CN104132895A - Buffer system suitable for continuous flow method for measuring total alkaloid in tobacco and tobacco products - Google Patents
Buffer system suitable for continuous flow method for measuring total alkaloid in tobacco and tobacco products Download PDFInfo
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Abstract
The invention provides a buffer system suitable for a continuous flow method for measuring total alkaloid in tobacco and tobacco products. The buffer system comprises a buffer solution A and a buffer solution B; wherein the buffer solution A is prepared by the following steps: weighing 60.5 to 83.0 grams of disodium hydrogen phosphate (the preferable amount is 71.6 grams) and 10.1 to 20.2 grams of trisodium phosphate (the preferable amount is 15.2 grams), placing the weighed substances into a beaker, dissolving the mixture with water, then transferring the solution into a volumetric flask, and then filling water into the volumetric flask until the water reaches the scale; and the buffer solution B is prepared by the following steps: weighing 5.5 to 8.0 grams of p-aminobenzene sulfonic acid (the preferable amount is 7.0 grams), 60.5 to 83.0 grams of disodium hydrogen phosphate (the preferable amount is 71.6 grams), 5.0 to 7.0 grams of sodium dihydrogen phosphate (the preferable amount is 6.2 grams), and 10.0 to 12.1 grams of sodium citrate (the preferable amount is 11.8 grams), placing the weighed substances into a beaker, dissolving the mixture with water, transferring the solution into a volumetric flask, and then filling water into the volumetric flask until the water reaches the scale.
Description
Technical field
The invention belongs to tobacco components detection technique field, be specifically related to be applicable to the buffer system that continuous flow method is measured total alkaloid in tobacco and tobacco product.
Background technology
Nicotine is the important component of tobacco, without nicotine, does not also just claim tobacco.In tobacco conventional analysis, conventionally by measuring the content of total alkaloid in tobacco, know the content information of nicotine.The standard of measuring about total alkaloid in tobacco of tobacco business issue at present has: GB/T23225-2008 " the mensuration photometry of tobacco and tobacco product total alkaloid ", YC/T160-2002 " the mensuration continuous flow method of tobacco and tobacco product total alkaloid " and YC/T468-2013 " mensuration continuous flow (potassium rhodanide) method of tobacco and tobacco product total alkaloid ".
Continuous flow method belongs to instrument analytical method, is applicable to mass sample introduction, and application is comparatively extensive at present.The measuring principle of YC/T160-2002 " the mensuration continuous flow method of tobacco and tobacco product total alkaloid " is to adopt potassium cyanide and toluene-sodium-sulfonchloramide to generate online cyanogen chloride, the pyridine ring of nicotine is disconnected, and then react with sulfanilic acid, reaction product is measured with tintmeter at 460nm wavelength place.Although potassium cyanide is comparatively stable, it is a kind of material of severe toxicity, is positioned at toxic chemical prostatitis.For the use of potassium cyanide, there is many scruple, its marketing channel is checked on very tight, and a lot of laboratory Buying Cycle are very long even cannot buy, and user also need to put on record etc. in public security organ.Because the method has requirement to reacting suitable acid or alkali environment, so the method is by buffer solution A and buffer solution B, to control the acid or alkali environment of reaction.Because the surge capability of buffer solution B is not strong, if the pH of some Chemical Analysis Lab waters is between 5.0～6.0, the surge capability of this buffer solution B does not reach test needs in the method.The method is actual the pH of water is required will be higher than the requirement of one-level water in GB6682/T-2008 " assay laboratory's water specification and test method ", in order to reach the water requirement of the method, Chemical Analysis Lab need to be processed one-level water again, makes the actual use of the method have certain limitation.
The measuring principle of YC/T468-2013 " mensuration continuous flow (potassium rhodanide) method of tobacco and tobacco product total alkaloid " is to adopt potassium rhodanide and sodium dichloro cyanurate to generate online cyanogen chloride, the pyridine ring of nicotine is disconnected, and then react with sulfanilic acid, reaction product is measured with tintmeter at 460nm wavelength place.Compared to YC/T160-2002, YC/T468-2013 is not used potassium cyanide, has improved the processing safety that total alkaloid is measured.In YC/T468-2013, to reacting suitable acid or alkali environment, also there is requirement, by buffer solution A and buffer solution B, to control the acid or alkali environment of reaction equally, although can effectively control the acid or alkali environment of reaction, but when the method buffer solution A and buffer solution B preparation, chemicals usage is larger, equally the use of the method is made troubles.
Summary of the invention
In order to overcome the defect of prior art, the invention provides a kind of new buffer system that is applicable to total alkaloid in continuous flow method mensuration tobacco and tobacco product.This buffer system is applicable to adopt continuous flow (potassium rhodanide) method to measure the total alkaloid in tobacco and tobacco product.When adopting the use amount of buffer system of the present invention chemicals when having reduced preparation, can control the acid or alkali environment reacting, guarantee that cyanogen chloride makes the pyridine ring fracture of vegetable soda, and then with the reacting of sulfanilic acid, reaction is carried out under the acid or alkali environment condition of needs.
The present invention adopts following technical scheme to realize.
