CN110333214A - The detection method of illegal addition drug ingredient in a kind of health care product - Google Patents
The detection method of illegal addition drug ingredient in a kind of health care product Download PDFInfo
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- CN110333214A CN110333214A CN201811352883.7A CN201811352883A CN110333214A CN 110333214 A CN110333214 A CN 110333214A CN 201811352883 A CN201811352883 A CN 201811352883A CN 110333214 A CN110333214 A CN 110333214A
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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
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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
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Abstract
The invention discloses a kind of detection methods of addition drug ingredient illegal in health care product, comprising the following steps: (1) takes health care product powder to be placed in a beaker, organic solvent ultrasonic extraction is added；Extracting solution is transferred in sample cell, the acid or aqueous slkali of addition, oscillation extraction, stratification；Water layer is transferred in centrifuge tube spare as sample to be tested；(2) sample to be tested is taken, metal-sol is sequentially added and concentration is inorganic salts flocculant of the 0.01M to saturation, mix, Raman spectrometer detection interior is then placed on and is detected.The detection method high sensitivity, detection limit is low, at low cost, the multicomponent to addition may be implemented, unknown ingredient drug detects.
Description
Technical field
The present invention relates to a kind of detection methods of addition drug ingredient illegal in health care product, belong to health care product detection field.
Background technique
Food and medicine Surveillance Authority, China issue from July, 2005 go into effect " health food registration management is done
Method (tentative) " in regulation: " health food refers to and claims with specific healthcare function or using replenishing vitamins, minerals as mesh
Food.It is edible to be suitable for specific crowd, there is adjusting body function not produce not for the purpose for the treatment of disease to human body
Raw acute, subacute or chronic hazard food." the 50th article of the law of food safety " production and operation are defined as to the ingredient of food
Food in must not add drug ".
From the point of view of security risk in recent years monitors and supervise sampling observation situation, weight-reducing class, improves sleep at auxiliary hyperglycemic class
Class, alleviation physical fatigue class, aided blood pressure-lowering these fifth types health food are the severely afflicated areas of illegal addition chemicals.It is eaten in country
Product Drug Administration announce " substance list (first) that may be illegally added in health food " be related to altogether weight-reducing, it is auxiliary
Hypoglycemic, antifatigue, adjusting is helped to be immunized, improve sleep, six major class health care product of aided blood pressure-lowering.
In " illegally the adding chemical component quick screening method theory and practice in health-oriented products " one that Xie Zhihao etc. writes
In book, the detection of the illegal addition drug ingredient of the other health care product of different lines is described, detection is the spy according to illegal addition drug
Determine group and predetermined substance generates sediment to determine whether containing illegal additive, easy to operate, the erroneous judgement of correlation method
Rate is lower, but its detection limit is generally higher.
In document " the 8 kinds of drug tests and instance analysis illegally added in hypoglycemic class health food ", " decompression class health care
The liquid chromatogram of chemicals is added in food and Chinese patent drug " in all detected using application of gas chromatorgraphy/mass, but the instrument of the detection
Device is expensive, at high cost.
Document " silaenafil that adds in In Situ Thin Layer Surface enhanced Raman spectroscopy method detection Chinese patent drug and health care product ",
" Raman spectrum quickly detects the research that phenolphthalein is illegally added in slimming health product ", " phenformin hydrochloride and Metformin hydrochloride
In the Surface enhanced Raman spectroscopy research of nanometer silver surface eutectoid content " and " surface of the demethyl ephedrine in thin-layer chromatography original position
Enhancing raman study " in a few illegal drug standard items is measured with Raman spectrum, or to certain health care product
The drug for adding certain ingredient carries out Raman detection, cannot detect to multicomponent, the unknown ingredient drug of addition, adaptability
It is wideless.
Summary of the invention
It is an object of the invention in place of overcome the deficiencies in the prior art, provide illegal addition drug in a kind of health care product
Detection method.
The technical solution adopted by the present invention to solve the technical problems is:
The detection method of illegal addition drug ingredient in a kind of health care product, comprising the following steps:
(1) it takes 0.1g~10g health care product powder to be placed in a beaker, 1mL~20mL intensive polar solvent ultrasonic extraction is added,
The mass volume ratio range of health care product and intensive polar solvent is 1:1~1:10g/mL；Extracting solution is transferred in sample cell, is added
5mL~20mL organic solvent, oscillation extraction, stratification；Organic solvent is transferred in Volatile bottle and is dried with nitrogen；
(2) take appropriate highly polar organic solvent in above-mentioned volatilization pipe, oscillation is spare as prepare liquid for several times；
(3) 10uL~500uL sample to be tested is taken, 50~200uL metal-sol is sequentially added and 50uL~200uL concentration is
0.01M is mixed to the inorganic salts flocculant of saturation, is then placed on Raman spectrometer detection interior and is detected.
