CN113340871A - Rapid detection method for illegally added metformin in health food - Google Patents
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- 238000001514 detection method Methods 0.000 title claims abstract description 28
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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Abstract
The invention discloses a rapid detection method for illegally adding metformin into health food, which comprises the following steps: preparing a standard substance to-be-detected liquid; (2) sample pretreatment: (21) weighing a proper amount of sample, adding absolute methanol for oscillation, and placing in an ultrasonic extractor for ultrasonic treatment for 10 minutes to obtain an extracting solution; (22) shaking the extractive solution, and filtering; (3) surface enhanced laser raman spectroscopy: taking appropriate amount of filtrate as to-be-detected liquid, sequentially adding surface enhancing reagent and acidifying agent, and recording to 705cm‑1(±3cm‑1)、957cm‑1(±3cm‑1)、1062cm‑1(±3cm‑1) The existence of characteristic peaks. The method is simple and convenient, has low cost, is beneficial to field operation, and can quickly detect the result; qualitative analysis of a large number of samples can be realized; the usage amount of chemical reagents is reduced, and the harm to operators and the pollution to the environment are reduced; high speed, low cost and easy operation.
Description
Technical Field
The invention relates to the technical field of health product detection, in particular to a rapid detection method for illegally adding metformin into health food.
Background
Metformin is a biguanide oral hypoglycemic agent. Has multiple mechanisms of action, including delaying the uptake of glucose from the gastrointestinal tract, increasing peripheral glucose utilization by increasing insulin sensitivity, and inhibiting excessive gluconeogenesis in the liver and kidney. The main side effect of metformin is gastrointestinal reaction, and nausea, vomiting and diarrhea are common. After being taken, the traditional Chinese medicine composition has the symptoms of hypodynamia, drowsiness, weight loss, dizziness, rash and the like in some cases. In addition, the drug may reduce vitamin B12The absorption of (b), affects the synthesis of hemoglobin. Metformin generally exists in the form of metformin hydrochloride, and the hypoglycemic bulk drugs such as metformin hydrochloride are listed in a substance list which is published by the office of the State food and drug administration in 2012 and is possibly illegally added to health food.
The existing detection method of metformin hydrochloride is' supplementary inspection method for drug inspection and inspection item approval part 2009029 of State food and drug administration. In the method, thin layer chromatography is used for rapid screening; high performance liquid chromatography is used for qualitative inspection; and (4) rapidly screening or qualitatively checking a sample with a positive result, and verifying the sample by a liquid chromatography-mass spectrometry method to give an inspection report. Wherein the thin layer chromatography for rapid screening is prepared by grinding capsule content, tablet or granule, ultrasonically extracting with methanol, filtering, volatilizing, adding 1mL methanol for redissolving as test solution, and adding 1mg/mL solution of metformin hydrochloride and methanol as control solution. Performing thin layer chromatography (appendix VI B of first edition of Chinese pharmacopoeia 2005) by sucking test solution and control solution 10 μ L respectively, and spotting on the same silica gel GF254Spreading ethyl acetate-methanol-water-glacial acetic acid (6:1:0.5:0.5) as developing agent on the thin layer plate, taking out, air drying, and spraying withAnd (3) placing the mixed solution of 10% sodium ferricyanide nitrite, 1% potassium ferricyanide and 10% sodium hydroxide solution in the same amount into the daylight for inspection, wherein if fluorescence quenching spots appear on the chromatogram of the test sample at the positions corresponding to the chromatogram of the reference sample, the mixed solution is positive by metformin hydrochloride, and if the fluorescence quenching spots do not appear in the chromatogram of the test sample, the mixed solution is negative. Although the method is simple to operate and short in time consumption compared with the high-performance liquid chromatography, the method uses a plurality of types of reagents, most of the reagents have certain toxicity, artificial influence factors are large, the experimental reproducibility is poor, and the experimental time is about 30-60 minutes.