On the one hand, the invention provides a kind of buffer system that continuous flow method is measured total alkaloid in tobacco and tobacco product that is applicable to, this buffer system comprises buffer solution A and buffer solution B;
Wherein, buffer solution A is formulated as: take sodium hydrogen phosphate 60.5-83.0g, be preferably 71.6g; Tertiary sodium phosphate 10.1-20.2g, is preferably 15.2g to beaker, and water dissolves, and then proceeds in 1L volumetric flask, and water is settled to scale;
Buffer solution B is formulated as: take sulfanilic acid 5.5-8.0g, be preferably 7.0g; Sodium hydrogen phosphate 60.5-83.0g, is preferably 71.6g; Sodium dihydrogen phosphate 5.0-7.0g, is preferably 6.2g and sodium citrate 10.0-12.1g, is preferably 11.8g to beaker, and water dissolves, and then proceeds in 1L volumetric flask, and water is settled to scale.
Above-mentioned sodium hydrogen phosphate, tertiary sodium phosphate, sodium dihydrogen phosphate, sodium citrate can be conventional existence form, for example sodium hydrogen phosphate exists with 12 water of crystallization forms, tertiary sodium phosphate exists with 12 water of crystallization forms, sodium dihydrogen phosphate exists with 2 water of crystallization forms, and sodium citrate exists with 2 water of crystallization forms.
Preferably, in above-mentioned buffer system, the amount ratio between buffer solution A and buffer solution B is 1:2 to 1:1 (volume ratio), is preferably 3:4 (volume ratio).
On the other hand, the invention provides a kind of above-mentioned buffer system and measure the purposes in the method for total alkaloid in tobacco or tobacco product at continuous flow method.
Preferably, the method that described continuous flow method is measured total alkaloid in tobacco and tobacco product refers to that employing potassium rhodanide and sodium dichloro cyanurate generate cyanogen chloride online, cyanogen chloride reacts with the total alkaloid (in nicotine) in described tobacco or tobacco product, the pyridine ring of nicotine is disconnected, and then react with sulfanilic acid, reaction product is measured at 460nm place with tintmeter.
Preferably, in described continuous flow method mensuration tobacco and tobacco product, the method for total alkaloid comprises:
(1) preparation of sample: prepare tobacco sample by YC/T31, and measure its moisture, then use 5% acetic acid to extract tobacco sample, filter, obtain filtrate for later use;
(2) preparation of standard solution:
Take nicotine or nicotine salt with 5% acetate dissolution, be mixed with at least 5 working stamndard liquid, in the standard solution of preparing, nicotine content concentration range is 0.5～7%;
(3) preparation of reaction reagent:
Being formulated as of potassium rhodanide solution: take potassium rhodanide to beaker, water dissolves, then proceeds in 250mL volumetric flask, water constant volume, and this solution concentration scope is 0.09～0.21mol/L, is preferably 0.12mol/L.
Being formulated as of sodium dichloro cyanurate solution: take sodium dichloro cyanurate to beaker, water dissolves, then proceeds in 250mL volumetric flask, water constant volume, and this solution concentration scope is 0.02～0.06mol/L, is preferably 0.04mol/L.
The preparation of buffer solution A: take sodium hydrogen phosphate 60.5-83.0g, be preferably 71.6g; Tertiary sodium phosphate 10.1-20.2g, is preferably 15.2g to beaker, and water dissolves, and then proceeds in 1L volumetric flask, and water is settled to scale;
The preparation of buffer solution B: take sulfanilic acid 5.5-8.0g, be preferably 7.0g; Sodium hydrogen phosphate 60.5-83.0g, is preferably 71.6g; , sodium dihydrogen phosphate 5.0-7.0g, be preferably 6.2g and sodium citrate 10.0-12.1g, be preferably 11.8g to beaker, water dissolves, and then proceeds in 1L volumetric flask, water is settled to scale;
Above-mentioned sodium hydrogen phosphate, tertiary sodium phosphate, sodium dihydrogen phosphate, sodium citrate can be conventional existence form, for example sodium hydrogen phosphate exists with 12 water of crystallization forms, tertiary sodium phosphate exists with 12 water of crystallization forms, sodium dihydrogen phosphate exists with 2 water of crystallization forms, and sodium citrate exists with 2 water of crystallization forms.
Detoxicating liquid A is formulated as: take 1g citric acid, 10g ferrous sulphate to beaker, water dissolves, and then proceeds in 1L volumetric flask, and water is settled to scale; The Main Function of this detoxicating liquid A is the toxicity that reduces the cyanogen chloride that has neither part nor lot in reaction, and this detoxicating liquid A is identical with the detoxicating liquid A in YC/T160-2002 (potassium cyanide method).
Detoxicating liquid B is formulated as: take 10g sodium carbonate to beaker, water dissolves, and then proceeds in 1L volumetric flask, and water is settled to scale; The Main Function of this detoxicating liquid B is the toxicity that reduces the cyanogen chloride that has neither part nor lot in reaction, and this detoxicating liquid B is identical with YC/T160-2002 (potassium cyanide method) detoxicating liquid B.
(4) use the filtrate of Continuous Flow Analysis instrument detecting step (1) under the reaction system of step (3) and the working stamndard liquid of step (2);
(5) according to the total alkaloid in following formula calculation sample:
In formula, X: the Instrument observation value of sample, every milliliter of unit milligram (mg/mL);
V: the extract volume adding, unit is milliliter (mL);
M: sample quality, unit is gram (g);
W: the percent water content of sample, % (massfraction);
Preferably, in said method, the amount ratio of buffer solution A and buffer solution B is 1:2 to 1:1 (volume ratio), is preferably 3:4 (volume ratio), and this amount ratio is controlled between 6.0～7.5 the pH value of reaction system;
Preferably, in said method, potassium rhodanide solution and sodium dichloro cyanurate solution concentration, than for 2.5:1 to 3.5:1, are preferably 3:1.
