CN111999284A - Flow chemical analyzer and method for measuring nicotine content in tobacco products - Google Patents
Flow chemical analyzer and method for measuring nicotine content in tobacco products Download PDFInfo
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- CN111999284A CN111999284A CN202010905554.1A CN202010905554A CN111999284A CN 111999284 A CN111999284 A CN 111999284A CN 202010905554 A CN202010905554 A CN 202010905554A CN 111999284 A CN111999284 A CN 111999284A
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- tobacco
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- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 title claims abstract description 47
- 229960002715 nicotine Drugs 0.000 title claims abstract description 47
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000000126 substance Substances 0.000 title claims abstract description 38
- 235000019505 tobacco product Nutrition 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 103
- 238000006243 chemical reaction Methods 0.000 claims abstract description 53
- 238000001514 detection method Methods 0.000 claims abstract description 53
- 238000005111 flow chemistry technique Methods 0.000 claims abstract description 18
- 241000208125 Nicotiana Species 0.000 claims description 55
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims description 54
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 45
- 238000002156 mixing Methods 0.000 claims description 41
- 239000007853 buffer solution Substances 0.000 claims description 34
- HVBSAKJJOYLTQU-UHFFFAOYSA-N 4-aminobenzenesulfonic acid Chemical compound NC1=CC=C(S(O)(=O)=O)C=C1 HVBSAKJJOYLTQU-UHFFFAOYSA-N 0.000 claims description 21
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000007795 chemical reaction product Substances 0.000 claims description 10
- CEJLBZWIKQJOAT-UHFFFAOYSA-N dichloroisocyanuric acid Chemical compound ClN1C(=O)NC(=O)N(Cl)C1=O CEJLBZWIKQJOAT-UHFFFAOYSA-N 0.000 claims description 10
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 claims description 10
- 229940116357 potassium thiocyanate Drugs 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- QPJDMGCKMHUXFD-UHFFFAOYSA-N cyanogen chloride Chemical compound ClC#N QPJDMGCKMHUXFD-UHFFFAOYSA-N 0.000 claims description 9
- 238000002347 injection Methods 0.000 claims description 8
- 239000007924 injection Substances 0.000 claims description 8
- 229950000244 sulfanilic acid Drugs 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 235000019504 cigarettes Nutrition 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 3
- 230000010355 oscillation Effects 0.000 claims description 3
- 238000004445 quantitative analysis Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 6
- 238000004458 analytical method Methods 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 30
- 239000012224 working solution Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 239000013068 control sample Substances 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 3
- 239000013589 supplement Substances 0.000 description 3
- 238000011077 uniformity evaluation Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 241000208292 Solanaceae Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
- G01N21/05—Flow-through cuvettes
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
- G01N2021/0325—Cells for testing reactions, e.g. containing reagents
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- Life Sciences & Earth Sciences (AREA)
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
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- Spectroscopy & Molecular Physics (AREA)
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Abstract
The invention belongs to the field of analysis and detection, and relates to a flow chemistry analyzer, which comprises a reagent A pipeline, a reagent B pipeline and a pre-reaction pipeline; wherein the flow rate of the reagent A pipeline is 0.17-0.5 mL/min; the flow rate of the reagent B pipeline is 0.17-0.5 mL/min; the pre-reaction pipeline is a spiral pipe with 6-10 turns, the outer diameter of the spiral cross section of the spiral pipe is 1-4 mm, the thread pitch is 2-7 mm, the inlet of the pre-reaction pipeline is connected with the outlet of the reagent A pipeline and the outlet of the reagent B pipeline through a three-way pipe respectively, and the flow rate of the pre-reaction pipeline is 0.3-1 mL/min. The invention also relates to a method for determining the nicotine content in tobacco products. When the flow chemical analyzer is used for measuring the nicotine content of the tobacco products, the problems of baseline drift, impurity peaks and peak dropping do not occur, and the flow chemical analyzer is high in detection accuracy, repeatability and reliability.
Description
Technical Field
The invention belongs to the field of analysis and detection, and particularly relates to a flow chemical analyzer for determining nicotine content and a method for determining nicotine content in tobacco products.
