobacco and tobacco product total alkaloid " and YC/T468-2013
The measure of vegetable soda continuously flows (potassium rhodanide) method ".
Continuous flow method belongs to instrument analytical method, is adapted to mass sample introduction, at present using relatively broad.YC/T160-
The measuring principle of 2002 " the measure continuous flow methods of tobacco and tobacco product total alkaloid " is online using potassium cyanide and toluene-sodium-sulfonchloramide
Cyanogen chloride is generated, the pyridine ring of nicotine is disconnected, and then reacted with p-aminobenzene sulfonic acid, reaction product is in 460nm wavelength
Place is measured with colorimeter.Potassium cyanide is although relatively stable, but it is a kind of hypertoxic material, before toxic chemical
Row.For the use of potassium cyanide, there is many scruple, its Sales Channel is checked on very sternly, and many laboratory Buying Cycle are very long very
It can not extremely buy, user also needs to put on record in public security organ etc..Wanted because this method acid or alkali environment suitable to reaction has
Ask, therefore this method is the acid or alkali environment that reaction is controlled by cushioning liquid A and buffering solution B.In the method due to slow
The buffer capacity for rushing solution B is not strong, and such as the pH of some Chemical Analysis Lab water is between 5.0~6.0, cushioning liquid B
Buffer capacity do not reach test needs.The pH of this method actual use water is higher than GB6682/T-2008 " analysis experiments
The requirement of one-level water in room water specification and test methods ", uses water requirement, Chemical Analysis Lab needs in order to reach this method
One-level water is reprocessed, make this method actual use that there is certain limitation.
YC/T468-2013 " measure of tobacco and tobacco product total alkaloid continuously flows (potassium rhodanide) method " measure
Principle is to generate cyanogen chloride online using potassium rhodanide and sodium dichloro cyanurate, disconnects the pyridine ring of nicotine, so with it is right
Aminobenzenesulfonic acid is reacted, and reaction product is measured at 460nm wavelength with colorimeter.Compared to YC/T160-2002,
YC/T468-2013 improves the processing safety of total alkaloid measure without using potassium cyanide.To anti-in YC/T468-2013
Answer suitable acid or alkali environment also to require, the acid or alkali environment of reaction controlled again by cushioning liquid A and buffering solution B,
Although the acid or alkali environment of reaction can be controlled effectively, chemicals usage when this method cushioning liquid A and buffering solution B are prepared
Larger, the use equally to this method is made troubles.
The content of the invention
In order to overcome the defect of prior art, the present invention provides a kind of new continuous flow method that is applied to and determines tobacco and cigarette
The buffer system of total alkaloid in straw-made articles.The buffer system be applied to using continuous flowing (potassium rhodanide) method determine tobacco and
Total alkaloid in tobacco product.Using the buffer system of the present invention when reducing preparation energy while the usage amount of chemicals
Control reaction acid or alkali environment, it is ensured that cyanogen chloride is broken the pyridine ring of vegetable soda, so with the reaction of p-aminobenzene sulfonic acid, make
Reaction is carried out under the conditions of the acid or alkali environment of needs.
The present invention adopts the following technical scheme that to realize.
On the one hand, the present invention provides a kind of the slow of total alkaloid suitable for continuous flow method measure tobacco and tobacco product
System is rushed, the buffer system includes cushioning liquid A and buffering solution B；
Wherein, cushioning liquid A is formulated as：Weigh disodium hydrogen phosphate 60.5-83.0g, preferably 71.6g；Tertiary sodium phosphate
10.1-20.2g, preferably 15.2g are dissolved into beaker with water, be then transferred in 1L volumetric flasks, scale is settled to water；
Cushioning liquid B's is formulated as：Weigh p-aminobenzene sulfonic acid 5.5-8.0g, preferably 7.0g；Disodium hydrogen phosphate 60.5-
83.0g, preferably 71.6g；Sodium dihydrogen phosphate 5.0-7.0g, preferably 6.2g and sodium citrate 10.0-12.1g, be preferably
11.8g is dissolved into beaker with water, is then transferred in 1L volumetric flasks, scale is settled to water.
Above-mentioned disodium hydrogen phosphate, tertiary sodium phosphate, sodium dihydrogen phosphate, sodium citrate can be the form that is conventionally present, for example
Disodium hydrogen phosphate exists in 12 crystallization water forms, and tertiary sodium phosphate exists in 12 crystallization water forms, and sodium dihydrogen phosphate is with 2 knots
Brilliant water form is present, and sodium citrate exists in 2 crystallization water forms.
Preferably, in above-mentioned buffer system, the amount ratio between cushioning liquid A and cushioning liquid B is 1：2 to 1：1 (body
Product ratio), preferably 3：4 (volume ratios).
On the other hand, a kind of above-mentioned buffer system of present invention offer is total in continuous flow method determines tobacco or tobacco product
Purposes in the method for vegetable soda.
Preferably, the continuous flow method determines the method for total alkaloid in tobacco and tobacco product and refers to use thiocyanic acid
Potassium and sodium dichloro cyanurate generate cyanogen chloride online, and cyanogen chloride is with the total alkaloid in the tobacco or tobacco product (with cigarette
Alkali meter) reaction, the pyridine ring of nicotine is disconnected, and then reacted with p-aminobenzene sulfonic acid, reaction product colorimeter exists
Determined at 460nm.