Preferably, in said method, the operational factor of Continuous Flow Analysis instrument is: sample introduction cleans than being 1.5,48 glasss/hour of sample introduction frequencies, the 18-60 that gains, 2.85 volts of light intensity.
In said method, the preparation of the preparation of sample, the preparation of standard solution, reaction reagent order can change.
In a specific embodiments, the concrete steps that described continuous flow method is measured the method for total alkaloid in tobacco and tobacco product are as follows:
(1) use 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) configure certain density buffer solution A and B, detoxicating liquid A, detoxicating liquid B, potassium rhodanide solution and sodium dichloro cyanurate solution;
(4) use 5% acetic acid preparation total alkaloid standard solution;
(5) by the pump line in total alkaloid module, according to snapping in peristaltic pump shown in Fig. 1, (in module, the internal diameter of different pump lines is different, and the flow velocity of corresponding reagent is different, reaches the object of control and participate in reaction reagent ratio by controlling the flow velocity of reaction reagent; Adding air pump line is for the solution in pipeline is mixed), pump cover is covered, Reagent Tube is put into water; Opening power, opens detecting device, peristaltic pump, automatic sampler, computing machine; Switch on peristaltic pump is allocated to Run; Double-click in computing machine and connect Continuous Flow Analysis workstation icon; Click the charting on workstation, after successful connection, peristaltic pump operation, water is just pumped in pipeline and cleans, and scavenging period is 20～30min; After baseline stability (now baseline fluctuation be less than ± 1%), different pipelines is put into corresponding reagent, continue operation, during regulate baseline to 5% left and right in the charting window that ejects at workstation; According to the prompting establishment working procedure of Analysis in the drop-down menu of workstation, treat baseline stability, the Run clicking in workstation can move; Treat program end of run, different pipelines is relay in backwater, clean 20～30min; After cleaning completes, close successively automatic sampler, peristaltic pump, detecting device, takes off pump cover, powered-down.
Above-mentioned steps (1) is specially: take offal sample (offal sample is prepared by YC/T31) to 50mL tool plug triangular flask, add 5% acetic acid vibration 30min, use qualitative filter paper to filter.
Above-mentioned steps (2) is specially: shown in Fig. 1, pump line is arranged on peristaltic pump, adds pump cover, water detergent line.
In above-mentioned steps (3), buffer solution A is formulated as: take the sodium hydrogen phosphate of 71.6 grams, the tertiary sodium phosphate of 15.2 grams to beaker, water dissolves, and then proceeds in 1L volumetric flask, and water is settled to scale.Wherein, sodium hydrogen phosphate, tertiary sodium phosphate can be conventional existence form, and for example sodium hydrogen phosphate exists with 12 water of crystallization forms, and tertiary sodium phosphate exists with 12 water of crystallization forms.
In above-mentioned steps (3), buffer solution B is formulated as: take 7g sulfanilic acid, 71.6 grams of sodium hydrogen phosphates, 6.2 grams of sodium dihydrogen phosphates and 11.8 grams of sodium citrates to beaker, water dissolves, and then proceeds in 1L volumetric flask, and water is settled to scale.Wherein, sodium hydrogen phosphate, sodium dihydrogen phosphate, sodium citrate can be conventional existence form, and for example sodium hydrogen phosphate exists with 12 water of crystallization forms, and sodium dihydrogen phosphate exists with 2 water of crystallization forms, and sodium citrate exists with 2 water of crystallization forms.
In above-mentioned steps (3), detoxicating liquid A is formulated as: take 1g citric acid, 10g ferrous sulphate to beaker, water dissolves, and then proceeds in 1L volumetric flask, and water is settled to scale.The Main Function of detoxicating liquid A is to reduce the toxicity that has neither part nor lot in reaction cyanogen chloride.In step (3), detoxicating liquid A is identical with YC/T160-2002 (potassium cyanide method) detoxicating liquid A.
The middle detoxicating liquid B of above-mentioned steps (3) is formulated as: take 10g sodium carbonate to beaker, water dissolves, and then proceeds in 1L volumetric flask, and water is settled to scale.The Main Function of detoxicating liquid B is to reduce the toxicity that has neither part nor lot in reaction cyanogen chloride.In step (3), detoxicating liquid B is identical with YC/T160-2002 (potassium cyanide method) detoxicating liquid B.
In above-mentioned steps (3), being formulated as of potassium rhodanide solution: take appropriate potassium rhodanide to beaker, water dissolves, and then proceeds in 250mL volumetric flask water constant volume.This solution concentration scope is 0.09～0.21mol/L.
In above-mentioned steps (3), being formulated as of sodium dichloro cyanurate solution: take appropriate sodium dichloro cyanurate to beaker, water dissolves, and then proceeds in 250mL volumetric flask water constant volume.This solution concentration scope is 0.02～0.06mol/L.
In above-mentioned steps (3), potassium rhodanide solution and sodium dichloro cyanurate solution concentration proportioning are about 3:1.
In above-mentioned steps (4), standard solution is formulated as: take appropriate nicotine in 250mL volumetric flask, use 5% acetate dissolution, be settled to scale.This solution is nicotine storing solution, the about 1.6mg/mL of nicotine content left and right.By at least 5 working stamndard liquid of nicotine storing solution preparation, its concentration range should cover the sample size that expectation detects.