The Raman spectrum is discovered in 1928, the Nobel prize of physics is obtained in 1930, the Nobel prize is universally existed in all molecules, the structure information of the molecules can be reliably provided, the Nobel prize is not influenced by various solvents, the laser Raman spectrum becomes an important analysis means of compounds along with the use of a laser light source, the Nobel prize is widely applied to the fields of criminal investigation identification, mineral analysis and the like, and the surface enhanced Raman scattering discovered in Fleischmann M in 1974 enables the detection of trace substances to be possible. The Surface Enhanced Raman Spectroscopy (SERS) utilizes trace molecules to be adsorbed on the surfaces of Cu, Ag, Au and other metal sols and electrodes, and Raman spectrum signals of the SERS can be enhanced by 104～106And the defect of low sensitivity of the conventional Raman spectroscopy is overcome. The technology has the characteristics of rapidness, sensitivity, rich information, high selectivity and the like, but is mainly used for qualitative detection. In recent years, surface-enhanced raman spectroscopy has begun to be applied to the detection of many illegal additives, functional components, and the like.
In order to overcome the defects of the existing detection method and technology, the invention provides a rapid qualitative detection method for illegally adding metformin into health-care food, which is based on a surface-enhanced Raman spectroscopy technology and can be sensitive, rapid and convenient.
Disclosure of Invention
The invention aims to solve the technical problem of providing a rapid detection method for illegally adding metformin into health food, which adopts Raman spectrum characteristic peak signals and selects 705cm-1(±3cm-1)、957cm-1(±3cm-1)、1062cm-1(±3cm-1) As a characteristic Raman peak, the method has accurate qualification and the whole detection process is finished within 15 minutesAnd the method realizes rapid qualitative, convenient and low-cost detection.
The technical problem to be solved by the invention is realized by the following technical scheme:
a rapid detection method for illegally adding metformin into health food comprises the following steps:
(1) preparing a standard substance to-be-detected liquid:
accurately weighing 10mg of metformin standard substance, and diluting to 10mL with anhydrous methanol to obtain 1000ppm of standard solution to be detected;
(2) sample pretreatment:
(21) weighing a proper amount of sample, adding absolute methanol for oscillation, and placing in an ultrasonic extractor for ultrasonic treatment for 10 minutes to obtain an extracting solution;
(22) shaking the extractive solution, and filtering;
(3) surface enhanced laser raman spectroscopy:
taking appropriate amount of filtrate as to-be-detected liquid, sequentially adding surface enhancing reagent and acidifying agent, and recording to 705cm-1(±3cm-1)、957cm-1(±3cm-1)、1062cm-1(±3cm-1) If no characteristic peak exists, the metformin is contained in the sample, and if no obvious characteristic Raman peak exists, the content of the metformin in the sample is below the detection limit value.
Preferably, in the above technical solution, the ratio of the absolute methanol added in step (21) to the sample is V: m ═ (5-10): 1.
Preferably, in the above technical solution, the ratio of the absolute methanol added in step (21) to the sample is V: m ═ 5-8: 1.
Preferably, in the above technical scheme, the surface enhancing reagent in step (3) is gold nano sol or silver nano sol.
Preferably, in the technical scheme, the acidifying agent in the step (3) is a 2mol/L nitric acid solution.
Preferably, in the above technical solution, the volume ratio of the surface enhancing reagent to the liquid to be detected in step (3) is (1-10): 1.
Preferably, in the above technical solution, the volume ratio of the surface enhancing reagent to the liquid to be measured in step (3) is (3-5): 1.
Preferably, in the technical scheme, the volume ratio of the acidifying agent to the liquid to be measured in the step (3) is (1-3): 1.
Preferably, in the technical scheme, the volume ratio of the acidifying agent to the liquid to be measured in the step (3) is (1-2): 1.
Preferably, in the above technical solution, the detection condition of the raman spectrum in step (3) includes:
laser power: 200 mW;
integration time: 5 s;
integration times: 1;
smoothing parameters: 3.
the technical scheme of the invention has the following beneficial effects:
1. the method is simple and convenient, has low cost, is beneficial to field operation, and can quickly give out a detection result;
2. qualitative analysis of a large number of samples can be realized simultaneously;
3. the using amount of chemical reagents is greatly reduced, the harm to operators is reduced, and the pollution of wastes to the environment is reduced;
4. high speed (within 15 min), low cost (about 5 yuan for each sample inspection), and easy operation.