Background
The chemical components of the tobacco leaves are the internal reflection of the quality of the tobacco leaves, and the main chemical components and the content thereof in the tobacco leaves determine the smoke characteristics of the tobacco leaves and directly influence the quality of the tobacco leaves. Therefore, the detection of the internal chemical components of the tobacco leaves is concerned, and the requirements on detection instruments are gradually increased.
The flow chemical analyzer is mainly used for detecting chemical components and contents of raw tobacco and finished tobacco lamina, and mainly relates to detection indexes including nicotine, total sugar, reducing sugar, total nitrogen, potassium and chlorine. On the basis, the flow chemical analyzer can also be used for carrying out uniformity evaluation on finished tobacco flakes, wherein the uniformity evaluation is mainly used for evaluating the variation coefficient of the nicotine index of the finished tobacco flakes, and the smaller the variation coefficient is, the better the uniformity is, so that the accuracy of measuring the nicotine content by using the flow chemical analyzer directly influences the reliability of the uniformity evaluation of the finished tobacco flakes.
The principle of measuring the nicotine content by adopting the flow chemical analyzer is as follows: the nicotine in the sample reacts with sulfanilic acid and cyanogen chloride, the obtained reaction product has the strongest absorption to light with the wavelength of 460nm, and the nicotine content is determined according to the reaction, wherein the cyanogen chloride can be generated by the reaction of potassium thiocyanate and sodium dichloroisocyanurate. Specifically, on equipment, in a flow chemical analyzer, a reagent containing sulfanilic acid, a reagent containing potassium thiocyanate and a reagent containing sodium dichloroisocyanurate respectively flow in different pipelines; during detection, firstly, a reagent containing potassium thiocyanate and a reagent containing sodium dichloroisocyanurate flow into a reaction pipeline in proportion to react to generate cyanogen chloride, then the generated reaction product, the reagent containing sulfanilic acid, a sample to be detected and a buffer solution are pumped into another reaction pipeline in proportion to react to obtain a final reaction product, and then the absorption of the final reaction product to light with wavelength of 460nm is detected by a digital photometer detector to obtain a detection result.
However, the phenomena of spectrogram baseline drift, more impurity peaks and frequent peak dropping exist when the flow chemical analyzer is adopted to detect the nicotine content in the tobacco leaves at present, and the problems of poor detection repeatability, low accuracy, low precision and the like also exist. Therefore, there is a need for a method for determining the content of nicotine in tobacco leaves that overcomes the above problems.
Disclosure of Invention
One of the purposes of the invention is to provide a flow chemical analyzer for measuring nicotine content, which adopts a reagent A pipeline and a reagent B pipeline with specific flow rates and a pre-reaction pipeline with specific flow rates and shapes to realize that the detection result has no problems of baseline drift, impurity peaks, peak dropping and the like, and has high detection accuracy and good repeatability. The invention also aims to provide a method for measuring the nicotine content in the tobacco products.
The invention relates to a flow chemistry analyzer for determining nicotine content, comprising a reagent A pipeline, a reagent B pipeline and a pre-reaction pipeline; wherein,
the reagent A pipeline is used for storing and/or conveying a reagent A containing potassium thiocyanate, and the flow rate of the reagent A pipeline is 0.17-0.5 mL/min (such as 0.2mL/min, 0.23mL/min and 0.3 mL/min);
the reagent B pipeline is used for storing and/or conveying the reagent B containing sodium dichloroisocyanurate, and the flow rate of the reagent B pipeline is 0.17-0.5 mL/min (such as 0.2mL/min, 0.23mL/min and 0.3 mL/min);
the pre-reaction pipeline is a spiral pipe with 6-10 turns (such as 7, 8 and 9), the spiral cross section of the spiral pipe has an outer diameter of 1-4 mm (such as 2, 2.5 and 3mm) and a screw pitch of 2-7 mm (such as 3, 4, 5 and 6mm), the inlet of the pre-reaction pipeline is respectively connected with the outlet of the reagent A pipeline and the outlet of the reagent B pipeline through a tee pipe, the flow rate of the pre-reaction pipeline is 0.3-1 mL/min (such as 0.4mL/min, 0.46mL/min, 0.5mL/min, 0.6mL/min, 0.7mL/min, 0.8mL/min and 0.9mL/min), and the pre-reaction pipeline is used for mixing the reagent A and the reagent B and reacting to generate a product containing cyanogen chloride.