Preferably, the continuous flow method determines the method for total alkaloid in tobacco and tobacco product and included：
(1) preparation of sample：Tobacco sample is prepared by YC/T31, and determines its moisture, then using 5% acetic acid pair
Tobacco sample is extracted, filtering, obtains filtrate standby；
(2) preparation of standard liquid：
Nicotine or nicotine salt are weighed with 5% acetate dissolution, at least five working stamndard liquid, the standard prepared is configured to
Nicotine content concentration range is 0.5~7% in solution；
(3) preparation of reaction reagent：
Potassium thiocyanate solution is formulated as：Potassium rhodanide is weighed into beaker, is dissolved with water, 250mL capacity is then transferred to
In bottle, water constant volume is used, the solution concentration scope is 0.09~0.21mol/L, preferably 0.12mol/L.
Sodium dichloro cyanurate solution is formulated as：Sodium dichloro cyanurate is weighed into beaker, is dissolved with water, Ran Houzhuan
Enter in 250mL volumetric flasks, use water constant volume, the solution concentration scope is 0.02~0.06mol/L, preferably 0.04mol/L.
Cushioning liquid A preparation：Weigh disodium hydrogen phosphate 60.5-83.0g, preferably 71.6g；Tertiary sodium phosphate 10.1-
20.2g, preferably 15.2g are dissolved into beaker with water, be then transferred in 1L volumetric flasks, scale is settled to water；
Cushioning liquid B preparation：Weigh p-aminobenzene sulfonic acid 5.5-8.0g, preferably 7.0g；Disodium hydrogen phosphate 60.5-
83.0g, preferably 71.6g；, sodium dihydrogen phosphate 5.0-7.0g, preferably 6.2g and sodium citrate 10.0-12.1g, be preferably
11.8g is dissolved into beaker with water, is then transferred in 1L volumetric flasks, scale is settled to water；
Above-mentioned disodium hydrogen phosphate, tertiary sodium phosphate, sodium dihydrogen phosphate, sodium citrate can be the form that is conventionally present, for example
Disodium hydrogen phosphate exists in 12 crystallization water forms, and tertiary sodium phosphate exists in 12 crystallization water forms, and sodium dihydrogen phosphate is with 2 knots
Brilliant water form is present, and sodium citrate exists in 2 crystallization water forms.
Detoxicating liquid A's is formulated as：1g citric acids, 10g ferrous sulfate are weighed into beaker, is dissolved with water, is then transferred to 1L
In volumetric flask, scale is settled to water；Detoxicating liquid A main function is the toxicity for the cyanogen chloride that reduction has neither part nor lot in reaction, should
Detoxicating liquid A is identical with the detoxicating liquid A in YC/T160-2002 (potassium cyanide method).
Detoxicating liquid B's is formulated as：10g sodium carbonate is weighed into beaker, is dissolved with water, is then transferred in 1L volumetric flasks, is used
Water is settled to scale；Detoxicating liquid B main function is the toxicity for the cyanogen chloride that reduction has neither part nor lot in reaction, detoxicating liquid B and YC/
T160-2002 (potassium cyanide method) detoxicating liquid B is identical.
(4) Continuous Flow Analysis the instrument filtrate of detecting step (1) and step (2) under the reaction system of step (3) are used
Working stamndard liquid；
(5) total alkaloid in sample is calculated according to following formula：
In formula, X：The Instrument observation value of sample, every milliliter (mg/mL) of unit milligram；
V：The extract volume of addition, unit is milliliter (mL)；
m：Sample quality, unit is gram (g)；
W：The percent water of sample, % (mass fraction)；
Preferably, in the above method, cushioning liquid A and cushioning liquid B amount ratio is 1：2 to 1：1 (volume ratio), preferably
For 3：4 (volume ratios), the amount ratio causes the pH value of reaction system to control between 6.0~7.5；
Preferably, in the above method, potassium thiocyanate solution and sodium dichloro cyanurate solution concentration ratio are 2.5：1 to 3.5：
1, preferably 3：1.
Preferably, in the above method, the operational factor of Continuous Flow Analysis instrument is：Sample introduction cleaning is than being 1.5, sample introduction frequency
48 glasss/hour, gain 18-60,2.85 volts of light intensity.
In the above-mentioned methods, the preparation of sample, the preparation of standard liquid, the preparation of reaction reagent order can change.
In a specific embodiment, the method that the continuous flow method determines total alkaloid in tobacco and tobacco product
Comprise the following steps that：
(1) using the total alkaloid in 5% Extraction of Acetic Acid offal sample (offal sample is prepared by YC/T31)；
(2) according to connecting line shown in Fig. 1：
(3) certain density cushioning liquid A and B, detoxicating liquid A, detoxicating liquid B, potassium thiocyanate solution and dichloro isocyanide are configured
Uric acid sodium solution；
(4) total alkaloid standard liquid is prepared using 5% acetic acid；
(5) by the pump line in total alkaloid module, according to peristaltic pump is caught in shown in Fig. 1, (internal diameter of different pump lines is not in module
Together, the flow velocity of corresponding reagent is different, reaches that control participates in the mesh of reaction reagent ratio by controlling the flow velocity of reaction reagent
's；It is in order that the solution in pipeline is well mixed to add air pump line), pump cover is covered, Reagent Tube is put into water；Open
Power supply, opens detector, peristaltic pump, automatic sampler, computer；Switch on peristaltic pump is allocated to Run；Double-click in computer
Connect Continuous Flow Analysis work station icon；The charting on work station is clicked on, after successful connection, wriggling pump operation, water is just
It is pumped in pipeline and cleans, scavenging period is 20~30min；, will not after after baseline stability (now baseline fluctuation be less than ± 1%)
Same pipeline is put into corresponding reagent, is continued to run with, is during which adjusted base in the charting windows that work station is ejected
Line is to 5% or so；Operation program is worked out according to the prompting of Analysis in the drop-down menu of work station, baseline stability is treated, clicks on
Run in work station can be run；Program end of run is treated, different pipelines is relay in backwater, 20~30min is cleaned；
After the completion of cleaning, automatic sampler is closed successively, peristaltic pump, detector removes pump cover, close power supply.
