CN115791943A - Electrochemical method for quantitatively detecting nicotine concentration - Google Patents
Electrochemical method for quantitatively detecting nicotine concentration Download PDFInfo
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- CN115791943A CN115791943A CN202211665937.1A CN202211665937A CN115791943A CN 115791943 A CN115791943 A CN 115791943A CN 202211665937 A CN202211665937 A CN 202211665937A CN 115791943 A CN115791943 A CN 115791943A
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Abstract
The invention relates to the technical field of electrochemical analysis and detection, in particular to an electrochemical method for quantitatively detecting nicotine concentration. The electrochemical method comprises the following steps: adding a sulfuric acid solution to a screen printing electrode for electrochemical treatment to prepare a pretreatment electrode; the screen printing electrode comprises a reference electrode, and the reference electrode comprises Ag and AgCl; the electrochemical treatment is to carry out voltammetry test; preparing diluted standard substances with different known concentrations, respectively detecting the current value of the diluted standard substances by using a voltammetry method through a pretreatment electrode, and performing linear fitting to prepare a standard curve; diluting a sample to be detected by using a buffer solution to prepare a diluted sample, detecting the current value of the diluted sample by using a pretreatment electrode through a voltammetry method, substituting the current value of the diluted sample into a standard curve, and calculating the nicotine concentration. The detection method of the invention activates the silver electrode by using sulfuric acid before detection, and the detected result has high precision and good repeatability RSD less than 3%.
Description
Technical Field
The invention relates to the technical field of electrochemical analysis and detection, in particular to an electrochemical method for quantitatively detecting nicotine concentration.
Background
Electronic cigarettes are a new tobacco substitute, also called as electric atomization cigarettes, and mainly comprise a cigarette rod and a cigarette cartridge. The cigarette cartridge contains nicotine, propylene glycol, glycerin or polyethylene glycol and the like, different flavors can be added into different electronic cigarettes to prepare various tastes, so that the requirements of smokers are met. At present, the nicotine content of electronic cigarettes of different brands is greatly different, the actual nicotine content of partial products is not consistent with the product labels, and the unified standard is lacked. At the same time, the release of e-cigarette smoke can cause an increase in the amount of nicotine deposited on the surface of windows, walls, floors, wood and metal, indicating that smoking e-cigarettes may indirectly expose people to nicotine. The standard (GB 41700-2022) states that the release of nicotine should not be higher than 0.2mg per mouth.
At present, the main methods for measuring the nicotine content include a mass analysis method, an atomic absorption spectrometry method, a spectrophotometry method, a titration method, a chromatography method and the like, wherein the gas chromatography method is the main method for measuring the content of the electronic cigarette in the traditional tobacco sample. However, the traditional detection method cannot achieve the effects of rapidness, portability and precision in detection, and the electrochemical detection method is generally used for high-precision detection of a large number of electronic cigarettes. Nicotine is a redox active molecule, and rapid, portable and on-site measurement based on an electrochemical analysis method can be realized by utilizing the electrochemical activity of nicotine.
However, most of the current detection methods have a standard fitting curve of a logarithmic function in the range of 0.02-0.5g/L of nicotine content, require multi-point fitting, are not favorable for concentration judgment, and have repeatability which is not enough and has a relative standard deviation RSD of more than 3%.
Therefore, it is highly desirable to provide an electrochemical method for quantitatively detecting nicotine concentration, which has high accuracy and good repeatability for detecting nicotine content.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. For this purpose, an electrochemical method for the quantitative determination of nicotine concentration is proposed.
The invention conception of the invention is as follows: according to the invention, the silver electrode is activated by using sulfuric acid before detection, and a specific acidic buffer solution is selected during detection, so that the accuracy of a unitary linear function fitting curve of a standard substance in the range of 0.05-0.45g/L of nicotine can be further improved, the detected detection result has high precision and good repeatability, and the relative standard deviation RSD is less than 3%.