Drawings
Fig. 1 is a raman spectrum of an illegal addition of metformin in the health food of the present invention.
Detailed Description
Specific examples of the invention are described in detail below to facilitate a further understanding of the invention.
All experimental procedures used in the following examples are conventional unless otherwise specified. Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Firstly, preparing standard substance to-be-detected liquid
Accurately weighing 10mg of metformin standard substance, and diluting to 10mL with anhydrous methanol to obtain 1000ppm standard solution to be detected.
Second, sample preparation
a. Weighing a proper amount of sample, adding methanol, oscillating, and placing in an ultrasonic extractor for ultrasonic treatment for 10 minutes.
b. Shaking the extractive solution, and filtering.
Third, qualitative determination
Conditions of the apparatus
a) Laser power: 200 mW.
b) Integration time: for 5 sec.
c) Integration times: 1.
d) smoothing parameters: 3.
taking appropriate amount of filtrate as to-be-detected solution, sequentially adding surface enhancing reagent and acidifying agent, shaking, detecting according to 705cm-1(±3cm-1)、957cm-1(±3cm-1)、1062cm-1(±3cm-1) Evaluating whether a characteristic Raman peak exists or not: if the sample contains metformin, the content of metformin in the sample is below the detection limit value if no obvious characteristic Raman peak exists.
Example 1 Rapid qualitative analysis of illegal addition of metformin to health food
Sample preparation: the capsule health-care food for reducing blood sugar is sold in the market.
Pretreatment:
a. the capsule content corresponding to one-time oral dosage is taken, added with 2mL of anhydrous methanol for oscillation, and placed in an ultrasonic extractor for ultrasonic treatment for 10 minutes.
b. Shaking the extractive solution, and filtering.
And (3) qualitative analysis:
taking 100 μ L sample filtrate, adding 400 μ L gold and silver intensifier, adding 100 μ L acidifying agent, shaking, and detecting according to 705cm-1(±3cm-1)、957cm-1(±3cm-1)、1062cm-1(±3cm-1) Evaluating whether a characteristic Raman peak exists or not:
if the liquid to be detected is 705cm-1(±3cm-1)、957cm-1(±3cm-1)、1062cm-1(±3cm-1) If there is a characteristic peak, it indicates that the sample contains metformin.
Example 2 Rapid qualitative analysis of illegal addition of metformin to health foods
Sample preparation: the sugar-reducing health-care food in the form of tablet or granule is sold in the market.
Pretreatment:
a. taking tablets or granules corresponding to one-time oral dosage, grinding, adding 2mL of anhydrous methanol, oscillating, and placing in an ultrasonic extractor for 10 minutes by ultrasonic treatment.
b. Shaking the extractive solution, and filtering.
And (3) qualitative analysis:
taking 100 μ L sample filtrate, adding 400 μ L gold and silver intensifier, adding 100 μ L acidifying agent, shaking, and detecting according to 705cm-1(±3cm-1)、957cm-1(±3cm-1)、1062cm-1(±3cm-1) Evaluating whether a characteristic Raman peak exists or not:
if the liquid to be detected is 705cm-1(±3cm-1)、957cm-1(±3cm-1)、1062cm-1(±3cm-1) If there is a characteristic peak, it indicates that the sample contains metformin.
Example 3 Rapid qualitative analysis of illegal addition of metformin to health foods
Sample preparation: the liquid hypoglycemic health food is sold in the market.
And (3) qualitative analysis:
the sample is not required to be pretreated, 100 mu L of sample is taken, 400 mu L of gold and silver reinforcing agent is added, 100 mu L of acidifying agent is added, the sample is shaken up and then detected according to 705cm-1(±3cm-1)、957cm-1(±3cm-1)、1062cm-1(±3cm-1) Evaluating whether a characteristic Raman peak exists or not:
if the liquid to be detected is 705cm-1(±3cm-1)、957cm-1(±3cm-1)、1062cm-1(±3cm-1) If there is a characteristic peak, it indicates that the sample contains metformin.