Above-mentioned steps (1) are specially：Offal sample (offal sample is prepared by YC/T31) is weighed to 50mL tool plug triangles
In bottle, 5% acetic acid vibration 30min is added, is filtered using qualitative filter paper.
Above-mentioned steps (2) are specially：According to shown in Fig. 1, pump line is arranged on peristaltic pump, pump cover is added, is cleaned with water
Pipeline.
In above-mentioned steps (3), cushioning liquid A's is formulated as：Weigh 71.6 grams disodium hydrogen phosphate, 15.2 grams of tricresyl phosphate
Sodium is dissolved into beaker with water, is then transferred in 1L volumetric flasks, scale is settled to water.Wherein, disodium hydrogen phosphate, tricresyl phosphate
Sodium can be the form that is conventionally present, and such as disodium hydrogen phosphate exists in 12 crystallization water forms, and tertiary sodium phosphate is with 12 crystallizations water
Form is present.
In above-mentioned steps (3), cushioning liquid B's is formulated as：Weigh 7g p-aminobenzene sulfonic acid, 71.6 grams of disodium hydrogen phosphates,
6.2 grams of sodium dihydrogen phosphates and 11.8 grams of sodium citrates are dissolved with water, are then transferred in 1L volumetric flasks, use water constant volume into beaker
To scale.Wherein, disodium hydrogen phosphate, sodium dihydrogen phosphate, sodium citrate can be the form that is conventionally present, such as disodium hydrogen phosphate with
12 crystallization water forms are present, and sodium dihydrogen phosphate exists in 2 crystallization water forms, and sodium citrate exists in 2 crystallization water forms.
In above-mentioned steps (3), detoxicating liquid A's is formulated as：1g citric acids, 10g ferrous sulfate are weighed into beaker, with water-soluble
Solution, is then transferred in 1L volumetric flasks, scale is settled to water.Detoxicating liquid A main function is that reduction has neither part nor lot in reaction cyanogen chloride
Toxicity.Detoxicating liquid A is identical with YC/T160-2002 (potassium cyanide method) detoxicating liquid A in step (3).
Detoxicating liquid B's is formulated as in above-mentioned steps (3)：10g sodium carbonate is weighed into beaker, is dissolved, is then transferred to water
In 1L volumetric flasks, scale is settled to water.Detoxicating liquid B main function is the toxicity that reduction has neither part nor lot in reaction cyanogen chloride.Step
(3) detoxicating liquid B is identical with YC/T160-2002 (potassium cyanide method) detoxicating liquid B in.
In above-mentioned steps (3), potassium thiocyanate solution is formulated as：Appropriate potassium rhodanide is weighed into beaker, is dissolved with water,
Then it is transferred in 250mL volumetric flasks, uses water constant volume.The solution concentration scope is 0.09~0.21mol/L.
In above-mentioned steps (3), sodium dichloro cyanurate solution is formulated as：Appropriate sodium dichloro cyanurate is weighed to beaker
In, dissolved, be then transferred in 250mL volumetric flasks with water, use water constant volume.The solution concentration scope is 0.02~0.06mol/L.
In above-mentioned steps (3), potassium thiocyanate solution and sodium dichloro cyanurate solution concentration proportioning about 3：1.
In above-mentioned steps (4), standard liquid is formulated as：Appropriate nicotine is weighed in 250mL volumetric flasks, it is molten with 5% acetic acid
Solution, is settled to scale.This solution is nicotine storing solution, nicotine content about 1.6mg/mL or so.At least 5 are prepared by nicotine storing solution
Individual working stamndard liquid, its concentration range should cover the estimated sample size detected.
In above-mentioned steps (5), the operational factor of Continuous Flow Analysis instrument is：Sample introduction cleaning is than being 1.5, sample introduction frequency 48
Cup/hour, gain 18-60,2.85 volts of light intensity.
Above-mentioned continuous flow method is determined in tobacco and tobacco product in total alkaloid, sample pre-treatments and YC/T468-2013
" measure of tobacco and tobacco product total alkaloid continuously flows (potassium rhodanide) method " unanimously, changes cushioning liquid A and buffering
Solution B, establishes a kind of new buffer system, reduces the usage amount of chemicals when preparing cushioning liquid A and buffering solution B, together
When ensure that the uniformity of same YC/T468-2013 methods test result.
At least there is following beneficial effect in the present invention：
The acid or alkali environment that the present invention can control to react before dialyzer using a kind of new cushioning liquid A, it is ensured that before dialyzer
Solution ph can't be impacted between 6.0~11.0 to the cushioning liquid B acid or alkali environments controlled；
The present invention can control the acid or alkali environment of reaction using a kind of new cushioning liquid B, regulation solution ph 6.0~
Between 7.5, it is ensured that cyanogen chloride is broken the pyridine ring of vegetable soda, so with the reaction of p-aminobenzene sulfonic acid, reaction need
Carried out under the conditions of acid or alkali environment；
The present invention establishes a kind of new continuous flowing (potassium rhodanide) method that is applied to and determined tobacco and tobacco product always
The buffer system of vegetable soda；
Using the continuous flow method of buffer system of the invention compared with YC/T468-2013, preparation cushioning liquid is reduced
The usage amount of chemicals when A and buffering solution B, while ensureing that data are consistent with YC/T468-2013.