In above-mentioned steps (5), the operational factor of Continuous Flow Analysis instrument is: sample introduction cleans than being 1.5,48 glasss/hour of sample introduction frequencies, the 18-60 that gains, 2.85 volts of light intensity.
Above-mentioned continuous flow method is measured in tobacco and tobacco product in total alkaloid, sample pre-treatments is consistent with YC/T468-2013 " mensuration continuous flow (potassium rhodanide) method of tobacco and tobacco product total alkaloid ", buffer solution A and buffer solution B have been changed, set up a kind of new buffer system, while reducing preparation buffer solution A and buffer solution B, the use amount of chemicals has guaranteed the consistance with YC/T468-2013 method test result simultaneously.
At least there is following beneficial effect in the present invention:
The present invention adopts a kind of new buffer solution A can control the acid or alkali environment reacting before dialyser, guarantees that the acid or alkali environment that the front pH of dialyser can't be controlled buffer solution B between 6.0～11.0 impact;
The present invention adopts a kind of new buffer solution B can control the acid or alkali environment of reaction, regulator solution pH value is between 6.0～7.5, guarantee that cyanogen chloride makes the pyridine ring fracture of vegetable soda, so with the reacting of sulfanilic acid, under the acid or alkali environment condition of reaction needed, carry out;
The present invention has set up the buffer system that a kind of new continuous flow (potassium rhodanide) method that is applicable to is measured total alkaloid in tobacco and tobacco product;
Adopt the continuous flow method of buffer system of the present invention to compare with YC/T468-2013, while having reduced preparation buffer solution A and buffer solution B, the use amount of chemicals guarantees that data are consistent with YC/T468-2013 simultaneously.
Accompanying drawing explanation
Fig. 1 is for adopting continuous flow method to measure the piping diagram of total alkaloid in tobacco and tobacco product.
Embodiment
Below in conjunction with embodiment, the present invention is described further.These embodiment are intended to help to set forth the content of invention rather than limit the scope of the invention.
embodiment 1: the mensuration of total alkaloid in flue-cured tobacco
1) sample pre-treatments
Flue-cured tobacco offal is prepared into sample according to YC/T31, and measure its moisture, and then take 0.25g sample in 50mL tool plug triangular flask, add 25mL5% acetic acid, cover stopper, vibration (rotating speed >150rpm) extraction 30min on oscillator.With fast qualitative Filter paper filtering extract, discard front 2mL～3mL filtrate, the use that after collecting, subsequent filtrate performs an analysis.
2) reaction reagent preparation
Buffer solution A is formulated as: take 15.2 grams of 71.6 grams of sodium hydrogen phosphates (12 water of crystallization), tertiary sodium phosphate (12 water of crystallization) to beaker, water dissolves, and then proceeds in 1L volumetric flask, and water is settled to scale.
Buffer solution B is formulated as: take 11.8 grams of 7g sulfanilic acid, 71.6 grams of sodium hydrogen phosphates (12 water of crystallization), 6.2 grams of sodium dihydrogen phosphates (2 water of crystallization) and sodium citrates (2 water of crystallization) to beaker, water dissolves, then proceed in 1L volumetric flask, water constant volume water is settled to scale.
When following mensuration, the amount ratio of buffer solution A and buffer solution B is 3:4 (volume ratio).
The preparation of detoxicating liquid A, detoxicating liquid B, potassium rhodanide solution and sodium dichloro cyanurate solution is identical with corresponding reagent in YC/T468-2013 " mensuration continuous flow (potassium rhodanide) method of tobacco and tobacco product total alkaloid ".
Specific as follows:
Being formulated as of removing toxic substances solution A:
Take 1g citric acid, 10g ferrous sulphate to beaker, water dissolves, and then proceeds in 1000mL volumetric flask, and water is settled to scale.
Being formulated as of removing toxic substances solution B:
Take 10g sodium carbonate to beaker, water dissolves, and then proceeds in 1000mL volumetric flask, and water is settled to scale.
Being formulated as of potassium rhodanide solution:
Take 2.88g potassium rhodanide to beaker, water dissolves, and then proceeds in 250mL volumetric flask, and water is settled to scale.
Being formulated as of sodium dichloro cyanurate solution:
Take 2.20g sodium dichloro cyanurate to beaker, water dissolves, and then proceeds in 250mL volumetric flask, and water is settled to scale.This solution should be now with the current.
3) preparation of standard solution
Take appropriate total alkaloid mark liquid (there is card mark thing in countries tobacco Quality Supervision and Inspection Center) and, in 250mL volumetric flask, be accurate to 0.0001g, water dissolves, and is settled to scale, and this solution is nicotine standard reserving solution, and nicotine content should be in 1.6mg/mL left and right.Pipette respectively 12.5mL, 10mL, 5mL, 2.5mL, 0.5mL nicotine standard reserving solution to 100mL volumetric flask, acetic acid constant volume with 5%, the concentration that obtains work mark liquid is respectively 1.2105mg/mL, 0.9683mg/mL, 0.4842mg/mL, 0.2421mg/mL, 0.0484mg/mL.