In some embodiments of the first aspect of the present invention, the inner diameter of the two inlets and one outlet of the tee is 1 to 2.3mm, such as 1.1mm, 1.2mm, 1.3mm, 1.5mm, 1.7mm, 1.8mm, 2.0mm, 2.1mm, 2.2 mm.
In some embodiments of the first aspect of the present invention, the outer diameter of the two inlets and one outlet of the tee is from 2.8 to 6mm, for example 3mm, 3.2mm, 3.5mm, 3.7mm, 3.8mm, 3.9mm, 4.0mm, 4.1mm, 4.2mm, 4.5mm, 4.6mm, 4.8mm, 5.0mm, 5.2mm, 5.4mm, 5.6mm, 5.8mm, 5.9 mm.
In some embodiments of the first aspect of the present invention, the flow chemistry analyzer further comprises a buffer solution line for storing and/or delivering a buffer solution; wherein the buffer solution comprises citric acid, disodium hydrogen phosphate and water.
In some embodiments of the first aspect of the present invention, the flow chemical analyzer further comprises a reagent C line for storing and/or transporting reagent C containing sulfanilic acid; wherein the reagent C comprises citric acid, disodium hydrogen phosphate, sulfanilic acid and water.
In some embodiments of the first aspect of the present invention, the flow chemistry analyzer further comprises a sample injection pipeline and a final reaction pipeline, wherein an outlet of the pre-reaction pipeline, an outlet of the buffer solution pipeline, an outlet of the reagent C pipeline, and an outlet of the sample injection pipeline are connected to an inlet of the final reaction pipeline, and the final reaction pipeline is used for mixing and reacting the cyanogen chloride-containing reaction product, the buffer solution, the reagent C, and the sample to be tested to generate a final product.
In some embodiments of the first aspect of the present invention, the flow chemical analyzer further includes a first mixing pipeline, an outlet of the buffer solution pipeline and an outlet of the sample introduction pipeline are connected to an inlet of the first mixing pipeline, and an outlet of the pre-reaction pipeline, an outlet of the first mixing pipeline, and an outlet of the reagent C pipeline are connected to an inlet of the final reaction pipeline.
In some embodiments of the first aspect of the present invention, the flow chemistry analyzer further includes a first air line, a second air line, and a second mixing line, an outlet of the first air line, an outlet of the buffer solution line, and an outlet of the sample injection line are connected to an inlet of the first mixing line, an outlet of the second air line and an outlet of the reagent C line are connected to an inlet of the second mixing line, and an outlet of the pre-reaction line, an outlet of the first mixing line, and an outlet of the second mixing line are connected to an inlet of the final reaction line.
In some embodiments of the first aspect of the present invention, the flow chemistry analyzer has one or more of the following characteristics a to j:
a. the flow chemistry analyzer further comprises a detector for detecting an end product;
b. the reagent A is 7-18 g/L (such as 10g/L, 11g/L and 12g/L) of potassium thiocyanate aqueous solution;
c. the reagent B is 3-14 g/L (such as 7g/L, 8.8g/L and 9g/L) sodium dichloroisocyanurate aqueous solution;
d. the buffer solution comprises 9.6-17 g/L (such as 10g/L, 10.4g/L, 11g/L, 15g/L) of citric acid and 61-75 g/L (such as 64g/L, 65g/L, 66g/L) of disodium hydrogen phosphate;
e. the flow rate of the buffer solution pipeline is 0.3-0.8 mL/min;
f. the reagent C comprises 5-14 g/L (such as 7g/L, 8.4g/L and 9g/L) of citric acid, 200-260 g/L (such as 210g/L, 220g/L, 222g/L and 230g/L) of disodium hydrogen phosphate and 2-18 g/L (such as 6g/L, 7g/L and 8g/L) of sulfanilic acid;
g. the flow rate of the reagent C pipeline is 0.6-1.1 mL/min;
h. the temperature of all the pipelines is 20-37 ℃, such as 30 ℃ and 35 ℃;
i. the flow rate of the sample introduction pipeline is 0.17-0.5 mL/min, such as 0.2mL/min, 0.23mL/min and 0.3 mL/min;
j. the inner diameter of the pre-reaction pipeline is 0.1-2 mm, such as 0.3mm, 0.4mm, 0.5mm, 0.6mm, 0.7mm, 0.8mm, 0.9mm, 1.0mm, 1.2mm, 1.4mm, 1.5mm, 1.6mm, 1.7mm, 1.9mm, 1.97 mm.