Brief description of the drawings
Fig. 1 is the piping diagram that total alkaloid in tobacco and tobacco product is determined using continuous flow method.
Embodiment
With reference to embodiment, the present invention is described further.These embodiments are intended to help the content for illustrating invention
Rather than limitation the scope of the present invention.
Embodiment 1：The measure of total alkaloid in flue-cured tobacco
1) sample pre-treatments
Flue-cured tobacco offal is prepared into sample according to YC/T31, and determines its moisture, then weigh 0.25g samples in
In 50mL conical flask with stopper, 25mL5% acetic acid is added, plug is covered, (rotating speed is vibrated on the oscillator>150rpm) extract
30min.With fast qualitative filter paper extracted by filtration liquid, preceding 2mL~3mL filtrates are discarded, subsequent filtrate, which performs an analysis, after collection is used.
2) preparation of reaction reagent
Cushioning liquid A's is formulated as：Weigh 71.6 grams of disodium hydrogen phosphate (12 crystallizations water), tertiary sodium phosphate (12 crystallizations
Water) 15.2 grams into beaker, dissolved with water, be then transferred in 1L volumetric flasks, scale is settled to water.
Cushioning liquid B's is formulated as：Weigh 7g p-aminobenzene sulfonic acid, 71.6 grams of disodium hydrogen phosphate (12 crystallizations water), phosphorus
11.8 grams of 6.2 grams of acid dihydride sodium (2 crystallizations water) and sodium citrate (2 crystallizations water) are dissolved with water, are then transferred into beaker
In 1L volumetric flasks, scale is settled to water with water constant volume.
In following measure, the amount ratio of cushioning liquid A and buffering solution B is 3：4 (volume ratios).
Detoxicating liquid A, detoxicating liquid B, preparation and the YC/T468-2013 of potassium thiocyanate solution and sodium dichloro cyanurate solution
Correspondence reagent is identical in " measure of tobacco and tobacco product total alkaloid continuously flows (potassium rhodanide) method ".
It is specific as follows：
Removing toxic substances solution A is formulated as：
1g citric acids, 10g ferrous sulfate are weighed into beaker, is dissolved with water, is then transferred in 1000mL volumetric flasks, uses water
It is settled to scale.
Removing toxic substances solution B is formulated as：
10g sodium carbonate is weighed into beaker, is dissolved with water, is then transferred in 1000mL volumetric flasks, scale is settled to water.
Potassium thiocyanate solution is formulated as：
2.88g potassium rhodanides are weighed into beaker, are dissolved with water, are then transferred in 250mL volumetric flasks, quarter is settled to water
Degree.
Sodium dichloro cyanurate solution is formulated as：
2.20g sodium dichloro cyanurates are weighed into beaker, are dissolved with water, are then transferred in 250mL volumetric flasks, it is fixed with water
Hold to scale.The solution should be now with the current.
3) preparation of standard liquid
Appropriate total alkaloid standard liquid (there is card mark thing in countries tobacco Quality Supervision and Inspection Center) is weighed in 250mL volumetric flasks
In, 0.0001g is accurate to, is dissolved with water, scale is settled to, this solution is nicotine standard storing solution, nicotine content should be
1.6mg/mL left and right.12.5mL, 10mL, 5mL, 2.5mL, 0.5mL nicotine standard storing solution are pipetted respectively to 100mL volumetric flasks
In, with 5% acetic acid constant volume, the concentration for obtaining work standard liquid is respectively 1.2105mg/mL, 0.9683mg/mL, 0.4842mg/
mL、0.2421mg/mL、0.0484mg/mL。
4) analytical instrument used in the present invention is the AA3 type Continuous Flow Analysises of German Bran ＆ Luebbe's production
Instrument.The pipeline for determining total alkaloid in tobacco and tobacco product using continuous flow method is as shown in Figure 1.By in total alkaloid module
Pump line according to peristaltic pump is caught in shown in Fig. 1, (internal diameter of different pump lines is different in module, and the flow velocity of corresponding reagent is different, leads to
The flow velocity of control reaction reagent is crossed to reach that control participates in the purpose of reaction reagent ratio；It is in order that pipeline to add air pump line
In solution be well mixed), pump cover is covered, Reagent Tube is put into water；Turn on the power, opening detector, peristaltic pump, automatically
Injector, computer；Switch on peristaltic pump is allocated to Run, connection Continuous Flow Analysis work station is double-clicked；Click on work station
Charting, after successful connection, wriggling pump operation, water be just pumped in pipeline clean, scavenging period be 20~30min；Treat
After baseline stability (now baseline fluctuation is less than ± 1%), different pipelines is put into corresponding reagent, continued to run with, the phase
Between baseline is adjusted in the charting windows that work station is ejected to 5% or so；According in the drop-down menu of work station
Analysis prompting establishment operation program, treats baseline stability, the Run clicked in work station can be run；Treat program operation knot
Beam, different pipelines is relay in backwater, cleans 20~30min；After the completion of cleaning, automatic sampler is closed successively, is wriggled
Pump, detector removes pump cover, closes power supply.
5) standard curve is using a curve；
6) data are calculated
The peak height at total alkaloid peak carries out regression analysis to its respective concentration, obtains standard curve.Then by detecting sample
The peak height of product, the corresponding concentration of sample, i.e. Instrument observation value are obtained by standard curve.
Total alkaloid content in terms of butt, is drawn by following formula：
In formula, X：The Instrument observation value of sample, every milliliter (mg/mL) of unit milligram；
V：The extract volume of addition, unit is milliliter (extract volume is 25mL herein)；
m：Sample quality, unit is gram (g)；
W：The percent water of sample, % (mass fraction)；
It is 0.5~3% to calculate total alkaloid content in flue-cured tobacco by above formula.