The invention adopts special software which is special and solidified in a portable Raman spectrometer to realize an ultra-fast, low-cost and on-site identification method for illegally adding metformin into health food. The detection time of one sample is less than 15 minutes, the operation is simple, the operator does not need to have a strong professional background, the reading is visual, and the numerical value can be directly read from the instrument interface.
The technology is applied to the detection of the illegal addition of the metformin in the health food for the first time, and the illegal addition of the metformin in the health food is determined by the Raman spectral characteristic analysis of the metformin, wherein the lowest detection limit of the detection method in the invention is 2 ppm. The test is completed within 15min, has the obvious characteristics of accuracy, rapidness, no damage and low cost, is suitable for field emergency detection, enterprise automatic control detection, large-batch sample screening detection and the like, effectively identifies illegal addition of metformin in the health food, and protects consumers' rights and benefits.
Although the present invention has been described with reference to the above embodiments, it should be understood that the present invention is not limited thereto, and various changes and modifications may be made by those skilled in the art without departing from the spirit and scope of the present invention.
Claims (10)
1. A rapid detection method for illegally adding metformin into health food is characterized by comprising the following steps:
(1) preparing a standard substance to-be-detected liquid:
accurately weighing 10mg of metformin standard substance, and diluting to 10mL with anhydrous methanol to obtain 1000ppm of standard solution to be detected;
(2) sample pretreatment:
(21) weighing a proper amount of sample, adding absolute methanol for oscillation, and placing in an ultrasonic extractor for ultrasonic treatment for 10 minutes to obtain an extracting solution;
(22) shaking the extractive solution, and filtering;
(3) surface enhanced laser raman spectroscopy:
taking appropriate amount of filtrate as to-be-detected liquid, sequentially adding surface enhancing reagent and acidifying agent, and recording to 705cm-1(±3cm-1)、957cm-1(±3cm-1)、1062cm-1(±3cm-1) If no characteristic peak exists, the sample contains metformin, and if no obvious characteristic Raman peak exists, the content of metformin in the sample is detectedThe limit value is less than or equal to.
2. The method for rapidly detecting the illegal addition of metformin according to claim 1, wherein the absolute methanol added in the step (21) is in a ratio of V: m ═ (5-10):1 with respect to the sample.
3. The method for rapidly detecting the illegal addition of metformin according to claim 2, wherein the absolute methanol added in the step (21) is added in a ratio of V: m ═ (5-8): 1.
4. The method for rapidly detecting the illegal addition of metformin according to claim 1, wherein the surface enhancing reagent in the step (3) is gold nanosol or silver nanosol.
5. The method for rapidly detecting the illegal addition of metformin according to claim 1, wherein the acidifying agent in step (3) is a 2mol/L nitric acid solution.
6. The method for rapidly detecting the illegal addition of metformin according to claim 1, wherein the volume ratio of the surface enhancing reagent to the liquid to be detected in the step (3) is (1-10): 1.
7. The method for rapidly detecting the illegal addition of metformin according to claim 6, wherein the volume ratio of the surface enhancing reagent to the liquid to be detected in the step (3) is (3-5): 1.
8. The method for rapidly detecting the illegal addition of the metformin according to claim 1, wherein the volume ratio of the acidifying agent to the liquid to be detected in the step (3) is (1-3): 1.
9. The method for rapidly detecting the illegal addition of the metformin according to claim 8, wherein the volume ratio of the acidifying agent to the liquid to be detected in the step (3) is (1-2): 1.
10. The method for rapidly detecting the illegal addition of metformin according to claim 1, wherein the detection conditions of Raman spectrum in step (3) comprise:
laser power: 200 mW;
integration time: 5 s;
integration times: 1;
smoothing parameters: 3.
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| 曹玲等: "显微共聚焦拉曼检测中药中非法添加的化学降糖药", 《药物分析杂志》 * |
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