Another technical solution of the invention are as follows: the detection method of illegal addition drug ingredient in a kind of health care product, including with
Lower step:
(1) it takes 0.1g~10g health care product powder to be placed in a beaker, 1mL~20mL organic solvent ultrasonic extraction is added, protect
The mass volume ratio range of strong product and organic solvent is 1:1~1:10g/mL；Extracting solution is transferred in sample cell, is added
Bis- aqueous solutions of 0.2mL~2mL, oscillation extraction, stratification；Water layer is transferred in centrifuge tube spare as sample to be tested；
(2) 10uL~500uL sample to be tested is taken, 50~200uL metal-sol is sequentially added and 50uL~200uL concentration is
0.01M is mixed to the inorganic salts flocculant of saturation, is then placed on Raman spectrometer detection interior and is detected.
Preferably, it is 0.1mM-1M acid or aqueous slkali that the secondary water, which is concentration,.
Preferably, the intensive polar solvent is methanol, ethyl alcohol, dimethyl sulfoxide, acetone, secondary water or its mixed solution.
Preferably, the organic solvent be n-hexane, ethyl acetate, hexamethylene, methylene chloride, toluene, heptane or its
Mixture.
Preferably, the metal-sol is nanogold or nano silver.
Preferably, the acid is citric acid, phosphoric acid, hydrochloric acid, nitric acid, sulfuric acid or acetic acid.
Preferably, the alkali is sodium hydroxide, potassium hydroxide or barium hydroxide.
Preferably, the inorganic salts flocculant is sulfate, nitrate, carbonate, silicate, acetate, phosphate, halogen
Or mixtures thereof salt dissolving.
Preferably, in step (1), extracting solution can be centrifuged before being transferred to sample cell or film filtering.
Preferably, in step (1), organic solvent can add adsorbent before volatilization or before oscillation.
Preferably, the adsorbent is N- propyl ethylenediamine, active carbon, phosphoenolpyruvate, graphitized carbon, oxidation
Or mixtures thereof aluminium, anhydrous sodium sulfate, anhydrous magnesium sulfate.
The technical program compared with the background art, it has the following advantages:
The inspection to drug ingredient is added in health care product may be implemented in the method that the present invention uses Surface enhanced Raman spectroscopy
It surveys, detection limit is not required to expensive instrument down to 1ppm, at low cost.
The method that the present invention uses Surface enhanced Raman spectroscopy, may be implemented the multicomponent to addition, unknown ingredient drug
It is detected, wide adaptation range.
The entire detection time of detection method of the invention is in 5min-10min, and convenient and efficient, the method pacifies operator
Completely without injury, it is well suited for the field quick detection to addition drug ingredient illegal in health care product.
Detailed description of the invention
Below with reference to figure, the invention will be further described with embodiment.
Fig. 1 is the surface-enhanced Raman light for assisting blood-pressure reducing health care product mark-on 100ppm clonidine hydrochloride different metal colloidal sol
Spectrum.
Fig. 2 is the Surface enhanced Raman spectroscopy for assisting anti-fatigue health-product containing mark-on 100ppm silaenafil.
Fig. 3 is the Surface enhanced Raman spectroscopy for assisting blood-pressure reducing health care product addition atenolol and whether adding graphitized carbon.
Fig. 4 is the Surface enhanced Raman spectroscopy for assisting slimming health product addition phenolphthalein.
Fig. 5 is the Surface enhanced Raman spectroscopy for assisting health-caring product capable of reducing blood sugar addition hydrochloric acid phenylacetic acid guanidine.
Specific embodiment
The contents of the present invention are illustrated below by embodiment:
The nanogold the preparation method comprises the following steps: 250mL round-bottomed flask is added in the aqueous solution of chloraurate of the 0.01wt% of 100mL
In, it is heated to after acutely boiling, is vigorously stirred down the 1wt% trisodium citrate aqueous solution for rapidly joining 1mL, continue heating stirring
After 60min, stop heating, continues to stand after stirring 30min, room temperature natural cooling.
The nano silver the preparation method comprises the following steps: the 1mM silver nitrate aqueous solution of 100mL is added in 250mL round-bottomed flask, heating
To violent boiling, it is vigorously stirred down the 1wt% trisodium citrate aqueous solution for rapidly joining 1mL, continues heating stirring 60min
Afterwards, stop heating, continue to stand after stirring 30min, room temperature natural cooling.Show that nanogold and nano silver can expire in Fig. 1
The detection of sufficient clonidine hydrochloride.