Embodiment 2：The measure of total alkaloid in burley tobaccos
1) sample pre-treatments
Burley tobaccos offal is prepared into sample according to YC/T31, and determines its moisture, 0.25g burley tobaccos are then weighed
Sample adds 25mL5% acetic acid, covers plug in 50mL conical flask with stopper, and (rotating speed is vibrated on the oscillator>150rpm) extract
Take 30min.With fast qualitative filter paper extracted by filtration liquid, preceding 2mL~3mL filtrates are discarded, subsequent filtrate, which performs an analysis, after collection is used.
2) preparation of reaction reagent
Cushioning liquid A's is formulated as：Weigh 71.6 grams of disodium hydrogen phosphate (12 crystallizations water), tertiary sodium phosphate (12 crystallizations
Water) 15.2 grams into beaker, dissolved with water, be then transferred in 1L volumetric flasks, scale is settled to water.
Cushioning liquid B's is formulated as：Weigh 7g p-aminobenzene sulfonic acid, 71.6 grams of disodium hydrogen phosphate (12 crystallizations water), phosphorus
11.8 grams of 6.2 grams of acid dihydride sodium (2 crystallizations water) and sodium citrate (2 crystallizations water) are dissolved with water, are then transferred into beaker
In 1L volumetric flasks, scale is settled to water with water constant volume.
In following measure, the amount ratio of cushioning liquid A and buffering solution B is that please supplement 3：4 (volume ratios).
Detoxicating liquid A, detoxicating liquid B, preparation and the YC/T468-2013 of potassium thiocyanate solution and sodium dichloro cyanurate solution
Correspondence reagent is identical in " measure of tobacco and tobacco product total alkaloid continuously flows (potassium rhodanide) method ".
It is specific as follows：
Removing toxic substances solution A is formulated as：
1g citric acids, 10g ferrous sulfate are weighed into beaker, is dissolved with water, is then transferred in 1000mL volumetric flasks, uses water
It is settled to scale.
Removing toxic substances solution B is formulated as：
10g sodium carbonate is weighed into beaker, is dissolved with water, is then transferred in 1000mL volumetric flasks, scale is settled to water.
Potassium thiocyanate solution is formulated as：
2.88g potassium rhodanides are weighed into beaker, are dissolved with water, are then transferred in 250mL volumetric flasks, quarter is settled to water
Degree.
Sodium dichloro cyanurate solution is formulated as：
2.20g sodium dichloro cyanurates are weighed into beaker, are dissolved with water, are then transferred in 250mL volumetric flasks, it is fixed with water
Hold to scale.The solution should be now with the current.
3) preparation of standard liquid
Appropriate total alkaloid standard liquid (there is card mark thing in countries tobacco Quality Supervision and Inspection Center) is weighed in 250mL volumetric flasks
In, 0.0001g is accurate to, is dissolved with water, scale is settled to, this solution is nicotine standard storing solution, nicotine content should be
1.6mg/mL left and right.12.5mL, 10mL, 5mL, 2.5mL, 0.5mL nicotine standard storing solution are pipetted respectively to 100mL volumetric flasks
In, with 5% acetic acid constant volume, the concentration for obtaining work standard liquid is respectively 1.2105mg/mL, 0.9683mg/mL, 0.4842mg/
mL、0.2421mg/mL、0.0484mg/mL。
4) analytical instrument used in the present invention is the AA3 type Continuous Flow Analysises of German Bran ＆ Luebbe's production
Instrument.The pipeline for determining total alkaloid in tobacco and tobacco product using continuous flow method is as shown in Figure 1.By in total alkaloid module
Pump line according to peristaltic pump is caught in shown in Fig. 1, (internal diameter of different pump lines is different in module, and the flow velocity of corresponding reagent is different, leads to
The flow velocity of control reaction reagent is crossed to reach that control participates in the purpose of reaction reagent ratio；It is in order that pipeline to add air pump line
In solution be well mixed), pump cover is covered, Reagent Tube is put into water；Turn on the power, opening detector, peristaltic pump, automatically
Injector, computer；Switch on peristaltic pump is allocated to Run, connection Continuous Flow Analysis work station is double-clicked；Click on work station
Charting, after successful connection, wriggling pump operation, water be just pumped in pipeline clean, scavenging period be 20~30min；Treat
After baseline stability (now baseline fluctuation is less than ± 1%), different pipelines is put into corresponding reagent, continued to run with, the phase
Between baseline is adjusted in the charting windows that work station is ejected to 5% or so；According in the drop-down menu of work station
Analysis prompting establishment operation program, treats baseline stability, the Run clicked in work station can be run；Treat program operation knot
Beam, different pipelines is relay in backwater, cleans 20~30min；After the completion of cleaning, automatic sampler is closed successively, is wriggled
Pump, detector removes pump cover, closes power supply.
5) standard curve is using a curve；
6) data are calculated
The peak height at total alkaloid peak carries out regression analysis to its respective concentration, obtains standard curve.Then by detecting sample
The peak height of product, the corresponding concentration of sample, i.e. Instrument observation value are obtained by standard curve.
Total alkaloid content in terms of butt, is drawn by following formula：
In formula, X：The Instrument observation value of sample, every milliliter (mg/mL) of unit milligram；
V：The extract volume of addition, unit is milliliter (extract volume is 25mL herein)；
m：Sample quality, unit is gram (g)；
W：The percent water of sample, % (mass fraction)；
It is 1~5% to calculate total alkaloid content in burley tobaccos by above formula.
