Rapid detection method for non-pralazone illegally added in food
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-01-12
- Publication Date
- 2026-04-03
AI Technical Summary
Current technologies lack rapid and low-cost methods for detecting illegally added non-prazones in food, and existing methods are time-consuming and costly.
The food samples were subjected to secondary extraction using both highly polar and non-polar extractants, followed by nitrogen blowing to remove the extractants. The samples were then eluted with a highly polar solvent and finally treated with nano-gold sol and inorganic salt flocculants before being detected by Raman spectroscopy.
It enables rapid detection of non-prazones in food, with low detection limits, simple detection steps, low cost, and short time, providing technical support for food safety.
Smart Images
Figure CN121783947A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of drug detection technology, and specifically relates to a rapid detection method for the illegal addition of non-prazone to food. Background Technology
[0002] Non-prazone is a nonsteroidal anti-inflammatory drug (NSAID) with antipyretic, analgesic, and anti-inflammatory effects. In my country, it is illegal to add non-prazone to food.
[0003] Currently, there is no comprehensive national standard method for the determination of non-prazoline, therefore, it is urgent to establish a rapid screening and detection method for non-prazoline. The currently reported methods for the determination of non-prazoline mainly include high-performance liquid chromatography (HPLC) and high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS), but these methods have drawbacks such as high detection costs and long processing times.
[0004] Therefore, there is a need to provide a rapid method for detecting the illegal addition of nonsteroidal anti-inflammatory drugs (NSAIDs) to food, providing technical support for the detection of illegally added NSAIDs in food and providing strong protection for food safety. Summary of the Invention
[0005] In view of this, the present invention provides a rapid detection method for the illegal addition of non-prazolam to food, aiming to solve at least one of the technical problems in the background art.
[0006] This invention is implemented as follows: A rapid detection method for the illegal addition of non-prazolam to food, comprising the following steps: The food sample was subjected to secondary extraction using a strongly polar extractant and a non-polar extractant, respectively, to obtain the supernatant after extraction; then, the non-polar extractant was removed from the supernatant using nitrogen blowing. The supernatant after nitrogen blowing was eluted with a highly polar solvent to obtain the test solution; Metal sol and inorganic salt flocculant were added sequentially to the test solution, mixed well, and then detected using a Raman spectrometer.
[0007] Furthermore, the highly polar extractant used in the secondary extraction is at least one of acetonitrile, acetone, and ethanol; the non-polar extractant is at least one of petroleum ether, n-hexane, and cyclohexane.
[0008] Furthermore, the highly polar extractant is acetonitrile; the non-polar extractant is petroleum ether.
[0009] Furthermore, the highly polar solvent used in the elution is ethanol or acetonitrile.
[0010] Furthermore, the metal sol is a nano-gold sol; the inorganic salt flocculant is a sodium chloride solution or a calcium chloride solution.
[0011] Furthermore, the concentration of the sodium chloride solution or calcium chloride solution is 0.1 M to 1 M; According to the volume ratio, the test solution: metal sol: inorganic salt flocculant = 1: (0.5~2): (0.5~2).
[0012] Furthermore, the secondary extraction step specifically includes: According to the ratio of food to highly polar extractant = 1g: (3~6)mL, add highly polar extractant to food, shake to extract, centrifuge to separate layers, and obtain the first extract; Add the non-polar extractant to the first extract at a volume ratio of (2~5):3, shake thoroughly for 8~12 seconds, centrifuge to separate the layers, and collect the supernatant.
[0013] Further, the elution step specifically involves adding a strong polar solvent to the supernatant after nitrogen blowing treatment according to a volume ratio of supernatant to strong polar solvent of 1:(0.1~0.3), shaking thoroughly for 10s~20s, and obtaining the test solution.
[0014] Furthermore, the laser wavelength used for detection by the Raman spectrometer is 785 nm.
[0015] Compared with other methods in the prior art, the surface-enhanced Raman spectroscopy (SERS) of this invention has the advantages of high sensitivity and low detection limit, with a detection limit of 1 mg / kg for non-prazone. This invention utilizes SERS technology for the rapid determination of illegally added non-prazone in food, providing technical support for the detection of illegally added non-steroidal anti-inflammatory drugs in food and offering strong protection for food safety.