4) the AA3 type Continuous Flow Analysis instrument that the analytical instrument of using in the present invention is produced for German Bran & Luebbe.Adopt the pipeline of total alkaloid in continuous flow method mensuration tobacco and tobacco product as shown in Figure 1.By the pump line in total alkaloid module, according to snapping in peristaltic pump shown in Fig. 1, (in module, the internal diameter of different pump lines is different, and the flow velocity of corresponding reagent is different, reaches the object of control and participate in reaction reagent ratio by controlling the flow velocity of reaction reagent; Adding air pump line is for the solution in pipeline is mixed), pump cover is covered, Reagent Tube is put into water; Opening power, opens detecting device, peristaltic pump, automatic sampler, computing machine; Switch on peristaltic pump is allocated to Run, double-clicks and connect Continuous Flow Analysis workstation; Click the charting on workstation, after successful connection, peristaltic pump operation, water is just pumped in pipeline and cleans, and scavenging period is 20～30min; After baseline stability (now baseline fluctuation be less than ± 1%), different pipelines is put into corresponding reagent, continue operation, during regulate baseline to 5% left and right in the charting window that ejects at workstation; According to the prompting establishment working procedure of Analysis in the drop-down menu of workstation, treat baseline stability, the Run clicking in workstation can move; Treat program end of run, different pipelines is relay in backwater, clean 20～30min; After cleaning completes, close successively automatic sampler, peristaltic pump, detecting device, takes off pump cover, powered-down.
5) typical curve adopts a curve;
6) data are calculated
The peak height at total alkaloid peak carries out regretional analysis to its respective concentration, obtains typical curve.Then by detecting the peak height of sample, by typical curve, obtain the concentration that sample is corresponding, i.e. Instrument observation value.
Total alkaloid content in butt, is drawn by following formula:
In formula, X: the Instrument observation value of sample, every milliliter of unit milligram (mg/mL);
V: the extract volume adding, unit is milliliter (extract volume is 25mL herein);
M: sample quality, unit is gram (g);
W: the percent water content of sample, % (massfraction);
By above formula, calculating total alkaloid content in flue-cured tobacco is 0.5～3%.
embodiment 2: the mensuration of total alkaloid in burley tobaccos
1) sample pre-treatments
Burley tobaccos offal is prepared into sample according to YC/T31, and measure its moisture, and then take 0.25g burley tobaccos sample in 50mL tool plug triangular flask, add 25mL5% acetic acid, cover stopper, vibration (rotating speed >150rpm) extraction 30min on oscillator.With fast qualitative Filter paper filtering extract, discard front 2mL～3mL filtrate, the use that after collecting, subsequent filtrate performs an analysis.
2) reaction reagent preparation
Buffer solution A is formulated as: take 15.2 grams of 71.6 grams of sodium hydrogen phosphates (12 water of crystallization), tertiary sodium phosphate (12 water of crystallization) to beaker, water dissolves, and then proceeds in 1L volumetric flask, and water is settled to scale.
Buffer solution B is formulated as: take 11.8 grams of 7g sulfanilic acid, 71.6 grams of sodium hydrogen phosphates (12 water of crystallization), 6.2 grams of sodium dihydrogen phosphates (2 water of crystallization) and sodium citrates (2 water of crystallization) to beaker, water dissolves, then proceed in 1L volumetric flask, water constant volume water is settled to scale.
When following mensuration, the amount ratio of buffer solution A and buffer solution B is for please supplement 3:4 (volume ratio).
The preparation of detoxicating liquid A, detoxicating liquid B, potassium rhodanide solution and sodium dichloro cyanurate solution is identical with corresponding reagent in YC/T468-2013 " mensuration continuous flow (potassium rhodanide) method of tobacco and tobacco product total alkaloid ".
Specific as follows:
Being formulated as of removing toxic substances solution A:
Take 1g citric acid, 10g ferrous sulphate to beaker, water dissolves, and then proceeds in 1000mL volumetric flask, and water is settled to scale.
Being formulated as of removing toxic substances solution B:
Take 10g sodium carbonate to beaker, water dissolves, and then proceeds in 1000mL volumetric flask, and water is settled to scale.
Being formulated as of potassium rhodanide solution:
Take 2.88g potassium rhodanide to beaker, water dissolves, and then proceeds in 250mL volumetric flask, and water is settled to scale.
Being formulated as of sodium dichloro cyanurate solution:
Take 2.20g sodium dichloro cyanurate to beaker, water dissolves, and then proceeds in 250mL volumetric flask, and water is settled to scale.This solution should be now with the current.
3) preparation of standard solution
Take appropriate total alkaloid mark liquid (there is card mark thing in countries tobacco Quality Supervision and Inspection Center) and, in 250mL volumetric flask, be accurate to 0.0001g, water dissolves, and is settled to scale, and this solution is nicotine standard reserving solution, and nicotine content should be in 1.6mg/mL left and right.Pipette respectively 12.5mL, 10mL, 5mL, 2.5mL, 0.5mL nicotine standard reserving solution to 100mL volumetric flask, acetic acid constant volume with 5%, the concentration that obtains work mark liquid is respectively 1.2105mg/mL, 0.9683mg/mL, 0.4842mg/mL, 0.2421mg/mL, 0.0484mg/mL.