In a first aspect, the present invention provides an electrochemical method for quantitatively determining nicotine concentration, the electrochemical method comprising the steps of:
(1) Adding a sulfuric acid solution to a screen printing electrode for electrochemical treatment to prepare a pretreatment electrode; the screen printing electrode comprises a reference electrode, and the reference electrode comprises Ag and AgCl; the electrochemical treatment is a voltammetry test;
(2) Preparing diluted standard substances with different known concentrations, respectively detecting the current value of the diluted standard substances by using the pretreatment electrodes through a voltammetry method, and performing linear fitting to prepare a standard curve;
(3) Diluting a sample to be detected by using a buffer solution to prepare a diluted sample, detecting the current value of the diluted sample by using the pretreatment electrode to perform voltammetry, substituting the current value of the diluted sample for the standard curve, and calculating the nicotine concentration.
Preferably, the standard curve is y =0.5758x-0.0046 2 =0.9976, x is the peak current in μ a, y is the nicotine concentration in mg/mL, R 2 The degree of fit was determined.
Compared with the prior art, the electrochemical method for quantitatively detecting the nicotine concentration provided by the first aspect of the invention has the following beneficial effects: according to the detection method, the specific Ag/AgCl electrode is activated by using sulfuric acid before detection, and the buffer solution is selected during detection, so that the accuracy of a unitary linear function fitting curve of the standard substance in the range of 0.05-0.35g/L of nicotine can be further improved, the detection result is high in precision, the repeatability is good, and the relative standard deviation RSD is less than 3%.
Preferably, the sulfuric acid solution is an aqueous solution of sulfuric acid, and the concentration of the sulfuric acid solution is 0.01-0.10mol/L; further preferably, the concentration of the sulfuric acid solution is 0.05-0.10mol/L.
Preferably, in the step (1), the addition amount of the sulfuric acid solution is 50-200 μ L; further preferably, the addition amount of the sulfuric acid solution is 100 to 200. Mu.L.
Preferably, in the step (1), the operating voltage of the electrochemical treatment ranges from-0.5V to +1.5V.
Preferably, in the step (1), the electrochemical treatment is to perform the voltammetry test on the sulfuric acid solution by using the screen-printed electrode until a stable arsenic characteristic peak map of the voltammetry curve is obtained.
Preferably, in step (1), the working electrode is a carbon working electrode, the reference electrode is an Ag/AgCl reference electrode, and the auxiliary electrode is a carbon-to-auxiliary electrode.
Preferably, in the step (1), the voltammetry includes at least one of cyclic voltammetry, square wave voltammetry, linear sweep voltammetry, conventional pulse voltammetry, and differential pulse voltammetry; further preferably, the cyclic voltammetry detection parameters are set as follows: the measuring voltage is-0.5 to 1.5V, the scanning speed is 30 to 60mV/s, and the scanning interval is 0.0005 to 0.0015V.
Preferably, in step (2), the fitting method of the standard curve comprises the following steps:
(a) The nicotine standard substance is subjected to gradient dilution by using the buffer solution to prepare diluted standard substances with different known concentrations;
(b) And respectively detecting the current values of the diluted standard products with different known concentrations by using the pretreatment electrodes to perform voltammetry, and performing linear fitting on the current values of the diluted standard products with different known concentrations to prepare the standard curve.
Preferably, in step (a), the concentration of the diluted standard substance is 0.01-0.5g/L.
Preferably, in the step (b), the voltammetry includes at least one of cyclic voltammetry, square wave voltammetry, linear sweep voltammetry, conventional pulse voltammetry, and differential pulse voltammetry. Further preferably, the cyclic voltammetry detection parameters are set as follows: the measuring voltage is-0.5 to 1.5V, the scanning speed is 30 to 60mV/s, and the scanning interval is 0.0005 to 0.0015V.
Preferably, in the step (3), the dilution factor is 2-100 times; further preferably, the dilution factor is 5 to 20.