In a second aspect, the present invention relates to a method for determining the nicotine content of a tobacco product, comprising the steps of:
(1) mixing the tobacco product with an acid solution, carrying out solid-liquid separation, and collecting a liquid phase substance;
(2) detecting the nicotine content in the liquid phase substance by using the flow chemical analyzer in the first aspect of the invention to obtain a detection result;
(3) and calculating the nicotine content in the tobacco product according to the detection result.
In some embodiments of the second aspect of the present invention, in step (1), the mixing is under shaking conditions.
In some embodiments of the second aspect of the present invention, in step (1), the oscillation rate is 200 to 300 times/min, for example 250 times/min.
In some embodiments of the second aspect of the present invention, one or more of the following features (a) to (e) are provided:
(a) the tobacco product is selected from tobacco leaves, raw tobacco, finished tobacco sheets, cigarettes and tobacco powder, and is preferably tobacco leaves and/or tobacco powder;
(b) in the step (1), the ratio of the tobacco product to the acid solution is (1-10) to 1g/L, such as 4:1, 5:1 and 6: 1;
(c) in the step (1), the mixing time is 5-100 minutes, such as 30 minutes;
(d) in the step (1), solid-liquid separation is carried out by filtration;
(e) and (3) calculating the nicotine content in the tobacco product by adopting an external standard quantitative analysis method according to the detection result.
In some embodiments of the second aspect of the present invention, the tobacco product is grade B2F tobacco leaves from fujian Longyan Yongding and/or shredded tobacco thereof.
A third aspect of the invention relates to the use of a flow chemical analyzer according to the first aspect of the invention for determining the nicotine content of a tobacco product.
In some embodiments of the third aspect of the present invention, the tobacco product is selected from the group consisting of tobacco leaves, raw tobacco, finished tobacco lamina, cigarettes and tobacco ends, preferably tobacco leaves and/or tobacco ends.
In some embodiments of the third aspect of the invention, the tobacco product is grade B2F tobacco leaves, produced from fujian Longyan Yongding, and/or shredded tobacco thereof.
In the present invention, unless otherwise specified, wherein:
the term "tobacco product" refers to a hobby commodity made from tobacco leaves. According to the characteristics of different types of tobacco leaves, different processing and manufacturing methods are applied to produce a variety of tobacco products so as to meet the hobby requirements of different consumers. Most of them are cigarettes.
The term "tobacco leaves" refers to the leaves of plants of the genus nicotiana of the family solanaceae, which are the main raw material of the tobacco industry.
The term "raw tobacco" refers to flue-cured tobacco leaves.
The term "finished tobacco lamina" refers to a product obtained by threshing and redrying tobacco leaves.
The invention has the following beneficial effects:
when the flow chemical analyzer is used for measuring the nicotine content in the tobacco products, the problems of baseline drift, impurity peaks and peak dropping do not occur, the detection accuracy is high, the repeatability is good, and the detection result is reliable.
Drawings
In order that the present disclosure may be more readily and clearly understood, the following detailed description of the present disclosure is provided in connection with specific embodiments thereof and the accompanying drawings, in which,
FIG. 1 is a schematic diagram of one embodiment of a flow chemistry analyzer for determining nicotine content in accordance with the present invention;
FIG. 2 is a spectrum of the detection result of example 2;
FIG. 3 is a spectrum of the result of the test of comparative example 1;
FIG. 4 is a spectrum of the result of detection in item (1) of comparative example 2;
the system comprises a sample injection device, a detector, a pre-reaction device, a reagent A pipeline, a reagent B pipeline, a three-way pipe, a pre-reaction pipeline, a reagent C pipeline, a buffer solution pipeline, a sample injection pipeline, a final reaction pipeline, a first air pipeline, a second air pipeline, a first mixing pipeline, a second mixing pipeline and a detector, wherein the sample injection device 1 is a reagent A pipeline, the reagent B pipeline 2 is a reagent B pipeline, the three-way pipe is 3, the pre-reaction pipeline 4 is a reagent C pipeline, the buffer solution pipeline 6 is.