4) the AA3 type Continuous Flow Analysis instrument that the analytical instrument of using in the present invention is produced for German Bran & Luebbe.Adopt the pipeline of total alkaloid in continuous flow method mensuration tobacco and tobacco product as shown in Figure 1.By the pump line in total alkaloid module, according to snapping in peristaltic pump shown in Fig. 1, (in module, the internal diameter of different pump lines is different, and the flow velocity of corresponding reagent is different, reaches the object of control and participate in reaction reagent ratio by controlling the flow velocity of reaction reagent; Adding air pump line is for the solution in pipeline is mixed), pump cover is covered, Reagent Tube is put into water; Opening power, opens detecting device, peristaltic pump, automatic sampler, computing machine; Switch on peristaltic pump is allocated to Run, double-clicks and connect Continuous Flow Analysis workstation; Click the charting on workstation, after successful connection, peristaltic pump operation, water is just pumped in pipeline and cleans, and scavenging period is 20～30min; After baseline stability (now baseline fluctuation be less than ± 1%), different pipelines is put into corresponding reagent, continue operation, during regulate baseline to 5% left and right in the charting window that ejects at workstation; According to the prompting establishment working procedure of Analysis in the drop-down menu of workstation, treat baseline stability, the Run clicking in workstation can move; Treat program end of run, different pipelines is relay in backwater, clean 20～30min; After cleaning completes, close successively automatic sampler, peristaltic pump, detecting device, takes off pump cover, powered-down.
5) typical curve adopts a curve;
6) data are calculated
The peak height at total alkaloid peak carries out regretional analysis to its respective concentration, obtains typical curve.Then by detecting the peak height of sample, by typical curve, obtain the concentration that sample is corresponding, i.e. Instrument observation value.
Total alkaloid content in butt, is drawn by following formula:
In formula, X: the Instrument observation value of sample, every milliliter of unit milligram (mg/mL);
V: the extract volume adding, unit is milliliter (extract volume is 25mL herein);
M: sample quality, unit is gram (g);
W: the percent water content of sample, % (massfraction);
By above formula, calculating total alkaloid content in burley tobaccos is 1～5%.
embodiment 3: the mensuration of total alkaloid in cigarette
1) sample pre-treatments
Cigarette shreds is prepared into sample according to YC/T31, and measure its moisture, and then take 0.25g cigarette sample in 50mL tool plug triangular flask, add 25mL5% acetic acid, cover stopper, vibration (rotating speed >150rpm) extraction 30min on oscillator.With fast qualitative Filter paper filtering extract, discard front 2mL～3mL filtrate, the use that after collecting, subsequent filtrate performs an analysis.
2) reaction reagent preparation
Buffer solution A is formulated as: take 20.0 grams of 83.0 grams of sodium hydrogen phosphates (12 water of crystallization), tertiary sodium phosphate (12 water of crystallization) to beaker, water dissolves, and then proceeds in 1L volumetric flask, and water is settled to scale.
Buffer solution B is formulated as: take 10.4 grams of 7g sulfanilic acid, sodium hydrogen phosphate (12 water of crystallization) gram, 5.2 grams of sodium dihydrogen phosphates (2 water of crystallization) and sodium citrates (2 water of crystallization) to beaker, water dissolves, then proceed in 1L volumetric flask, water constant volume water is settled to scale.
When following mensuration, the amount ratio of buffer solution A and buffer solution B is 3:4 (volume ratio)
The preparation of detoxicating liquid A, detoxicating liquid B, potassium rhodanide solution and sodium dichloro cyanurate solution is identical with corresponding reagent in YC/T468-2013 " mensuration continuous flow (potassium rhodanide) method of tobacco and tobacco product total alkaloid ".
Specific as follows:
Being formulated as of removing toxic substances solution A:
Take 1g citric acid, 10g ferrous sulphate to beaker, water dissolves, and then proceeds in 1000mL volumetric flask, and water is settled to scale.
Being formulated as of removing toxic substances solution B:
Take 10g sodium carbonate to beaker, water dissolves, and then proceeds in 1000mL volumetric flask, and water is settled to scale.
Being formulated as of potassium rhodanide solution:
Take 2.88g potassium rhodanide to beaker, water dissolves, and then proceeds in 250mL volumetric flask, and water is settled to scale.
Being formulated as of sodium dichloro cyanurate solution:
Take 2.20g sodium dichloro cyanurate to beaker, water dissolves, and then proceeds in 250mL volumetric flask, and water is settled to scale.This solution should be now with the current.
3) preparation of standard solution
Take appropriate total alkaloid mark liquid (there is card mark thing in countries tobacco Quality Supervision and Inspection Center) and, in 250mL volumetric flask, be accurate to 0.0001g, water dissolves, and is settled to scale, and this solution is nicotine standard reserving solution, and nicotine content should be in 1.6mg/mL left and right.Pipette respectively 12.5mL, 10mL, 5mL, 2.5mL, 0.5mL nicotine standard reserving solution to 100mL volumetric flask, acetic acid constant volume with 5%, the concentration that obtains work mark liquid is respectively 1.2105mg/mL, 0.9683mg/mL, 0.4842mg/mL, 0.2421mg/mL, 0.0484mg/mL.
