CN113311040A - Electrochemical method for detecting capsaicin in food - Google Patents
Electrochemical method for detecting capsaicin in food Download PDFInfo
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- CN113311040A CN113311040A CN202110579471.2A CN202110579471A CN113311040A CN 113311040 A CN113311040 A CN 113311040A CN 202110579471 A CN202110579471 A CN 202110579471A CN 113311040 A CN113311040 A CN 113311040A
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- YKPUWZUDDOIDPM-SOFGYWHQSA-N capsaicin Chemical compound COC1=CC(CNC(=O)CCCC\C=C\C(C)C)=CC=C1O YKPUWZUDDOIDPM-SOFGYWHQSA-N 0.000 title claims abstract description 131
- 229960002504 capsaicin Drugs 0.000 title claims abstract description 64
- 235000017663 capsaicin Nutrition 0.000 title claims abstract description 64
- 235000013305 food Nutrition 0.000 title claims abstract description 23
- 238000002848 electrochemical method Methods 0.000 title claims abstract description 19
- 239000012086 standard solution Substances 0.000 claims abstract description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 25
- 238000007650 screen-printing Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000001514 detection method Methods 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 238000012417 linear regression Methods 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 11
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims abstract description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 15
- 230000003647 oxidation Effects 0.000 claims description 12
- 238000007254 oxidation reaction Methods 0.000 claims description 12
- 238000001903 differential pulse voltammetry Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000012982 microporous membrane Substances 0.000 claims description 9
- 230000003321 amplification Effects 0.000 claims description 8
- 238000003199 nucleic acid amplification method Methods 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 7
- 150000001450 anions Chemical class 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000002414 normal-phase solid-phase extraction Methods 0.000 claims description 6
- 238000000746 purification Methods 0.000 claims description 6
- 238000002137 ultrasound extraction Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000007865 diluting Methods 0.000 claims description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000012085 test solution Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 4
- 239000012670 alkaline solution Substances 0.000 claims 1
- 230000035945 sensitivity Effects 0.000 abstract description 4
- 239000007772 electrode material Substances 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 238000003950 stripping voltammetry Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 description 5
- 238000004128 high performance liquid chromatography Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 235000007862 Capsicum baccatum Nutrition 0.000 description 3
- 240000001844 Capsicum baccatum Species 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 235000019633 pungent taste Nutrition 0.000 description 3
- 239000012535 impurity Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002048 multi walled nanotube Substances 0.000 description 2
- 230000001953 sensory effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241001132374 Asta Species 0.000 description 1
- 206010006784 Burning sensation Diseases 0.000 description 1
- 235000002566 Capsicum Nutrition 0.000 description 1
- CMSMOCZEIVJLDB-UHFFFAOYSA-N Cyclophosphamide Chemical compound ClCCN(CCCl)P1(=O)NCCCO1 CMSMOCZEIVJLDB-UHFFFAOYSA-N 0.000 description 1
- 241000124008 Mammalia Species 0.000 description 1
- 239000006002 Pepper Substances 0.000 description 1
- 241000722363 Piper Species 0.000 description 1
- 235000016761 Piper aduncum Nutrition 0.000 description 1
- 235000017804 Piper guineense Nutrition 0.000 description 1
- 235000008184 Piper nigrum Nutrition 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 229940007061 capsicum extract Drugs 0.000 description 1
- 239000001943 capsicum frutescens fruit extract Substances 0.000 description 1
- 238000012864 cross contamination Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010794 food waste Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 235000019617 piquancy Nutrition 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000006188 syrup Substances 0.000 description 1
- 235000020357 syrup Nutrition 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
Abstract
The invention discloses an electrochemical method for detecting capsaicin in food, which specifically comprises the following steps: (1) preparing a screen printing carbon electrode; (2) preparing a capsaicin standard solution; (3) drawing a standard curve: taking a screen printing carbon electrode as a working electrode, taking a saturated calomel electrode as a reference electrode, taking a platinum wire electrode as a counter electrode to obtain a three-electrode system, then inserting the three-electrode system into a capsaicin standard solution, stirring, enriching and scanning to obtain a linear regression equation, and drawing a standard curve; (4) preparing a solution to be detected; (5) and (6) detecting. According to the method, an unmodified silk-screen printing carbon electrode is used as an electrode material, differential pulse-adsorption stripping voltammetry is adopted, and the detection sensitivity can be greatly improved according to the linear relation between an electrochemical response signal and the concentration of an object to be detected, so that the background current is effectively reduced, and the capsaicin is quantitatively detected simply, quickly and accurately.