Embodiment 1: taking 0.1g aided blood pressure-lowering health care product powder to be placed in a beaker, and mark-on 100ppm clonidine hydrochloride adds
Enter 3mL methylene chloride ultrasonic extraction, will be collected after the used membrane filtration of extracting solution with sample cell, the vibration of 0.5mL1mM hydrochloric acid is added
Swing extraction.Water layer is transferred to after stratification spare in centrifuge tube.Take two parts of 200uL samples in Raman sample bottle, respectively
100uL nanogold and nano silver is added, then is separately added into the mixing of 100uL 0.5M sodium sulphate.Raman sample bottle is transferred to drawing
Graceful sensing chamber carries out Raman detection, investigates the influence of different metal colloidal sol detection, obtains the Surface enhanced Raman spectroscopy such as Fig. 1, schemes
1 display the method can satisfy the detection of clonidine hydrochloride in aided blood pressure-lowering health care product.
Embodiment 2: 0.5g auxiliary anti-fatigue health-product containing powder is taken to be placed in a beaker, mark-on 10ppm silaenafil is added
5mL secondary water ultrasonic extraction, which is 0.1mM-1M acid or aqueous slkali, for extracting solution centrifugation is transferred to sample
It is collected in pipe, 5mL methylene chloride oscillation extraction is added.Organic phase is transferred in Volatile bottle after stratification and is dried with nitrogen.Add
Enter the oscillation of 1ml methanol, it is spare as prepare liquid.Take 100uL sample in Raman sample bottle, addition 100uL nanogold, then plus
Enter the mixing of 100uL 0.1M sodium chloride.Raman sample bottle is transferred to Raman detection room, Raman detection is carried out, obtains the table such as Fig. 2
Face enhances Raman spectrum.The preparation method is the same as that of Example 1 for the nanogold.Fig. 2 shows that the method can satisfy anti-fatigue health-product containing
The detection of middle silaenafil.
Embodiment 3: taking 2g aided blood pressure-lowering health care product powder to be placed in a beaker, and mark-on 100ppm atenolol, adds respectively
Enter 10mL petroleum ether ultrasonic extraction, extracting solution be divided into two parts to be transferred in sample cell and is collected, addition 2mL 0.1M acetic acid,
And 0.3g graphitized carbon is added in portion thereto, graphitized carbon, oscillation extraction is not added in another.Water layer is shifted after stratification
It is spare into centrifuge tube.Two parts of samples respectively take 200uL in Raman sample bottle, addition 50uL nano silver, add 50uL 2M
Potassium phosphate mixes.Raman sample bottle is transferred to Raman detection room, Raman detection is carried out, investigates the detection of different blood pressure lowering drugs
Situation obtains the Surface enhanced Raman spectroscopy such as Fig. 3.The preparation method is the same as that of Example 1 for the nano silver.It shows, add or is not added in Fig. 3
Graphitized carbon can satisfy the detection of aided blood pressure-lowering health care product mark-on 100ppm atenolol.
Embodiment 4: 1g auxiliary slimming health product powder is taken to be placed in a beaker, 5mL n-hexane is added in mark-on 100ppm phenolphthalein
Extracting solution is transferred in sample cell and collects by ultrasonic extraction, and 1mL 1M sodium hydroxide oscillation extraction is added.By water after stratification
Layer is transferred to spare in centrifuge tube.It takes three parts of 100uL samples in Raman sample bottle, all addition 100uL nanogold, then adds respectively
Enter the mixing of 100uL 0.1M barium chloride.Raman sample bottle is transferred to Raman detection room, Raman detection is carried out, obtains the table such as Fig. 4
Face enhances Raman spectrum.The preparation method is the same as that of Example 1 for the nanogold.Show that the method can satisfy auxiliary weight-reducing and protect in Fig. 4
The detection of strong product mark-on 100ppm phenolphthalein.
Embodiment 5: taking 5g aided blood pressure-lowering health care product powder to be placed in a beaker, and mark-on 100ppm hydrochloric acid benzene second is double respectively
Guanidine is added 10mL toluene ultrasonic extraction, extracting solution is transferred in sample cell and is collected, and 1mL 0.1M sulfuric acid oscillation extraction is added.
Water layer is transferred to after stratification spare in centrifuge tube.Take five parts of 200uL samples in Raman sample bottle, all addition 100uL
Nanogold, then it is separately added into the mixing of 100uL 1M potassium chloride.Raman sample bottle is transferred to Raman detection room, carries out Raman inspection
It surveys, obtains the Surface enhanced Raman spectroscopy such as Fig. 5.The preparation method is the same as that of Example 1 for the nanogold.Show that the method can expire in Fig. 5
The detection of sufficient aided blood pressure-lowering health care product mark-on 100ppm phenformin hydrochloride.
The above is only the preferred embodiment of the present invention, the range implemented of the present invention that therefore, it cannot be limited according to, i.e., according to
Equivalent changes and modifications made by the invention patent range and description, should still be within the scope of the present invention.