Embodiment 3：The measure of total alkaloid in cigarette
1) sample pre-treatments
Cigarette shreds are prepared into sample according to YC/T31, and determine its moisture, 0.25g cigarette samples are then weighed
In 50mL conical flask with stopper, 25mL5% acetic acid is added, plug is covered, (rotating speed is vibrated on the oscillator>150rpm) extract
30min.With fast qualitative filter paper extracted by filtration liquid, preceding 2mL~3mL filtrates are discarded, subsequent filtrate, which performs an analysis, after collection is used.
2) preparation of reaction reagent
Cushioning liquid A's is formulated as：Weigh 83.0 grams of disodium hydrogen phosphate (12 crystallizations water), tertiary sodium phosphate (12 crystallizations
Water) 20.0 grams into beaker, dissolved with water, be then transferred in 1L volumetric flasks, scale is settled to water.
Cushioning liquid B's is formulated as：Weigh 7g p-aminobenzene sulfonic acid, disodium hydrogen phosphate (12 crystallizations water) gram, di(2-ethylhexyl)phosphate
10.4 grams of 5.2 grams of hydrogen sodium (2 crystallizations water) and sodium citrate (2 crystallizations water) are dissolved into beaker with water, are then transferred to 1L appearances
In measuring bottle, scale is settled to water with water constant volume.
In following measure, the amount ratio of cushioning liquid A and buffering solution B is 3：4 (volume ratios)
Detoxicating liquid A, detoxicating liquid B, preparation and the YC/T468-2013 of potassium thiocyanate solution and sodium dichloro cyanurate solution
Correspondence reagent is identical in " measure of tobacco and tobacco product total alkaloid continuously flows (potassium rhodanide) method ".
It is specific as follows：
Removing toxic substances solution A is formulated as：
1g citric acids, 10g ferrous sulfate are weighed into beaker, is dissolved with water, is then transferred in 1000mL volumetric flasks, uses water
It is settled to scale.
Removing toxic substances solution B is formulated as：
10g sodium carbonate is weighed into beaker, is dissolved with water, is then transferred in 1000mL volumetric flasks, scale is settled to water.
Potassium thiocyanate solution is formulated as：
2.88g potassium rhodanides are weighed into beaker, are dissolved with water, are then transferred in 250mL volumetric flasks, quarter is settled to water
Degree.
Sodium dichloro cyanurate solution is formulated as：
2.20g sodium dichloro cyanurates are weighed into beaker, are dissolved with water, are then transferred in 250mL volumetric flasks, it is fixed with water
Hold to scale.The solution should be now with the current.
3) preparation of standard liquid
Appropriate total alkaloid standard liquid (there is card mark thing in countries tobacco Quality Supervision and Inspection Center) is weighed in 250mL volumetric flasks
In, 0.0001g is accurate to, is dissolved with water, scale is settled to, this solution is nicotine standard storing solution, nicotine content should be
1.6mg/mL left and right.12.5mL, 10mL, 5mL, 2.5mL, 0.5mL nicotine standard storing solution are pipetted respectively to 100mL volumetric flasks
In, with 5% acetic acid constant volume, the concentration for obtaining work standard liquid is respectively 1.2105mg/mL, 0.9683mg/mL, 0.4842mg/
mL、0.2421mg/mL、0.0484mg/mL。
4) analytical instrument used in the present invention is the AA3 type Continuous Flow Analysises of German Bran ＆ Luebbe's production
Instrument.The pipeline for determining total alkaloid in tobacco and tobacco product using continuous flow method is as shown in Figure 1.By in total alkaloid module
Pump line according to peristaltic pump is caught in shown in Fig. 1, (internal diameter of different pump lines is different in module, and the flow velocity of corresponding reagent is different, leads to
The flow velocity of control reaction reagent is crossed to reach that control participates in the purpose of reaction reagent ratio；It is in order that pipeline to add air pump line
In solution be well mixed), pump cover is covered, Reagent Tube is put into water；Turn on the power, opening detector, peristaltic pump, automatically
Injector, computer；Switch on peristaltic pump is allocated to Run, connection Continuous Flow Analysis work station is double-clicked；Click on work station
Charting, after successful connection, wriggling pump operation, water be just pumped in pipeline clean, scavenging period be 20~30min；Treat
After baseline stability (now baseline fluctuation is less than ± 1%), different pipelines is put into corresponding reagent, continued to run with, the phase
Between baseline is adjusted in the charting windows that work station is ejected to 5% or so；According in the drop-down menu of work station
Analysis prompting establishment operation program, treats baseline stability, the Run clicked in work station can be run；Treat program operation knot
Beam, different pipelines is relay in backwater, cleans 20~30min；After the completion of cleaning, automatic sampler is closed successively, is wriggled
Pump, detector removes pump cover, closes power supply.
5) standard curve is using a curve；
6) data are calculated
The peak height at total alkaloid peak carries out regression analysis to its respective concentration, obtains standard curve.Then by detecting sample
The peak height of product, the corresponding concentration of sample, i.e. Instrument observation value are obtained by standard curve.
Total alkaloid content in terms of butt, is drawn by following formula：
In formula, X：The Instrument observation value of sample, every milliliter (mg/mL) of unit milligram；
V：The extract volume of addition, unit is milliliter (extract volume is 25mL herein)；
m：Sample quality, unit is gram (g)；
W：The percent water of sample, % (mass fraction)；
It is 0.5~4% to calculate total alkaloid content in cigarette by above formula.