Description
Technical Field
The invention relates to the technical field of analytical chemistry, in particular to an electrochemical method for detecting capsaicin in food.
Background
The chemical name of capsaicin is trans-8-methyl-N-vanillyl-6-nonenamide with the chemical formula of C18H27NO3Is an active ingredient of the pepper. Capsaicin is irritating to mammals, including humans, and produces burning sensations in the mouth.
The conventional measure of pungency is the Schoville Heat Unit (SHU), measured by the Schoville sensory technique or test. According to this technique, the capsicum extract was diluted in syrup until the heat or acridity was no longer perceived by the tongue of five tasters (especially trained volunteers). However, the biggest drawback of the schwarrior sensory test is inaccuracy, since it depends on human subjectivity. An alternative technique for the quantitative measurement of spiciness is High Pressure Liquid Chromatography (HPLC), which measures spiciness in ASTA piquancy units, although more objective and accurate than the traditional schoeweiler unit, is more complex to operate and more expensive.
Several researchers have additionally studied electrochemical methods for detecting capsaicinoids. Electrochemical methods include determining a relationship between the potential and the concentration of a redox species at the electrode surface. To detect capsaicin, the electrode surface is modified by a nano-scale structure such as multi-walled carbon nanotubes (MWCNTs). However, such electrode surface modifications lead to unnecessary expense and complexity and may limit the performance or measurement reliability of the electrode under certain conditions.
Therefore, how to develop a rapid, simple and low-cost method for detecting capsaicin is a problem to be solved urgently by the technical personnel in the field.
Disclosure of Invention
In view of the above, the present invention provides an electrochemical method for detecting capsaicin in food, so as to solve the deficiencies in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
an electrochemical method for detecting capsaicin in food specifically comprises the following steps:
(1) preparation of screen-printed carbon electrodes
Soaking the screen printing carbon electrode in alkali liquor, then repeatedly washing with water, and airing to obtain the screen printing carbon electrode for later use;
(2) preparation of capsaicin standard solution
Firstly, weighing a certain amount of capsaicin solid, then adding absolute ethyl alcohol to dissolve, diluting and fixing the volume to obtain a series of capsaicin standard solutions with different concentrations;
(3) drawing of standard curve
Taking a screen printing carbon electrode as a working electrode, taking a saturated calomel electrode as a reference electrode, taking a platinum wire electrode as a counter electrode to obtain a three-electrode system, then inserting the three-electrode system into a capsaicin standard solution, stirring and enriching, finally scanning by using a differential pulse voltammetry method, obtaining a linear regression equation according to the linear relation between the oxidation peak current value and the concentration of the capsaicin standard solution, and drawing a standard curve;
(4) preparation of the test solution
Sequentially carrying out ultrasonic extraction and anion solid phase extraction and small column purification treatment on a food sample to be detected, dissolving the obtained extract with water, and filtering the dissolved extract through a microporous membrane to obtain a liquid to be detected;
(5) detection of
Inserting the three-electrode system into the liquid to be detected, stirring and enriching, then scanning by using differential pulse voltammetry, and calculating according to the oxidation peak current value and a linear regression equation to obtain the content of capsaicin in the liquid to be detected.
The invention has the advantages that the manufacturing cost of the screen printing carbon electrode is low, the manufacturing process is simple and quick, the mass production can be realized, the time and energy loss of the traditional column electrode grinding and polishing is avoided, and the experimental cross contamination possibly caused in the repeated use process of the column electrode is also avoided.