Preferably, in the step (3), the buffer solution comprises a weak acid salt, and the weak acid salt comprises phosphate and acetate; further preferably, the phosphate: the molar ratio of the acetate is 1: (0.5-1.5).
Preferably, in the step (3), the concentration of the weak acid salt is 0.001-2M; further preferably, the concentration of the weak acid salt is 0.005-0.05M.
Preferably, in the step (3), the pH of the buffer solution is 6 to 8; further preferably, the pH of the buffer solution is 6.5 to 7.5.
Preferably, the temperature of the diluted sample is 15 ℃ to 35 ℃; further preferably, the temperature of the diluted sample is 25-30 ℃.
Compared with the prior art, the invention has the following beneficial effects:
according to the detection method, the silver electrode is activated by using sulfuric acid before detection, and a specific acidic buffer solution is selected during detection, so that the accuracy of a unitary linear function fitting curve of the standard substance in the range of 0.05-0.45g/L of nicotine can be further improved, and the detection result is high in precision and good in repeatability, and the relative standard deviation RSD is less than 3%.
Drawings
FIG. 1 is a calibration curve of the standard of example 1 of the present invention.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples are given for illustration. It should be noted that the following examples are not intended to limit the scope of the claimed invention.
The starting materials, reagents or apparatuses used in the following examples are, unless otherwise specified, either commercially available from conventional sources or can be obtained by known methods.
Example 1
The nicotine content of the electronic cigarette liquid is detected electrochemically, the whole process is carried out at 25 ℃, and the detection method comprises the following steps:
(1) Activation treatment of C-Ag/AgCl-C screen printing electrode: under the condition that the measuring voltage is-0.5 to +1.5V, 200 mu L of sulfuric acid solution with the concentration of 0.1mol/L is dripped on a screen printing electrode for electrochemical treatment, and the initial potential is 0.4V and the final potential is 1.4V by cyclic voltammetry until a stable cyclic voltammetry curve graph is obtained to prepare a pretreatment electrode.
(2) Drawing a standard curve: nicotine standard solutions of 0.0561g/L, 0.1136g/L, 0.1682g/L, 0.2351g/L were formulated using nicotine standard and 0.01mol/L buffer solution (phosphate: citrate molar ratio =1, ph = 6.8). And (2) respectively dropwise adding 200 mu L of nicotine standard solution to the pretreatment electrode obtained in the step (1), performing cyclic voltammetry analysis on the potential (the initial voltage is 0.4V, and the termination voltage is 1.4V), and recording a voltammetry curve to obtain a characteristic response current value of the nicotine. Under the same test condition, the characteristic response current value corresponding to the concentration of each standard solution is recorded in sequence and is drawn into a standard curve.
(3) Measurement of electronic cigarette samples: a diluted sample was prepared by diluting 0.5mL of electronic cigarette liquid to 5mL using the above phosphoric acid buffer solution (phosphate: citrate molar ratio =1, ph =6.8, 0.01mol/L). And (3) detecting the current value of the diluted sample by using a cyclic voltammetry method through a pretreatment electrode, detecting the sample in parallel for five times, substituting the detected current value into the standard curve in the step (2), calculating to obtain a nicotine concentration detection value in the diluted sample, further calculating to obtain the nicotine concentration in the electronic cigarette liquid, and recording the nicotine concentration detection value in a table 1.
(4) And (4) repeating the step (3), except that 1mg/mL of nicotine standard substance is added in the process of preparing the diluted sample in the step (3) so that the concentration of the nicotine standard substance in the diluted sample is 0.100g/L (nicotine plus scalar), and the nicotine concentration detection values are recorded in Table 1.
(5) And (4) repeating the step (3), except that 1mg/mL of nicotine standard substance is added in the process of preparing the diluted sample in the step (3) so that the concentration of the nicotine standard substance in the diluted sample is 0.400g/L (nicotine plus scalar), and the nicotine concentration detection values are recorded in Table 1.