Detailed Description
Embodiments of the present invention will now be described more fully hereinafter with reference to the accompanying examples, in which some, but not all embodiments of the invention are shown. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Fig. 1 is a schematic structural diagram of one embodiment of a flow chemistry analyzer for determining nicotine content in accordance with the present invention.
The flow chemical analyzer for measuring the nicotine content comprises a reagent A pipeline 1, a reagent B pipeline 2 and a pre-reaction pipeline 4; wherein,
the reagent A pipeline 1 is used for storing and/or conveying a reagent A containing potassium thiocyanate, and the flow rate of the reagent A pipeline 1 is 0.17-0.5 mL/min;
the reagent B pipeline 2 is used for storing and/or conveying the reagent B containing sodium dichloroisocyanurate, and the flow rate of the reagent B pipeline 2 is 0.17-0.5 mL/min;
the pre-reaction pipeline 4 is a spiral pipe with 6-10 turns, the outer diameter of the spiral cross section of the spiral pipe is 1-4 mm, the thread pitch is 2-7 mm, and the inner diameter of the pipe is 0.1-2 mm, the inlet of the pre-reaction pipeline 4 is respectively connected with the outlet of the reagent A pipeline 1 and the outlet of the reagent B pipeline 2 through a three-way pipe fitting 3, the flow rate of the pre-reaction pipeline 4 is 0.3-1 mL/min, and the pre-reaction pipeline 4 is used for mixing the reagent A and the reagent B and reacting to generate a product containing cyanogen chloride.
In the embodiment, the inner diameters of two inlets and one outlet of the three-way pipe fitting 3 are 1-2.3 mm.
In the embodiment, the outer diameters of two inlets and one outlet of the three-way pipe fitting 3 are 2.8-6 mm.
In this embodiment, the flow chemistry analyzer further comprises a buffer solution line 6 for storing and/or delivering a buffer solution; wherein the buffer solution comprises citric acid, disodium hydrogen phosphate and water.
In this embodiment, the flow chemical analyzer further includes a reagent C line 5 for storing and/or transporting a reagent C containing sulfanilic acid; wherein the reagent C comprises citric acid, disodium hydrogen phosphate, sulfanilic acid and water.
In this embodiment, the flow chemistry analyzer further includes a sample introduction pipeline 7, a first air pipeline 9, a second air pipeline 10, a first mixing pipeline 11, a second mixing pipeline 12, and a final reaction pipeline 8, an outlet of the first air pipeline 9, an outlet of the buffer solution pipeline 6, and an outlet of the sample introduction pipeline 7 are connected to an inlet of the first mixing pipeline 11, an outlet of the second air pipeline 10 and an outlet of the reagent C pipeline 5 are connected to an inlet of the second mixing pipeline 12, an outlet of the pre-reaction pipeline 4, an outlet of the first mixing pipeline 11, and an outlet of the second mixing pipeline 12 are connected to an inlet of the final reaction pipeline 8, and the final reaction pipeline 8 is configured to mix and react a reaction product containing cyanogen chloride, the buffer solution, the reagent C, and a sample to be detected to generate a final product.
In this embodiment, the flow chemical analyzer further comprises a detector 13 for detecting the end product.
In the embodiment, the reagent A is 7-18 g/L potassium thiocyanate aqueous solution.
In this embodiment, the reagent B is 3-14 g/L sodium dichloroisocyanurate aqueous solution.
In this embodiment, the buffer solution contains 9.6-17 g/L citric acid and 61-75 g/L disodium hydrogen phosphate.
In this embodiment, the flow rate of the buffer solution pipeline 6 is 0.3-0.8 mL/min.
In this embodiment, the reagent C comprises 5-14 g/L citric acid, 200-260 g/L disodium hydrogen phosphate and 2-18 g/L sulfanilic acid.
In this embodiment, the flow rate of the reagent C pipe 5 is 0.6-1.1 mL/min.
In this example, the temperature of all the lines was 20 ℃ to 37 ℃.
In this embodiment, the flow rate of the sample introduction pipeline 7 is 0.17-0.5 mL/min.