Further, in the step (1), the alkali liquor is NaOH solution with the molar concentration of 1-2 mol/L; soaking for 30-50 min; the number of rinsing times is 3-5.
The further beneficial effect of the adoption is that the impurities on the surface of the screen printing carbon electrode can be removed through soaking in alkali liquor, washing and drying, so that the sensitivity of the screen printing carbon electrode is improved.
Further, in the step (2), the concentration of the capsaicin standard solution is 1-10 μ g/L.
Further, in the steps (3) and (5), the stirring and enriching speed is 80-120r/min, and the time is 5-8 min.
The method has the further beneficial effects that the detection of oxidation peak current of capsaicin in the standard solution and the solution to be detected on the screen printing carbon electrode is facilitated through stirring and enrichment, so that the detection accuracy is improved.
Further, in the steps (3) and (5), the scanning voltage is 0.2-0.4V, the potential amplification is 3-5mV, the pulse amplitude is 40-60mV, and the pulse frequency is 40-60 Hz.
The method has the further beneficial effects that through the setting of the parameters, the oxidation peak current values of the standard solution and the liquid to be detected can be efficiently and accurately measured by adopting the differential pulse voltammetry.
Further, in the step (4), the pore diameter of the microporous membrane is 100-1000 nm.
The food residue detection device has the further beneficial effects that residues in food to be detected can be removed through microporous membrane filtration, and the influence of impurities on the detection result of liquid to be detected is avoided.
According to the technical scheme, compared with the prior art, the invention has the following beneficial effects:
according to the method, an unmodified silk-screen printing carbon electrode is used as an electrode material, differential pulse-adsorption stripping voltammetry is adopted, and the detection sensitivity can be greatly improved according to the linear relation between an electrochemical response signal and the concentration of an object to be detected, so that the background current is effectively reduced, and the capsaicin is quantitatively detected simply, quickly and accurately.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. 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.
Example 1
The electrochemical method for detecting the capsaicin in the food specifically comprises the following steps:
(1) preparation of screen-printed carbon electrodes
Soaking the screen printing carbon electrode in NaOH solution with the molar concentration of 1mol/L for 50min, then repeatedly washing with water for 3 times, and airing to obtain the screen printing carbon electrode for later use;
(2) preparation of capsaicin standard solution
Firstly weighing a certain amount of capsaicin solid, then adding absolute ethyl alcohol to dissolve, diluting and fixing the volume to obtain a series of capsaicin standard solutions with different concentrations (1 mug/L, 2 mug/L, 6 mug/L, 8 mug/L and 10 mug/L);
(3) drawing of standard curve
Taking a silk-screen printing carbon electrode as a working electrode, taking a saturated calomel electrode as a reference electrode, taking a platinum wire electrode as a counter electrode to obtain a three-electrode system, then inserting the three-electrode system into a capsaicin standard solution, stirring for 8min at the speed of 80r/min for enrichment, finally scanning by a differential pulse voltammetry method, wherein the scanning voltage is 0.2V, the potential amplification is 3mV, the pulse amplitude is 40mV, the pulse frequency is 40Hz, obtaining a linear regression equation according to the linear relation between the oxidation peak current value and the concentration of the capsaicin standard solution, and drawing a standard curve;
(4) preparation of the test solution
Sequentially carrying out ultrasonic extraction and anion solid phase extraction and small column purification treatment on a food sample to be detected, dissolving the obtained extract with water, and filtering the dissolved extract through a microporous membrane with the aperture of 100nm to obtain a liquid to be detected;
(5) detection of
Inserting the three-electrode system into the liquid to be detected, stirring for 8min at the speed of 80r/min for enrichment, then scanning by a differential pulse voltammetry, wherein the scanning voltage is 0.2V, the potential amplification is 3mV, the pulse amplitude is 40mV, and the pulse frequency is 40Hz, and calculating according to the oxidation peak current value and a linear regression equation to obtain the content of capsaicin in the liquid to be detected.