Test parameters of cyclic voltammetry: the measuring voltage is-0.5 to 1.4V, and the scanning speed is 200mV/s
TABLE 1 detection of nicotine concentration by electrochemical method
| Serial number | Nicotine adding quantity (g/L) | Nicotine detection value (g/L) | Recovery (%) | RSD(％) |
| 1 | 0 | 0.215 | - | 2.4 |
| 2 | 0.100 | 0.320 | 101.59％ | 2.8 |
| 3 | 0.400 | 0.598 | 97.24％ | 2.6 |
The serial number 1 is nicotine detection data of a diluted sample prepared after the electronic cigarette liquid is diluted; number 2 is nicotine concentration detection data detected after a nicotine standard is additionally added in the process of preparing an electronic cigarette liquid diluted sample so that the concentration of the nicotine standard is 0.100 g/L; and the number 3 is the nicotine concentration detection data detected after the nicotine standard substance is additionally added in the process of preparing the electronic cigarette liquid diluted sample so that the concentration of the nicotine standard substance is 0.400 g/L.
FIG. 1 is a standard curve of a standard substance of example 1 of the present invention, with peak current (in μ A) on the abscissa and concentration (in g/L) on the ordinate; the standard curve of the standard is y =0.5758x-0.0046 2 =0.9976, x is the peak current and y is the nicotine concentration of the diluted standard.
In the embodiment 1, the silver electrode is activated by using sulfuric acid before detection, and a specific acidic buffer solution is selected during detection, so that the accuracy of a unitary linear function fitting curve of the standard substance in the range of 0.05-0.45g/L of nicotine can be further improved, and compared with the comparative example 1, the detection result is high in precision and good in repeatability, and the relative standard deviation RSD is less than 3%.
Comparative example 1
Detecting the nicotine content of the electronic cigarette liquid by High Performance Liquid Chromatography (HPLC), wherein the detection method comprises the following steps:
(1) Diluting 0.5mL of electronic cigarette liquid to 5mL by using a buffer solution to prepare a diluted sample;
(2) Detecting the nicotine content of the diluted sample by using a high performance liquid chromatography external standard method, wherein the nicotine detection value is recorded in table 2;
(3) Repeating the steps (1) and (2), except that 1mg/mL nicotine standard substance is added in the process of preparing the diluted sample in the step (1) to ensure that the concentration of the nicotine standard substance in the diluted sample is 0.100g/L (nicotine plus scalar), and the nicotine concentration detection value is recorded in a table 2;
(4) Different in the step (1) and the step (2) are repeated, in the process of preparing the diluted sample in the step (1), 1mg/mL nicotine standard substance is added, so that the concentration of the nicotine standard substance in the diluted sample is 0.400g/L (nicotine plus scalar), and the nicotine concentration detection value is recorded in a table 2.
TABLE 2 detection of nicotine concentration by high performance liquid chromatography
| Serial number | Nicotine adding quantity (g/L) | Nicotine detection value (g/L) | Recovery (%) | RSD(％) |
| 1 | 0 | 0.220 | - | 2.1 |
| 2 | 0.100 | 0.325 | 101.56％ | 2.5 |
| 3 | 0.400 | 0.635 | 102.42％ | 2.7 |
Comparative example 2
Comparative example 2 differs from example 1 in that comparative example 2 does not have an electrochemical treatment step.
The nicotine content of the electronic cigarette liquid is detected electrochemically, the whole process is carried out at 25 ℃, and the detection method comprises the following steps:
(1) Drawing a standard curve: a nicotine standard solution of known gradient concentration was prepared using a nicotine standard and 0.01mol/L buffer solution (phosphate: citrate molar ratio =1, ph = 6.8). Respectively dropping 200 μ L of nicotine standard solution on a C-Ag/AgCl-C screen printing electrode, performing cyclic voltammetry analysis (initial voltage is 0.4V and final voltage is 1.4V) on the potential, and recording voltammetry curve to obtain the characteristic response current value of nicotine. Under the same test condition, the characteristic response current value corresponding to each standard solution concentration is recorded in sequence and is drawn into a standard curve.