Embodiment 4：Continuous flow method using buffer system of the present invention and the continuous flow method using other buffer systems
The comparative study of testing result
Unless otherwise specified, the reagent and method that the present embodiment is used are consistent with YC/T468-2013.
The continuous flow method and other buffer systems of buffer system of the present invention is respectively adopted (except buffer system and the present invention not
With outside, remaining reagent all same) to flue-cured tobacco, burley tobaccos, Turkish tobaccos, five kinds of samples of Virginian-type cigarette and blended type cigarette are carried out
Determine, its measurement result is shown in Table 1~table 7.It was found from 1~table of table 7：Same sample uses the continuous flowing of buffer system of the present invention
Method measurement result is respectively less than 0.04 relative to the absolute difference of YC/T468-2013 methods, and other buffer system measurement results are relative
It is larger in the absolute difference of YC/T468-2013 methods.Listed in table 8 and same sample is respectively adopted buffering of the present invention
The measurement result of the continuous flow method of system, the continuous flow method of other buffer systems and YC/T468-2013 methods is matched
T examines (α=0.05), as a result, use the continuous flow method result of buffer system of the present invention for P=0.35>0.05, illustrate two kinds
Analysis method does not have significant difference, shows the continuous flow method using buffer system of the present invention and YC/T468-2013 standard sides
Method result is consistent；Using the detection method P of other buffer systems<0.05, illustrate that two kinds of analysis methods have significant difference, table
It is bright inconsistent using the method and YC/T468-2013 standard method test results of other buffer systems.
Table 1 is compared using the continuous flow method of buffer system of the present invention with YC/T468-2013 method measurement results
The disodium hydrogen phosphate of table 2, borax system and YC/T468-2013 method measurement results are compared
The sodium dihydrogen phosphate of table 3, sodium hydroxide system and YC/T468-2013 method measurement results are compared
The sodium phosphate of table 4, citric acid systems and YC/T468-2013 method measurement results are compared
The sodium citrate of table 5, citric acid systems and YC/T468-2013 method measurement results are compared
The calmine of table 6, hydrochloric acid system and YC/T468-2013 method measurement results are compared
The trishydroxymethylaminomethane of table 7, hydrochloric acid system and YC/T468 method measurement results are compared
The different buffer systems of table 8 and YC/T468-2013 method measurement result paired t-tests
Claims (26)
1. a kind of cushioning liquid that total alkaloid tobacco and tobacco product is determined suitable for continuous flow method, the cushioning liquid bag
A containing cushioning liquid and buffering solution B；
Wherein, cushioning liquid A is formulated as：Weigh disodium hydrogen phosphate 60.5-83.0g；Tertiary sodium phosphate 10.1-20.2g is to beaker
In, dissolved with water, be then transferred in 1L volumetric flasks, scale is settled to water；
Cushioning liquid B's is formulated as：Weigh p-aminobenzene sulfonic acid 5.5-8.0g, disodium hydrogen phosphate 60.5-83.0g, biphosphate
Sodium 5.0-7.0g and sodium citrate 10.0-12.1g are dissolved into beaker with water, are then transferred in 1L volumetric flasks, are settled to water
Scale；
Wherein, the amount ratio between the cushioning liquid A and the cushioning liquid B is 3：4.
2. cushioning liquid according to claim 1, it is characterised in that weigh disodium hydrogen phosphate when preparing cushioning liquid A
71.6g。
3. cushioning liquid according to claim 1, it is characterised in that weigh tertiary sodium phosphate when preparing cushioning liquid A
15.2g。
4. cushioning liquid according to claim 1, it is characterised in that weigh p-aminobenzene sulfonic acid when preparing cushioning liquid B
7.0g。
5. cushioning liquid according to claim 1, it is characterised in that weigh disodium hydrogen phosphate when preparing cushioning liquid B
71.6g。
6. cushioning liquid according to claim 1, it is characterised in that weigh sodium dihydrogen phosphate when preparing cushioning liquid B
6.2g。
7. cushioning liquid according to claim 1, it is characterised in that weigh sodium citrate when preparing cushioning liquid B
11.8g。
8. cushioning liquid according to claim 1, it is characterised in that cushioning liquid A's is formulated as：Weigh disodium hydrogen phosphate
71.6g；Tertiary sodium phosphate 15.2g is dissolved into beaker with water, is then transferred in 1L volumetric flasks, scale is settled to water.
9. cushioning liquid according to claim 1, it is characterised in that cushioning liquid B's is formulated as：Weigh p-aminophenyl sulphur
Sour 7.0g, disodium hydrogen phosphate 71.6g, sodium dihydrogen phosphate 6.2g and sodium citrate 11.8g are dissolved, Ran Houzhuan into beaker with water
Enter in 1L volumetric flasks, scale is settled to water.
10. the cushioning liquid any one of claim 1 to 9 is always planted in continuous flow method determines tobacco or tobacco product
Purposes in the method for alkaloids.
11. purposes according to claim 10, it is characterised in that the continuous flow method is determined in tobacco and tobacco product
The method of total alkaloid refers to generate cyanogen chloride, cyanogen chloride and the tobacco online using potassium rhodanide and sodium dichloro cyanurate
Or the total alkaloid reaction in tobacco product in terms of nicotine, disconnect the pyridine ring of nicotine, and then occur with p-aminobenzene sulfonic acid
Reaction, reaction product colorimeter is determined at 460nm.