4) the AA3 type Continuous Flow Analysis instrument that the analytical instrument of using in the present invention is produced for German Bran & Luebbe.Adopt the pipeline of total alkaloid in continuous flow method mensuration tobacco and tobacco product as shown in Figure 1.By the pump line in total alkaloid module, according to snapping in peristaltic pump shown in Fig. 1, (in module, the internal diameter of different pump lines is different, and the flow velocity of corresponding reagent is different, reaches the object of control and participate in reaction reagent ratio by controlling the flow velocity of reaction reagent; Adding air pump line is for the solution in pipeline is mixed), pump cover is covered, Reagent Tube is put into water; Opening power, opens detecting device, peristaltic pump, automatic sampler, computing machine; Switch on peristaltic pump is allocated to Run, double-clicks and connect Continuous Flow Analysis workstation; Click the charting on workstation, after successful connection, peristaltic pump operation, water is just pumped in pipeline and cleans, and scavenging period is 20～30min; After baseline stability (now baseline fluctuation be less than ± 1%), different pipelines is put into corresponding reagent, continue operation, during regulate baseline to 5% left and right in the charting window that ejects at workstation; According to the prompting establishment working procedure of Analysis in the drop-down menu of workstation, treat baseline stability, the Run clicking in workstation can move; Treat program end of run, different pipelines is relay in backwater, clean 20～30min; After cleaning completes, close successively automatic sampler, peristaltic pump, detecting device, takes off pump cover, powered-down.
5) typical curve adopts a curve;
6) data are calculated
The peak height at total alkaloid peak carries out regretional analysis to its respective concentration, obtains typical curve.Then by detecting the peak height of sample, by typical curve, obtain the concentration that sample is corresponding, i.e. Instrument observation value.
Total alkaloid content in butt, is drawn by following formula:
In formula, X: the Instrument observation value of sample, every milliliter of unit milligram (mg/mL);
V: the extract volume adding, unit is milliliter (extract volume is 25mL herein);
M: sample quality, unit is gram (g);
W: the percent water content of sample, % (massfraction);
By above formula, calculating total alkaloid content in cigarette is 0.5～4%.
embodiment 4: the continuous flow method and the comparative study that adopts the continuous flow method testing result of other buffer systems that adopt buffer system of the present invention
If no special instructions, the present embodiment is used reagent and method are all consistent with YC/T468-2013.
The continuous flow method that adopts respectively buffer system of the present invention with other buffer systems (except buffer system is different from the present invention, all the other reagent are all identical) to flue-cured tobacco, burley tobaccos, Turkish tobaccos, Virginian-type cigarette and five kinds of samples of blended type cigarette are measured, and its measurement result is in Table 1～table 7.From table 1～table 7: the continuous flow method measurement result that same sample adopts buffer system of the present invention is all less than 0.04 with respect to the absolute difference of YC/T468-2013 method, and other buffer system measurement results are all larger with respect to the absolute difference of YC/T468-2013 method.In table 8, listed same sample has been adopted respectively to the continuous flow method of buffer system of the present invention, the measurement result of the continuous flow method of other buffer systems and YC/T468-2013 method is carried out paired t-test (α=0.05), result, adopting the continuous flow method result of buffer system of the present invention is P=0.35>0.05, illustrate that two kinds of analytical approachs do not have significant difference, show to adopt the continuous flow method of buffer system of the present invention consistent with YC/T468-2013 standard method result; Adopt the detection method P<0.05 of other buffer systems, illustrate that two kinds of analytical approachs exist significant difference, show to adopt the method for other buffer systems and YC/T468-2013 standard method test result inconsistent.
Table 1 adopts continuous flow method and the YC/T468-2013 method measurement result of buffer system of the present invention to compare
Table 2 sodium hydrogen phosphate, borax system and YC/T468-2013 method measurement result are compared
Table 3 sodium dihydrogen phosphate, NaOH system and YC/T468-2013 method measurement result are compared
Table 4 sodium phosphate, citric acid system and YC/T468-2013 method measurement result are compared
Table 5 sodium citrate, citric acid system and YC/T468-2013 method measurement result are compared
Table 6 calmine, hydrochloric acid system and YC/T468-2013 method measurement result are compared
Table 7 trishydroxymethylaminomethane, hydrochloric acid system and YC/T468 method measurement result are compared
The different buffer systems of table 8 and YC/T468-2013 method measurement result paired t-test
Claims (8)
1. be applicable to continuous flow method and measure a buffer solution for total alkaloid in tobacco and tobacco product, this buffer solution comprises buffer solution A and buffer solution B;
Wherein, buffer solution A is formulated as: take sodium hydrogen phosphate 60.5-83.0g, be preferably 71.6g; Tertiary sodium phosphate 10.1-20.2g, is preferably 15.2g to beaker, and water dissolves, and then proceeds in 1L volumetric flask, and water is settled to scale;
Buffer solution B is formulated as: take sulfanilic acid 5.5-8.0g, be preferably 7.0g, sodium hydrogen phosphate 60.5-83.0g, be preferably 71.6g, sodium dihydrogen phosphate 5.0-7.0g, be preferably 6.2g and sodium citrate 10.0-12.1g, be preferably 11.8g to beaker, water dissolves, and then proceeds in 1L volumetric flask, and water is settled to scale.
2. buffer solution according to claim 1, is characterized in that, the amount ratio between buffer solution A and buffer solution B is 1:2 to 1:1, is preferably 3:4.
3. the buffer solution described in a claim 1 or 2 is measured the purposes in the method for total alkaloid in tobacco or tobacco product at continuous flow method.
4. purposes according to claim 3, it is characterized in that, the method that described continuous flow method is measured total alkaloid in tobacco and tobacco product refers to that employing potassium rhodanide and sodium dichloro cyanurate generate cyanogen chloride online, cyanogen chloride reacts with the total alkaloid (in nicotine) in described tobacco or tobacco product, the pyridine ring of nicotine is disconnected, and then react with sulfanilic acid, reaction product is measured at 460nm place with tintmeter.