(2) Measurement of electronic cigarette samples: a diluted sample was prepared by diluting 0.5mL of electronic cigarette liquid to 5mL using the above phosphoric acid buffer solution (phosphate: citrate molar ratio =1, ph =6.8, 0.01mol/L). And (2) detecting the current value of the diluted sample by using a C-Ag/AgCl-C screen printing electrode to perform cyclic voltammetry, detecting the sample in parallel for five times, substituting the detected current value into the standard curve obtained in the step (1), calculating to obtain a nicotine concentration detection value in the diluted sample, further calculating to obtain the nicotine concentration in the electronic cigarette liquid, and recording the nicotine concentration detection value in a table 3.
(3) And (4) repeating the step (3), except that 1mg/mL of nicotine standard is added in the process of preparing the diluted sample in the step (3) so that the concentration of the nicotine standard in the diluted sample is 0.100g/L (nicotine plus scalar), and the nicotine concentration detection values are recorded in Table 3.
(4) And (4) repeating the step (3), except that 1mg/mL of nicotine standard substance is added in the process of preparing the diluted sample in the step (3) so that the concentration of the nicotine standard substance in the diluted sample is 0.400g/L (nicotine plus scalar), and the nicotine concentration detection values are recorded in Table 3.
Table 3 comparative example 2 detection of electrochemical nicotine concentration
| Serial number | Nicotine adding quantity (g/L) | Nicotine detection value (g/L) | Recovery (%) | RSD(％) |
| 1 | 0 | 0.189 | - | 3.5 |
| 2 | 0.100 | 0.236 | 81.67％ | 4.9 |
| 3 | 0.400 | 0.387 | 65.70％ | 7.6 |
Comparative example 3
Comparative example 3 is different from example 1 in that a 220AT screen-printed gold electrode manufactured by wangton china ltd, switzerland was used as the screen-printed electrode.
The nicotine content of the electronic cigarette liquid is detected electrochemically, the whole process is carried out at 25 ℃, and the detection method comprises the following steps:
(1) Activation treatment of 220AT screen printing gold electrode: under the condition that the measuring voltage is-0.5 to +1.5V, 200 mu L of sulfuric acid solution with the concentration of 0.1mol/L is dripped on a screen printing electrode for electrochemical treatment, and the initial potential is 0.4V and the final potential is 1.4V through cyclic voltammetry until a stable cyclic voltammetry curve graph is obtained to prepare a pretreatment electrode.
(2) Drawing a standard curve: a nicotine standard solution of known gradient concentration was prepared using a nicotine standard and 0.01mol/L buffer solution (phosphate: citrate molar ratio =1, ph = 6.8). And (2) respectively dropwise adding 200 mu L of nicotine standard solution to the pretreatment electrode obtained in the step (1), carrying out cyclic voltammetry analysis (the initial voltage is 0.4V, and the final voltage is 1.4V) on the potential, and recording a voltammetry curve to obtain the characteristic response current value of the nicotine. Under the same test condition, the characteristic response current value corresponding to each standard solution concentration is recorded in sequence and is drawn into a standard curve.
(3) Measurement of electronic cigarette samples: a diluted sample was prepared by diluting 0.5mL of electronic cigarette liquid to 5mL using the above phosphoric acid buffer solution (phosphate: citrate molar ratio =1, ph =6.8, 0.01mol/L). And (3) detecting the current value of the diluted sample by using a cyclic voltammetry method through a pretreatment electrode, detecting the sample in parallel for five times, substituting the detected current value into the standard curve in the step (2), calculating to obtain a nicotine concentration detection value in the diluted sample, further calculating to obtain the nicotine concentration in the electronic cigarette liquid, and recording the nicotine concentration detection value in a table 4.