12. the purposes according to claim 10 or 11, it is characterised in that the continuous flow method determines tobacco and tobacco system
The method of total alkaloid includes in product：
(1) preparation of sample：Tobacco sample is prepared by YC/T31, and determines its moisture, then using 5% acetic acid to tobacco
Sample is extracted, filtering, obtains filtrate standby；
(2) preparation of standard liquid：
Nicotine or nicotine salt are weighed with 5% acetate dissolution, at least five working stamndard liquid, the standard liquid prepared is configured to
Middle nicotine content concentration range is 0.5~7%；
(3) preparation of reaction reagent：
Potassium thiocyanate solution is formulated as：Potassium rhodanide is weighed into beaker, is dissolved with water, is then transferred in 250mL volumetric flasks,
Water constant volume is used, the solution concentration scope is 0.09~0.21mol/L；
Sodium dichloro cyanurate solution is formulated as：Sodium dichloro cyanurate is weighed into beaker, is dissolved with water, is then transferred to
In 250mL volumetric flasks, water constant volume is used, the solution concentration scope is 0.02~0.06mol/L；
Cushioning liquid A preparation：Disodium hydrogen phosphate 60.5-83.0g, tertiary sodium phosphate 10.1-20.2g are weighed into beaker, water is used
Dissolving, is then transferred in 1L volumetric flasks, scale is settled to water；Cushioning liquid B preparation：Weigh p-aminobenzene sulfonic acid 5.5-
8.0g, disodium hydrogen phosphate 60.5-83.0g, sodium dihydrogen phosphate 5.0-7.0g and sodium citrate 10.0-12.1g use water into beaker
Dissolving, is then transferred in 1L volumetric flasks, scale is settled to water；
Detoxicating liquid A's is formulated as：1g citric acids, 10g ferrous sulfate are weighed into beaker, is dissolved with water, is then transferred to 1L capacity
In bottle, scale is settled to water；
Detoxicating liquid B's is formulated as：10g sodium carbonate is weighed into beaker, is dissolved with water, is then transferred in 1L volumetric flasks, it is fixed with water
Hold to scale；
(4) using the work of Continuous Flow Analysis the instrument filtrate of detecting step (1) and step (2) under the reaction system of step (3)
Make titer；
(5) total alkaloid in sample is calculated according to following formula：
In formula, X：The Instrument observation value of sample, every milliliter (mg/mL) of unit milligram；
V：The extract volume of addition, unit is milliliter (mL)；
m：Sample quality, unit is gram (g)；
W：The percent water of sample, % (mass fraction)；
The total alkaloid that above formula is calculated is the content of the total alkaloid in terms of butt.
13. purposes according to claim 12, it is characterised in that the concentration of potassium thiocyanate solution is 0.12mol/L.
14. purposes according to claim 12, it is characterised in that the concentration of sodium dichloro cyanurate solution is 0.04mol/
L。
15. purposes according to claim 12, it is characterised in that weigh disodium hydrogen phosphate when preparing cushioning liquid A
71.6g。
16. purposes according to claim 12, it is characterised in that weigh tertiary sodium phosphate 15.2g when preparing cushioning liquid A.
17. purposes according to claim 12, it is characterised in that weigh p-aminobenzene sulfonic acid when preparing cushioning liquid B
7.0g。
18. purposes according to claim 12, it is characterised in that weigh disodium hydrogen phosphate when preparing cushioning liquid B
71.6g。
19. purposes according to claim 12, it is characterised in that weigh sodium dihydrogen phosphate 6.2g when preparing cushioning liquid B.
20. purposes according to claim 12, it is characterised in that weigh sodium citrate 11.8g when preparing cushioning liquid B.
21. purposes according to claim 12, it is characterised in that cushioning liquid A's is formulated as：Weigh disodium hydrogen phosphate
71.6g；Tertiary sodium phosphate 15.2g is dissolved into beaker with water, is then transferred in 1L volumetric flasks, scale is settled to water.
22. purposes according to claim 12, it is characterised in that cushioning liquid B's is formulated as：Weigh p-aminobenzene sulfonic acid
7.0g, disodium hydrogen phosphate 71.6g, sodium dihydrogen phosphate 6.2g and sodium citrate 11.8g are dissolved with water, are then transferred into beaker
In 1L volumetric flasks, scale is settled to water.
23. purposes according to claim 12, it is characterised in that cushioning liquid A and cushioning liquid B amount ratio is 3：4,
The amount ratio causes the pH value of reaction system to control between 6.0~7.5.
24. purposes according to claim 12, it is characterised in that potassium thiocyanate solution and sodium dichloro cyanurate solution are dense
Degree is than being 2.5：1 to 3.5：1.
25. purposes according to claim 24, it is characterised in that potassium thiocyanate solution and sodium dichloro cyanurate solution are dense
Degree is than being 3：1.
26. purposes according to claim 12, it is characterised in that the operational factor of Continuous Flow Analysis instrument is：Sample introduction is clear
Wash than for 1.5, glass/hour of sample introduction frequency 48, gain 18-60,2.85 volts of light intensity.
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| CN201410322455.5A CN104132895B (en) | 2014-07-08 | 2014-07-08 | The buffer system of total alkaloid tobacco and tobacco product is determined suitable for continuous flow method |
| PCT/CN2015/076250 WO2016004779A1 (en) | 2014-07-08 | 2015-04-10 | Buffer system and method of using the buffer system to measure total alkaloid in tobacco or tobacco products through continuous flow |
| EP15819267.4A EP3168605B1 (en) | 2014-07-08 | 2015-04-10 | Buffer system and method of using the buffer system to measure total alkaloid in tobacco or tobacco products through continuous flow |
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| CN111380817A (en) * | 2018-12-28 | 2020-07-07 | 贵州中烟工业有限责任公司 | Method for measuring total sulfur dioxide in tobacco or tobacco products by continuous flow method |
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