5. according to the purposes described in claim 3 or 4, it is characterized in that, the method that described continuous flow method is measured total alkaloid in tobacco and tobacco product comprises:
(1) preparation of sample: prepare tobacco sample by YC/T31, and measure its moisture, then use 5% acetic acid to extract tobacco sample, filter, obtain filtrate for later use;
(2) preparation of standard solution:
Take nicotine or nicotine salt with 5% acetate dissolution, be mixed with at least 5 working stamndard liquid, in the standard solution of preparing, nicotine content concentration range is 0.5～7%;
(3) preparation of reaction reagent:
Being formulated as of potassium rhodanide solution: take potassium rhodanide to beaker, water dissolves, then proceeds in 250mL volumetric flask, water constant volume, and this solution concentration scope is 0.09～0.21mol/L, is preferably 0.12mol/L;
Being formulated as of sodium dichloro cyanurate solution: take sodium dichloro cyanurate to beaker, water dissolves, then proceeds in 250mL volumetric flask, water constant volume, and this solution concentration scope is 0.02～0.06mol/L, is preferably 0.04mol/L;
The preparation of buffer solution A: take sodium hydrogen phosphate 60.5-83.0g, be preferably 71.6g, tertiary sodium phosphate 10.1-20.2g, be preferably 15.2g to beaker, water dissolves, and then proceeds in 1L volumetric flask, and water is settled to scale; The preparation of buffer solution B: take sulfanilic acid 5.5-8.0g, be preferably 7.0g, sodium hydrogen phosphate 60.5-83.0g, be preferably 71.6g, sodium dihydrogen phosphate 5.0-7.0g, be preferably 6.2g and sodium citrate 10.0-12.1g, be preferably 11.8g to beaker, water dissolves, and then proceeds in 1L volumetric flask, and water is settled to scale;
Detoxicating liquid A is formulated as: take 1g citric acid, 10g ferrous sulphate to beaker, water dissolves, and then proceeds in 1L volumetric flask, and water is settled to scale;
Detoxicating liquid B is formulated as: take 10g sodium carbonate to beaker, water dissolves, and then proceeds in 1L volumetric flask, and water is settled to scale;
(4) use the filtrate of Continuous Flow Analysis instrument detecting step (1) under the reaction system of step (3) and the working stamndard liquid of step (2);
(5) according to the total alkaloid in following formula calculation sample:
In formula, X: the Instrument observation value of sample, every milliliter of unit milligram (mg/mL);
V: the extract volume adding, unit is milliliter (mL);
M: sample quality, unit is gram (g);
W: the percent water content of sample, % (massfraction);
The total alkaloid that above formula calculates is the content of the total alkaloid in butt.
6. purposes according to claim 5, is characterized in that, the amount ratio of buffer solution A and buffer solution B is 1:2 to 1:1, is preferably 3:4, and this amount ratio is controlled between 6.0～7.5 the pH value of reaction system.
7. purposes according to claim 5, is characterized in that, potassium rhodanide solution and sodium dichloro cyanurate solution concentration, than for 2.5:1 to 3.5:1, are preferably 3:1.
8. purposes according to claim 5, is characterized in that, the operational factor of Continuous Flow Analysis instrument is: sample introduction cleans than being 1.5,48 glasss/hour of sample introduction frequencies, the 18-60 that gains, 2.85 volts of light intensity.
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| 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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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016004779A1 (en) * | 2014-07-08 | 2016-01-14 | 国家烟草质量监督检验中心 | Buffer system and method of using the buffer system to measure total alkaloid in tobacco or tobacco products through continuous flow |
| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1089834A (en) * | 1993-10-14 | 1994-07-27 | 王子芸 | The prescription of chewing gum for giving-up smoking and processing technique |
| CN101301275A (en) * | 2001-03-26 | 2008-11-12 | 史密丝克莱恩比彻姆公司 | Method for preparing nicotine containing oral dosage form |
-
2014
- 2014-07-08 CN CN201410322455.5A patent/CN104132895B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1089834A (en) * | 1993-10-14 | 1994-07-27 | 王子芸 | The prescription of chewing gum for giving-up smoking and processing technique |
| CN101301275A (en) * | 2001-03-26 | 2008-11-12 | 史密丝克莱恩比彻姆公司 | Method for preparing nicotine containing oral dosage form |
Non-Patent Citations (4)
| Title |
|---|
| 国家烟草专卖局: "《中华任免共和国烟草行业标准》", 30 June 2013, 中国标准出版社 * |
| 张威等: "连续流动法测定烤烟总植物碱的不确定度", 《烟草科技》 * |
| 张杰等: "硫氰化钾与DCIC反应法测定烟草总植物碱", 《烟草化学》 * |
| 李苓等: "连续流动分析仪测定烟草总植物碱的条件探索", 《云南大学学报（自然科学版）》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016004779A1 (en) * | 2014-07-08 | 2016-01-14 | 国家烟草质量监督检验中心 | Buffer system and method of using the buffer system to measure total alkaloid in tobacco or tobacco products through continuous flow |
| EP3168605A4 (en) * | 2014-07-08 | 2018-01-17 | China National Tobacco Quality Supervision&test Center | Buffer system and method of using the buffer system to measure total alkaloid in tobacco or tobacco products through continuous flow |
| 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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