(4) And (4) repeating the step (3), except that 1mg/mL of nicotine standard is added in the process of preparing the diluted sample in the step (3) so that the concentration of the nicotine standard in the diluted sample is 0.100g/L (nicotine plus scalar), and the nicotine concentration detection values are recorded in Table 4.
(5) And (4) repeating the step (3), except that 1mg/mL of nicotine standard substance is added in the process of preparing the diluted sample in the step (3) so that the concentration of the nicotine standard substance in the diluted sample is 0.400g/L (nicotine plus scalar), and the nicotine concentration detection values are recorded in a table 4.
Table 4 comparative example 3 detection of electrochemical nicotine concentration
| Serial number | Nicotine adding quantity (g/L) | Nicotine detection value (g/L) | Recovery (%) | RSD(％) |
| 1 | 0 | 0.206 | - | 3.4 |
| 2 | 0.100 | 0.308 | 100.65％ | 3.6 |
| 3 | 0.400 | 0.632 | 104.29％ | 3.9 |
It can be seen that when the reference electrode is replaced with the corresponding gold electrode, the relative standard deviation RSD of the corresponding detection method is greater than 3%.
Claims (10)
1. An electrochemical method for quantitatively determining a nicotine concentration, comprising the steps of:
(1) Adding a sulfuric acid solution to a screen printing electrode for electrochemical treatment to prepare a pretreatment electrode; the screen printing electrode comprises a reference electrode, and the reference electrode comprises Ag and AgCl; the electrochemical treatment is a voltammetry test;
(2) Preparing diluted standard substances with different known concentrations, respectively detecting the current value of the diluted standard substances by using the pretreatment electrodes through a voltammetry method, and performing linear fitting to prepare a standard curve;
(3) And diluting a sample to be detected by using a buffer solution to prepare a diluted sample, detecting the current value of the diluted sample by using the pretreatment electrode to perform voltammetry, substituting the current value of the diluted sample into the standard curve, and calculating the nicotine concentration.
2. The electrochemical process of claim 1, wherein the standard curve is y =0.5758x-0.0046, x is peak current, and y is nicotine concentration.
3. The electrochemical method of claim 1, wherein in step (1), the screen-printed electrodes further comprise a carbon working electrode, an auxiliary electrode; the working electrode is a carbon working electrode, the reference electrode is an Ag/AgCl reference electrode, and the auxiliary electrode is a carbon-to-auxiliary electrode.
4. The electrochemical process of claim 1, wherein the sulfuric acid solution is an aqueous solution of sulfuric acid having a concentration of 0.01 to 0.10mol/L.
5. The electrochemical method according to claim 1, wherein in the step (1), the electrochemical treatment is to perform the voltammetry test on the sulfuric acid solution by using the screen-printed electrode, and the step is stopped when a stable arsenic peak profile of the voltammetry curve is obtained.
6. The electrochemical method of claim 1, wherein in step (1), the voltammetry comprises at least one of cyclic voltammetry, square wave voltammetry, linear sweep voltammetry, conventional pulse voltammetry, and differential pulse voltammetry.
7. The electrochemical method according to claim 6, wherein the test parameters of the cyclic voltammetry are: the measuring voltage is-0.5 to 1.5V, the scanning speed is 30 to 60mV/s, and the scanning interval is 0.0005 to 0.0015V.
8. The electrochemical method according to claim 1, wherein in the step (3), the buffer solution comprises a weak acid salt, the weak acid salt comprises a phosphate and an acetate, and the phosphate: the molar ratio of the acetate is 1: (0.5-1.5).
9. The electrochemical process of claim 8, wherein the weak acid salt is present in a concentration of 0.001 to 2M in step (3).
10. The electrochemical process according to claim 1, wherein in the step (3), the buffer solution has a pH of 6 to 8.
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