Example 2
The electrochemical method for detecting the capsaicin in the food specifically comprises the following steps:
(1) preparation of screen-printed carbon electrodes
Soaking the screen printing carbon electrode in NaOH solution with the molar concentration of 2mol/L for 40min, then repeatedly washing with water for 4 times, and airing to obtain the screen printing carbon electrode for later use;
(2) preparation of capsaicin standard solution
Firstly weighing a certain amount of capsaicin solid, then adding absolute ethyl alcohol to dissolve, diluting and fixing the volume to obtain a series of capsaicin standard solutions with different concentrations (1 mug/L, 2 mug/L, 6 mug/L, 8 mug/L and 10 mug/L);
(3) drawing of standard curve
Taking a silk-screen printing carbon electrode as a working electrode, taking a saturated calomel electrode as a reference electrode, taking a platinum wire electrode as a counter electrode to obtain a three-electrode system, then inserting the three-electrode system into a capsaicin standard solution, stirring for 6min at the speed of 100r/min for enrichment, finally scanning by a differential pulse voltammetry method, wherein the scanning voltage is 0.3V, the potential amplification is 4mV, the pulse amplitude is 50mV, the pulse frequency is 50Hz, obtaining a linear regression equation according to the linear relation between the oxidation peak current value and the concentration of the capsaicin standard solution, and drawing a standard curve;
(4) preparation of the test solution
Sequentially carrying out ultrasonic extraction and anion solid phase extraction and small column purification treatment on a food sample to be detected, dissolving the obtained extract with water, and filtering the dissolved extract through a microporous membrane with the aperture of 500nm to obtain a liquid to be detected;
(5) detection of
Inserting the three-electrode system into the liquid to be detected, stirring for 6min at the speed of 100r/min for enrichment, then scanning by a differential pulse voltammetry, wherein the scanning voltage is 0.3V, the potential amplification is 4mV, the pulse amplitude is 50mV, and the pulse frequency is 50Hz, and calculating according to the oxidation peak current value and a linear regression equation to obtain the content of capsaicin in the liquid to be detected.
Example 3
The electrochemical method for detecting the capsaicin in the food specifically comprises the following steps:
(1) preparation of screen-printed carbon electrodes
Soaking the screen printing carbon electrode in NaOH solution with the molar concentration of 2mol/L for 30min, then repeatedly washing with water for 5 times, and airing to obtain the screen printing carbon electrode for later use;
(2) preparation of capsaicin standard solution
Firstly weighing a certain amount of capsaicin solid, then adding absolute ethyl alcohol to dissolve, diluting and fixing the volume to obtain a series of capsaicin standard solutions with different concentrations (1 mug/L, 2 mug/L, 6 mug/L, 8 mug/L and 10 mug/L);
(3) drawing of standard curve
Taking a silk-screen printing carbon electrode as a working electrode, taking a saturated calomel electrode as a reference electrode, taking a platinum wire electrode as a counter electrode to obtain a three-electrode system, then inserting the three-electrode system into a capsaicin standard solution, stirring at the speed of 120r/min for 5min for enrichment, finally scanning by a differential pulse voltammetry method, wherein the scanning voltage is 0.4V, the potential amplification is 5mV, the pulse amplitude is 60mV, the pulse frequency is 60Hz, obtaining a linear regression equation according to the linear relation between the oxidation peak current value and the concentration of the capsaicin standard solution, and drawing a standard curve;
(4) preparation of the test solution
Sequentially carrying out ultrasonic extraction and anion solid phase extraction and small column purification treatment on a food sample to be detected, dissolving the obtained extract with water, and filtering the dissolved extract through a microporous membrane with the pore diameter of 1000nm to obtain a liquid to be detected;
(5) detection of
Inserting the three-electrode system into the liquid to be detected, stirring at the speed of 120r/min for 5min for enrichment, scanning by a differential pulse voltammetry, wherein the scanning voltage is 0.4V, the potential amplification is 5mV, the pulse amplitude is 60mV, and the pulse frequency is 60Hz, and calculating according to the oxidation peak current value and a linear regression equation to obtain the content of capsaicin in the liquid to be detected.