[0016] Furthermore, the detection steps of this invention are simple and low-cost; the pretreatment and detection time is short. Attached Figure Description
[0017] Figure 1 SERS spectra of non-prazoline standards at gradient concentrations; Figure 2 The SERS spectra of the simulated sample in Example 1 are compared with those of the non-prazoline standard. Figure 3 This is a comparison of the SERS spectra of the simulated sample and the non-prazoline standard in Example 2. Detailed Implementation
[0018] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention.
[0019] A rapid detection method for the illegal addition of non-prazolam to food, comprising the following steps: S1. The food sample is subjected to secondary extraction using a strong polar extractant and a non-polar extractant, respectively, to obtain the supernatant after extraction; then the strong polar extractant and non-polar extractant are removed from the supernatant by nitrogen blowing. In this invention, highly polar extractants and non-polar extractants are used as water-soluble reagents, which can be used for direct extraction. By rationally selecting extractants with matching polarities, the extraction efficiency of non-prazoline can be significantly improved.
[0020] S1 specifically includes: S11. According to the ratio of food to highly polar extractant = 1g: (3~6)mL, add highly polar extractant (at least one of acetonitrile, acetone, and ethanol, preferably acetonitrile) to the food, shake and extract, centrifuge to separate the layers, and obtain the first extract. S12. According to the volume ratio of the first extract to the non-polar extractant = (2~5):3, add the non-polar extractant (at least one of petroleum ether, n-hexane, and cyclohexane, preferably petroleum ether) to the first extract, shake thoroughly for 8s~12s, centrifuge to separate the layers, and collect the supernatant. S13. Take the supernatant into a evaporation bottle, and pass nitrogen gas through it to evaporate the supernatant, thereby removing the strongly polar extractant and non-polar extractant from the supernatant.
[0021] S2. The supernatant after nitrogen blowing is eluted with a strong polar solvent (ethanol or acetonitrile) to obtain the test solution; Specifically: referring to the volume ratio of supernatant to strong polar solvent = 1: (0.1~0.3), add strong polar solvent to the supernatant after nitrogen blowing treatment, shake thoroughly for 10s~20s to obtain the test solution.
[0022] S3. Add metal sol and inorganic salt flocculant to the test solution in sequence, mix well and then use a Raman spectrometer for detection. Compare the detection results with the SERS spectrum of non-prazone standard to determine whether the food contains non-prazone and its content.
[0023] Specifically, the metal sol is a nano-gold sol; the synthesis steps of the nano-gold sol are as follows: first, heat 100 mL of HAuCl4 solution containing 0.01% to boiling, then quickly add 1 mL of 1% trisodium citrate aqueous solution, heat under reflux for 1 h, and cool to room temperature.
[0024] The inorganic salt flocculant is a sodium chloride solution or a calcium chloride solution with a concentration of 0.1 M to 1 M.
[0025] According to the volume ratio, the test solution: metal sol: inorganic salt flocculant = 1: (0.5~2): (0.5~2).
[0026] The laser wavelength used for Raman spectroscopy is 785 nm.
[0027] In practice, non-prazolam standards with gradient concentrations (0.01 mg / kg, 0.1 mg / kg, 1 mg / kg, 10 mg / kg) were accurately prepared using ultrapure water; 200 μL of the standard, 50 μL of sodium chloride solution (1 M), and 50 μL of gold nanoparticle sol were mixed and tested using a Raman spectrometer, forming a pattern as shown in the image. Figure 1 The SERS spectrum of the non-Prazoline standard is shown.
[0028] Example 1 A rapid detection method for the illegal addition of non-prazolam to food, comprising the following steps: S1. Weigh 1 g of food sample (compressed candy after crushing) containing 1 mg / kg of non-prazolam into a centrifuge tube, add 3 mL of acetonitrile for extraction, shake and centrifuge to separate the layers, take 2 mL of supernatant into another sample tube, add 3 mL of petroleum ether, shake thoroughly for about 10 s; take 1 mL of supernatant into a evaporation bottle and pass nitrogen gas through it for evaporation.
[0029] S2. Measure 0.2 mL of ethanol solution and add it to the evaporation bottle from step S1 for elution. Shake well for about 15 s and use it as the test solution.
[0030] S3. Take 50 μL of the test solution into the Raman sample cell, add 100 μL of gold nanoparticle sol and 100 μL of sodium chloride solution (1M), mix well, and then detect using a Raman spectrometer with a laser wavelength of 785 nm; collect the following... Figure 2 The Raman spectrum shown is compared with that shown below. Figure 1 Compare the SERS spectra of the non-prazoline standard shown, and determine whether the food contains non-prazoline based on the characteristic peaks.