Claims (10)
1. the detection method of illegal addition drug ingredient in a kind of health care product, it is characterised in that: the following steps are included:
(1) it takes 0.1g~10g health care product powder to be placed in a beaker, 1mL~20mL intensive polar solvent ultrasonic extraction, health care is added
The mass volume ratio range of product and intensive polar solvent is 1:1~1:10g/mL；Extracting solution is transferred in sample cell, 5mL is added
~20mL organic solvent, oscillation extraction, stratification；Organic solvent is transferred in Volatile bottle and is dried with nitrogen；
(2) take appropriate highly polar organic solvent in above-mentioned volatilization pipe, oscillation is spare as prepare liquid for several times；
(3) 10uL~500uL sample to be tested is taken, 50~200uL metal-sol is sequentially added and 50uL~200uL concentration is
0.01M is mixed to the inorganic salts flocculant of saturation, is then placed on Raman spectrometer detection interior and is detected.
2. the detection method of illegal addition drug ingredient in a kind of health care product, it is characterised in that: the following steps are included:
(1) it takes 0.1g~10g health care product powder to be placed in a beaker, 1mL~20mL organic solvent ultrasonic extraction is added；It will extract
Liquid is transferred in sample cell, and bis- aqueous solutions of 0.5mL~5mL, oscillation extraction, stratification is added；Water layer is transferred to centrifugation
It is spare as sample to be tested in pipe；
(2) 50uL~500uL sample to be tested is taken, 50~100uL metal-sol is sequentially added and 10uL~200uL concentration is
0.01M is mixed to the inorganic salts flocculant of saturation, is then placed on Raman spectrometer detection interior and is detected.
3. the detection method of illegal addition drug ingredient in health care product according to claim 2, it is characterised in that: described
Secondary water is that concentration is 0.1mM-1M acid or aqueous slkali.
4. the detection method of illegal addition drug ingredient in health care product according to claim 1 or 2, it is characterised in that: institute
The organic solvent stated is or mixtures thereof n-hexane, ethyl acetate, hexamethylene, methylene chloride, toluene, heptane.
5. the detection method of illegal addition drug ingredient in health care product according to claim 1, it is characterised in that: described
Intensive polar solvent is methanol, ethyl alcohol, dimethyl sulfoxide, acetone, secondary water or its mixed solution.
6. the detection method of illegal addition drug ingredient in health care product according to claim 1 or 2, it is characterised in that: institute
Stating inorganic salts flocculant is or mixtures thereof sulfate, nitrate, carbonate, silicate, acetate, phosphate, halide salt.
7. the detection method of illegal addition drug ingredient in health care product according to claim 1, it is characterised in that: in step
(1) in, extracting solution first centrifugation or film filtering before being transferred to sample cell.
8. the detection method of illegal addition drug ingredient in health care product according to claim 1, it is characterised in that: in step
(1) in, adsorbent is first added before organic reagent volatilization.
9. the detection method of illegal addition drug ingredient in health care product according to claim 2, it is characterised in that: in step
(1) in, organic reagent first adds adsorbent before secondary water extraction is added.
10. the detection method of illegal addition drug ingredient in health care product according to claim 8, it is characterised in that: described
Adsorbent is N- propyl ethylenediamine, active carbon, phosphoenolpyruvate, graphitized carbon, aluminium oxide, anhydrous sodium sulfate, anhydrous
Or mixtures thereof magnesium sulfate.
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Cited By (5)
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| CN112213294A (en) * | 2020-09-22 | 2021-01-12 | 立穹(上海)光电科技有限公司 | Method for rapidly detecting sildenafil in health-care product |
| CN113092445A (en) * | 2021-04-14 | 2021-07-09 | 中朗正健(苏州)生物技术有限公司 | Method for detecting illegal addition of omeprazole in weight-losing health-care food |
| CN113324978A (en) * | 2021-06-01 | 2021-08-31 | 天津市食品安全检测技术研究院 | Method for detecting calcium and iron in health food |
| CN113340871A (en) * | 2021-06-09 | 2021-09-03 | 河北省食品检验研究院 | Rapid detection method for illegally added metformin in health food |
| CN113984737A (en) * | 2021-11-19 | 2022-01-28 | 北京鉴知技术有限公司 | Surface enhanced Raman spectroscopy detection method for detecting phenolphthalein in sample |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113092445A (en) * | 2021-04-14 | 2021-07-09 | 中朗正健(苏州)生物技术有限公司 | Method for detecting illegal addition of omeprazole in weight-losing health-care food |
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| CN113984737A (en) * | 2021-11-19 | 2022-01-28 | 北京鉴知技术有限公司 | Surface enhanced Raman spectroscopy detection method for detecting phenolphthalein in sample |
| CN113984737B (en) * | 2021-11-19 | 2024-03-01 | 北京鉴知技术有限公司 | Surface enhanced Raman spectrum detection method for detecting phenolphthalein in sample |
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