CN104132937A - Continuous flow method for measuring total alkaloid in tobacco or tobacco products - Google Patents
Continuous flow method for measuring total alkaloid in tobacco or tobacco products Download PDFInfo
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Abstract
The invention provides a continuous flow method for measuring total alkaloid in tobacco or tobacco products. In the method, potassium thiocyanate and sodium dichloro isocyanurate are adopted to carry out reactions to generate cyanogen chloride on line. The cyanogen chloride can carry out reactions with total alkaloid (calculated in the form of nicotine) in tobacco or tobacco products to break off the pyridine rings of nicotine, and then further carries out reactions with p-aminobenzene sulfonic acid. The reaction products are measured by a chromometer at 460 nm. The method uses a buffer system to control the pH value of the reaction system in a range of 6.0 to 7.5, and the buffer system is composed of a buffer solution A and a buffer solution B. The buffer solution A is prepared by the following steps: weighing disodium hydrogen phosphate and trisodium phosphate, placing the weighed substances in a beaker, dissolving the substances with water, transferring the solution to a volumetric flask (1L), and adding water into the volumetric flask until the water reaches the scale. The buffer solution B is prepared by the following steps: weighing p-aminobenzene sulfonic acid, disodium hydrogen phosphate, sodium dihydrogen phosphate, and sodium citrate, placing the weighed substances into a beaker, dissolving the substances with water, transferring the solution to a volumetric flask (1L), and then adding 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 a kind of method of measuring total alkaloid in tobacco or tobacco product with continuous flow method.
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 method of measuring total alkaloid in tobacco or tobacco product with continuous flow method.The method has changed buffer solution A and the buffer solution B in YC/T468-2013, 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.
The present invention adopts following technical scheme to realize.
A kind of method of measuring total alkaloid in tobacco or tobacco product with continuous flow method, the method adopts potassium rhodanide and sodium dichloro cyanurate to generate online cyanogen chloride, 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, and the method comprises:
Adopt buffer solution A and buffer solution B that the pH value of reaction system is controlled between 6.0～7.5;
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 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);
Preferably, said method also comprises:
Being prepared as of sample: prepare tobacco sample by YC/T31, and measure its moisture, then use 5% acetic acid to extract tobacco sample, filter, obtain filtrate.
Preferably, said method also comprises:
Being formulated as 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%;
Preferably, said method also comprises:
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.
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.
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, said method also comprises:
Use Continuous Flow Analysis instrument to detect, then 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.
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.
Preferably, said method 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, 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.
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, method concrete steps of the present invention 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.
Adopt method of the present invention, 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 method of 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;
Compare with YC/T468-2013, when method of the present invention has 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 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: buffer system of the present invention and the comparative study that adopts the continuous flow method testing result of other buffer systems
Below for adopting the method for the embodiment of the present invention 1, the experimental result that different buffer systems is tested.
Adopting respectively buffer system of the present invention (is buffer solution A and the buffer solution B using in the embodiment of the present invention 1, the amount ratio of buffer solution A and buffer solution B is identical from embodiment 1) and other buffer systems (except buffer system is different with 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: same sample adopts buffer system measurement result of the present invention to be 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 and adopted respectively the assay method of buffer system of the present invention, other buffer systems and the measurement result of YC/T468-2013 method to carry out paired t-test (α=0.05) to same sample, result, the methods and results 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 that the method for buffer system of the present invention is 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 that other buffer systems and YC/T468-2013 standard method test result are inconsistent.
The method of this buffer system of table 1 and YC/T468-2013 method measurement result are compared
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 (10)
1. a method of measuring total alkaloid in tobacco or tobacco product with continuous flow method, the method adopts potassium rhodanide and sodium dichloro cyanurate to generate online cyanogen chloride, 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, and the method comprises:
Adopt buffer solution A and/or buffer solution B that the pH value of reaction system is controlled between 6.0～7.5;
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. method according to claim 1, 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.
3. method according to claim 1 and 2, is characterized in that, described method also comprises:
Being prepared as of sample: prepare tobacco sample by YC/T31, and measure its moisture, then use 5% acetic acid to extract tobacco sample, filter, obtain filtrate.
4. according to the method in any one of claims 1 to 3, it is characterized in that, described method also comprises:
Being formulated as 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%.
5. according to the method described in any one in claim 1 to 4, it is characterized in that, described method also comprises:
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;
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;
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.
6. according to the method described in any one in claim 1 to 5, it is characterized in that, described method also comprises:
Use Continuous Flow Analysis instrument to detect, then 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.
7. according to the method described in any one in claim 1 to 6, it is characterized in that, in described 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.
8. method according to claim 1, is characterized in that, described method 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.
9. method according to claim 8, 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; Preferably, potassium rhodanide solution and sodium dichloro cyanurate solution concentration, than for 2.5:1 to 3.5:1, are preferably 3:1.
10. method according to claim 8 or claim 9, 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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| CN201410324273.1A CN104132937B (en) | 2014-07-08 | 2014-07-08 | A kind of method that total alkaloid in tobacco or tobacco product is determined with 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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