[0031] Figure 2 The results showed that the Raman spectrum of the food sample in Example 1 had the same characteristic peaks as the SERS spectrum of the non-prazone standard, verifying that the food sample contained the illegal additive - non-prazone.
[0032] Example 2 A rapid detection method for the illegal addition of non-prazolam to food, comprising the following steps: S1. Weigh 5 g of food sample (coffee powder) containing 5 mg / kg of non-prazolam into a centrifuge tube, add 10 mL of ethanol for extraction, vortex, centrifuge to separate the layers, take 5 mL of supernatant into another sample tube, add 3 mL of n-hexane, and vortex thoroughly for about 10 s. Take 1 mL of supernatant into a evaporation flask and purge with nitrogen gas for evaporation.
[0033] S2. Measure 0.2 mL of acetonitrile solution into a evaporation flask and elute. Shake well for about 20 s and use as the test solution.
[0034] S3. Take 100 μL of the test solution into the Raman sample cell, add 100 μL of gold nanoparticle sol and 100 μL of calcium chloride solution (0.1 M), mix well, and then detect using a Raman spectrometer with a laser wavelength of 785 nm. Collect samples as shown below. Figure 3 The Raman spectrum shown is compared with that shown below. Figure 1 Compare the SERS spectra of the non-prazoline standard shown, and determine whether the food contains non-prazoline based on the characteristic peaks.
[0035] Figure 3 The results showed that the Raman spectrum of the food sample in Example 2 had the same characteristic peaks as the SERS spectrum of the non-prazone standard, verifying that the food sample contained the illegal additive - non-prazone.
[0036] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these modifications and improvements all fall within the scope of protection of the present invention. Therefore, the scope of protection of this patent should be determined by the appended claims.
Claims
1. A rapid detection method for illegally added non-prazone in food, characterized in that, The rapid detection method includes the following steps: The food sample was subjected to secondary extraction using a strongly polar extractant and a non-polar extractant, respectively, to obtain the supernatant after extraction; then, the non-polar extractant was removed from the supernatant using nitrogen blowing. The supernatant after nitrogen blowing was eluted with a highly polar solvent to obtain the test solution; Metal sol and inorganic salt flocculant were added sequentially to the test solution, mixed well, and then detected using a Raman spectrometer.
2. The rapid detection method for illegally added non-prazolam in food according to claim 1, characterized in that, The highly polar extractant used in the secondary extraction is at least one of acetonitrile, acetone, and ethanol; the non-polar extractant is at least one of petroleum ether, n-hexane, and cyclohexane.
3. The rapid detection method for illegally added non-prazolam in food according to claim 2, characterized in that, The highly polar extractant is acetonitrile; the non-polar extractant is petroleum ether.
4. The rapid detection method for illegally added non-prazolam in food according to claim 1, characterized in that, The highly polar solvent used in the elution is ethanol or acetonitrile.
5. The rapid detection method for illegally added non-prazolam in food according to claim 1, characterized in that, The metal sol is a nano-gold sol; the inorganic salt flocculant is a sodium chloride solution or a calcium chloride solution.
6. A rapid detection method for illegally added non-prazolam in food according to claim 5, characterized in that, The concentration of the sodium chloride solution or calcium chloride solution is 0.1 M to 1 M; According to the volume ratio, the test solution: metal sol: inorganic salt flocculant = 1: (0.5~2): (0.5~2).
7. A rapid detection method for illegally added non-prazolam in food according to claim 2 or 3, characterized in that, The specific steps of the secondary extraction are as follows: According to the ratio of food to highly polar extractant = 1g: (3~6)mL, add highly polar extractant to food, shake to extract, centrifuge to separate layers, and obtain the first extract; Add the non-polar extractant to the first extract at a volume ratio of (2~5):3, shake thoroughly for 8~12 seconds, centrifuge to separate the layers, and collect the supernatant.
8. A rapid detection method for illegally added non-prazolam in food according to claim 4, characterized in that, The elution step is as follows: according to the volume ratio of supernatant to strong polar solvent = 1: (0.1~0.3), add strong polar solvent to the supernatant after nitrogen blowing treatment, shake thoroughly for 10s~20s to obtain the test solution.
9. A rapid detection method for illegally added non-prazolam in food according to claim 1, characterized in that, The laser wavelength used for Raman spectroscopy is 785 nm.