EXAMPLE 1 detection of Nicotine content in samples
1. Preparation of reagents and detection equipment:
preparation of reagent A: adding water into 2.88g of potassium thiocyanate to supplement the water to 250mL, and uniformly mixing to obtain a solution serving as a reagent A;
preparation of reagent B: adding water into 2.2g of sodium dichloroisocyanurate for supplementing to 250mL, and uniformly mixing to obtain a solution serving as a reagent B;
preparation of reagent C: adding water to 8.4g of citric acid, 222g of disodium hydrogen phosphate and 7g of sulfanilic acid to supplement the solution to 1000mL, and uniformly mixing to obtain a solution as a reagent C;
preparing a buffer solution: adding water into 10.4g of citric acid and 65.5g of disodium hydrogen phosphate to supplement the solution to 1000mL, and uniformly mixing to obtain a buffer solution;
preparation of standard working solution: uniformly mixing a nicotine standard substance (with the purity of 99.9%) with distilled water to obtain a nicotine stock solution with the concentration of 2 g/L; transferring 2ml, 4ml, 6ml, 8ml and 10ml of nicotine stock solution into 5 volumetric flasks by a pipette, and diluting with 100ml of acetic acid to obtain S1-S5 standard working solutions with the concentrations of 0.04g/L, 0.08g/L, 0.12g/L, 0.16g/L and 0.2 g/L.
2. Sample pretreatment:
weighing 0.43-0.44 g of tobacco powder sample, adding 100mL of 5% (W/W) acetic acid solution, mixing for 30 minutes under the action of an oscillator, wherein the oscillation rate is 250 times/minute, and filtering to obtain filtrate as a sample to be detected for later use.
3. Detecting the nicotine content:
the flow chemical analyzer shown in fig. 1 was used for detection.
(1) Starting the machine, washing the whole pipeline by distilled water, checking whether the pipeline connection of the instrument is normal or not, and checking whether the signal transmission of the instrument is normal or not; injecting all reagents into a flow chemical analyzer to test the peak shape and the baseline [ the operating conditions are the same as those in the step (2) ];
(2) and detecting the nicotine content of each standard working solution and the sample to be detected by adopting a flow chemical analyzer.
And respectively adding the reagent A, the reagent B, the reagent C and the buffer solution into corresponding pipelines of the flow chemical analyzer. The operating conditions of the flow chemical analyzer were:
the flow rate of the reagent A pipeline 1 is 0.23 mL/min;
the flow rate of the reagent B pipeline 2 is 0.23 mL/min;
the flow rate of the reagent C pipeline 5 is 0.8 mL/min;
the flow rate of the buffer solution pipeline 6 is 0.6 mL/min;
the pre-reaction pipeline 4 is spiral, the number of turns is 10, the outer diameter of the spiral cross section is 2.6mm, the thread pitch is 4.0mm, and the inner diameter of the pipe is 0.82 mm;
the three-way pipe fitting 3 is a SKALAR accessory 5204 three-way pipe, and has an outer diameter of 4.03mm and an inner diameter of 1.79 mm;
the temperature of all pipelines is kept between 20 and 37 ℃;
the sample injection amount is 0.23 mL/min;
4. And (3) calculation and result:
and establishing a standard working curve y which is 35488x +978 according to the concentration of the standard working solution and the detection peak height, substituting the detection peak height of the sample to be detected into the standard working curve, calculating the nicotine content of the sample to be detected, and converting to obtain the nicotine content in the tobacco powder of 3.91-3.99%.
Example 2 verification of accuracy and repeatability
(1) Pretreatment:
weighing 0.43-0.44 g of tobacco powder sample (obtained by crushing B2F grade tobacco leaves produced from Fujian Longyan Yongding), and processing according to the method of 'sample pretreatment' in the embodiment 1 to obtain a sample to be detected for later use.
(2) And (3) detection:
on the same day, each standard working solution (prepared according to the method in example 1), the sample to be tested and the laboratory control sample (purchased from the national tobacco quality supervision and inspection center, and the detection result of nicotine content is between 1.76% and 1.96% indicating that the detection method has high accuracy) were tested according to the method of "detecting nicotine content" in example 1, wherein the test was repeated for 20 times on the sample to be tested, and the detection result is shown in fig. 2. In fig. 2, from left to right, the 2 nd to 6 th peaks represent S1-S5 standard working solutions, the 8 th to 27 th peaks represent results of 20-time repeated tests of samples to be tested, the 28 th peak represents results of laboratory control sample tests, the 1 st peak represents S5 standard working solutions (for determining the starting position of the spectrogram), and the 7 th peak and the last peak represent S4 standard working solutions (used as references for adjustment).