Performance testing
Preparing a screen-printed carbon electrode according to the method of example 2, preparing a capsaicin standard solution, drawing a standard curve, sequentially performing ultrasonic extraction and anion solid phase extraction and small column purification treatment on the commercially available pod pepper, dissolving the obtained extract with water, filtering the dissolved extract through a microporous membrane with the pore diameter of 500nm to obtain a solution to be detected, detecting the content of capsaicin in the solution to be detected, and comparing the content of capsaicin with the detection result of HPLC. In parallel with three experiments, the content of capsaicin in the pod pepper detected by the method of example 2 is 4.2mg/kg, and the content of capsaicin in the pod pepper detected by HPLC is 4.2 mg/kg.
The tests show that the method takes an unmodified silk-screen printing carbon electrode as an electrode material, adopts the differential pulse-adsorption stripping voltammetry, can greatly improve the detection sensitivity according to the linear relation between the electrochemical response signal and the concentration of the object to be detected, effectively reduces the background current, and realizes simple, quick and accurate quantitative detection of capsaicin.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. An electrochemical method for detecting capsaicin in food is characterized by comprising the following steps:
(1) preparation of screen-printed carbon electrodes
Soaking the screen printing carbon electrode in alkali liquor, then repeatedly washing with water, and airing to obtain the screen printing carbon electrode for later use;
(2) preparation of capsaicin standard solution
Firstly, weighing a certain amount of capsaicin solid, then adding absolute ethyl alcohol to dissolve, diluting and fixing the volume to obtain a series of capsaicin standard solutions with different concentrations;
(3) drawing of standard curve
Taking a screen printing carbon electrode as a working electrode, taking a saturated calomel electrode as a reference electrode, taking a platinum wire electrode as a counter electrode to obtain a three-electrode system, then inserting the three-electrode system into a capsaicin standard solution, stirring and enriching, finally scanning by using a differential pulse voltammetry method, obtaining a linear regression equation according to the linear relation between the oxidation peak current value and the concentration of the capsaicin standard solution, and drawing a standard curve;
(4) preparation of the test solution
Sequentially carrying out ultrasonic extraction and anion solid phase extraction and small column purification treatment on a food sample to be detected, dissolving the obtained extract with water, and filtering the dissolved extract through a microporous membrane to obtain a liquid to be detected;
(5) detection of
Inserting the three-electrode system into the liquid to be detected, stirring and enriching, then scanning by using differential pulse voltammetry, and calculating according to the oxidation peak current value and a linear regression equation to obtain the content of capsaicin in the liquid to be detected.
2. The electrochemical method for detecting capsaicin in food according to claim 1, wherein in the step (1), the alkaline solution is a NaOH solution with a molar concentration of 1-2 mol/L.
3. The electrochemical method for detecting capsaicin in food according to claim 1, wherein the soaking time in the step (2) is 30-50 min.
4. The electrochemical method for detecting capsaicin in food according to claim 1, wherein in the step (1), the washing is performed 3 to 5 times.
5. The electrochemical method for detecting capsaicin in food according to claim 1, wherein in the step (2), the concentration of the standard capsaicin solution is 1-10 μ g/L.
6. The electrochemical method for detecting capsaicin in food according to claim 1, wherein in the steps (3) and (5), the stirring enrichment speed is 80-120r/min, and the time is 5-8 min.
7. The electrochemical method for detecting capsaicin in food according to claim 1, wherein in the steps (3) and (5), the scanned voltage is 0.2-0.4V, the potential amplification is 3-5mV, the pulse amplitude is 40-60mV, and the pulse frequency is 40-60 Hz.
8. The electrochemical method for detecting capsaicin in food according to claim 1, wherein in the step (4), the pore size of the microporous membrane is 100-1000 nm.
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