And establishing a standard working curve according to the concentration of the standard working solution and the detection peak height, substituting the detection peak heights of the sample to be detected and the laboratory control sample into the standard working curve, and calculating the nicotine content of each detection of the sample to be detected and the nicotine content of the laboratory control sample, wherein the detection result of the nicotine content of the laboratory control sample is 1.85%, and is 1.76-1.96%, which shows that the detection method has high accuracy.
The nicotine content of each detection of the sample to be detected is converted to obtain the nicotine content of each detection of the tobacco powder, and the result is shown in table 1.
TABLE 1
As can be seen from Table 1, the standard deviation of 20 detections is only 0.03, and the coefficient of variation is only 0.66, which indicates that the method of the invention has high detection repeatability and good reliability.
Comparative example 1
The tobacco powder samples in example 2 were tested, the flow rates of the reagent A and B lines were adjusted to 0.1mL/min, and the three-way pipe fitting was SKALAR 5220-1C (1.22 mm in outside diameter and 0.46mm in inside diameter), and the rest was the same as in example 2.
As shown in fig. 3, the detection result shows that there are baseline drift, impurity peaks (for example, split peaks appear in the 3 rd and 20 th peaks from left to right), and peak dropping phenomena, which indicates that the detection method of comparative example 1 has poor repeatability and low accuracy, and cannot obtain an accurate and reliable detection result.
Comparative example 2
The tobacco dust samples from example 2 were also tested.
(1) The number of turns of the first reaction line was adjusted to 5, and the rest was the same as in example 2.
As shown in fig. 4, the detection result shows that there are severe peak dropping and impurity peaks (for example, a 19 th peak from left to right shows a split peak), and the detection peak height of the laboratory control sample is not accurate, which indicates that the detection method of comparative example 2 has poor repeatability and low accuracy, and cannot obtain an accurate and reliable detection result.
(2) The number of turns of the first reaction line was adjusted to 11, and the rest was the same as in example 1. The detection is repeated a plurality of times.
As a result, the problem of tube explosion, namely the disconnection of the interface between the tubes in the detection process, is easily caused along with the increase of the detection times.
Comparative example 3
The tobacco dust samples from example 1 were also tested.
(1) The amount of disodium hydrogen phosphate was reduced to 60.5g at the time of buffer solution preparation, and the rest was the same as in example 1. The test was repeated a number of times.
As a result, the peak heights in the multiple detection results are inconsistent, and the repeatability of the detection results is poor.
(2) The citric acid was reduced to 9.4g at the time of buffer solution preparation, and the rest was the same as in example 1. The test was repeated a number of times.
As a result, the peak heights in the multiple detection results are inconsistent, and the repeatability of the detection results is poor.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A flow chemistry analyzer for determining nicotine content includes a reagent A line, a reagent B line, and a pre-reaction line; wherein,
the reagent A pipeline is used for storing and/or conveying a reagent A containing potassium thiocyanate, and the flow rate of the reagent A pipeline is 0.17-0.5 mL/min;
the reagent B pipeline is used for storing and/or conveying the reagent B containing sodium dichloroisocyanurate, and the flow rate of the reagent B pipeline is 0.17-0.5 mL/min;
the pre-reaction pipeline is a spiral pipe with 6-10 turns, the outer diameter of the spiral cross section of the spiral pipe is 1-4 mm, the thread pitch is 2-7 mm, the inlet of the pre-reaction pipeline is respectively connected with the outlet of the reagent A pipeline and the outlet of the reagent B pipeline through a three-way pipe, the flow rate of the pre-reaction pipeline is 0.3-1 mL/min, and the pre-reaction pipeline is used for mixing the reagent A and the reagent B and reacting to generate a product containing cyanogen chloride.
2. The flow chemistry analyzer of claim 1, wherein the inner diameter of the two inlets and one outlet of the tee is 1-2.3 mm;
preferably, the outer diameter of two inlets and one outlet of the tee pipe fitting is 2.8-6 mm.
3. The flow chemistry analyzer of claim 1, further comprising a buffer solution line for storing and/or delivering a buffer solution; wherein the buffer solution comprises citric acid, disodium hydrogen phosphate and water.
4. The flow chemical analyzer according to any one of claims 1 to 3, further comprising a reagent C line for storing and/or transporting reagent C containing sulfanilic acid; wherein the reagent C comprises citric acid, disodium hydrogen phosphate, sulfanilic acid and water.
5. The flow chemistry analyzer of claim 4, further comprising a sample introduction pipeline and a final reaction pipeline, wherein an outlet of the pre-reaction pipeline, an outlet of the buffer solution pipeline, an outlet of the reagent C pipeline, and an outlet of the sample introduction pipeline are connected with an inlet of the final reaction pipeline, and the final reaction pipeline is used for mixing and reacting a reaction product containing cyanogen chloride, the buffer solution, the reagent C and a sample to be detected to generate a final product;
preferably, the flow chemical analyzer further comprises a first mixing pipeline, the outlet of the buffer solution pipeline and the outlet of the sample introduction pipeline are connected with the inlet of the first mixing pipeline, and the outlet of the pre-reaction pipeline, the outlet of the first mixing pipeline and the outlet of the reagent C pipeline are connected with the inlet of the final reaction pipeline;
more preferably, the flow chemistry analyzer further comprises a first air pipeline, a second air pipeline and a second mixing pipeline, wherein an outlet of the first air pipeline, an outlet of the buffer solution pipeline and an outlet of the sample injection pipeline are connected with an inlet of the first mixing pipeline, an outlet of the second air pipeline and an outlet of the reagent C pipeline are connected with an inlet of the second mixing pipeline, and an outlet of the pre-reaction pipeline, an outlet of the first mixing pipeline and an outlet of the second mixing pipeline are connected with an inlet of the final reaction pipeline.
6. The flow chemistry analyzer of any one of claims 1 to 5, characterized by one or more of the following a to j:
a. the flow chemistry analyzer further comprises a detector for detecting an end product;
b. the reagent A is a 7-18 g/L potassium thiocyanate aqueous solution;
c. the reagent B is 3-14 g/L sodium dichloroisocyanurate aqueous solution;
d. the buffer solution comprises 9.6-17 g/L of citric acid and 61-75 g/L of disodium hydrogen phosphate;
e. the flow rate of the buffer solution pipeline is 0.3-0.8 mL/min;
f. the reagent C comprises 5-14 g/L of citric acid, 200-260 g/L of disodium hydrogen phosphate and 2-18 g/L of sulfanilic acid;
g. the flow rate of the reagent C pipeline is 0.6-1.1 mL/min;
h. the temperature of all pipelines is 20-37 ℃;
i. the flow rate of the sample introduction pipeline is 0.17-0.5 mL/min;
j. the inner diameter of the pre-reaction pipeline is 0.1-2 mm.
7. A method of determining the nicotine content of a tobacco product, comprising the steps of:
(1) mixing the tobacco product with an acid solution, carrying out solid-liquid separation, and collecting a liquid phase substance;
(2) detecting the nicotine content in the liquid phase substance by using the flow chemical analyzer of any one of claims 1 to 6 to obtain a detection result;
(3) and calculating the nicotine content in the tobacco product according to the detection result.
8. The method according to claim 7, wherein in step (1), the mixing is performed under shaking conditions;
preferably, the oscillation rate is 200 to 300 times/min.
9. The method of claim 7 or 8, characterized by one or more of the following (a) to (e):
(a) the tobacco product is selected from tobacco leaves, raw tobacco, finished tobacco sheets and cigarettes, preferably tobacco leaves;
(b) in the step (1), the ratio of the tobacco product to the acid solution is (1-10) to 1 g/L;
(c) in the step (1), the mixing time is 5-100 minutes;
(d) in the step (1), solid-liquid separation is carried out by filtration;
(e) and (3) calculating the nicotine content in the tobacco product by adopting an external standard quantitative analysis method according to the detection result.
10. Use of the flow chemical analyzer of any one of claims 1 to 6 for determining nicotine content of a tobacco product;
preferably, the tobacco product is selected from the group consisting of tobacco leaves, raw tobacco, finished tobacco lamina and cigarettes, more preferably tobacco leaves.
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| CN114544884A (en) * | 2022-03-10 | 2022-05-27 | 广东中烟工业有限责任公司 | Estimation method of cyanide release amount after tobacco combustion |
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