Method for determining main components of calcined nacre mother medicinal material before and after irradiation

Abstract

The invention discloses a method for measuring main components of a calcined nacre mother medicinal material before and after irradiation, which comprises the following steps: (1) preparation of a test sample: weighing the irradiated calcined nacre mother, adding potassium bromide, putting into an agate mortar, uniformly grinding under an infrared lamp to obtain mixed powder, transferring the mixed powder into a mold, transferring the mold to a tablet press, vacuumizing, pressurizing, and drying to obtain the test sample; a test sample is obtained; (2) preparation of a reference substance: weighing calcined mother-of-pearl before irradiation, adding potassium bromide, placing in an agate mortar, uniformly grinding under an infrared lamp to obtain mixed powder, transferring the mixed powder into a mold, transferring the mold to a tablet press, vacuumizing and pressurizing to obtain the reference substance; and (3) determining the fingerprints of the test sample and the reference substance by using an infrared spectrometer method, and carrying out fingerprint change analysis. The method is of great significance to quality research before and after irradiation of the calcined mother-of-pearl and guarantee of the curative effect of the product.

Description

Technical Field

[0001] This invention belongs to the field of traditional Chinese medicine analysis technology, specifically relating to a method for determining the main components of calcined mother-of-pearl before and after irradiation. Background Technology

[0002] Mother-of-pearl, a traditional Chinese medicine. It refers to the shells of the three-sailed mussel *Hyriopsis cumingii* (Lea), the pleated crown mussel *Cristaria plicata* (Leach), or the pearl oyster *Pteria martensii* (Dunker). Calcined mother-of-pearl: Clean mother-of-pearl is calcined until brittle using the open calcination method. It has the functions of calming the liver and suppressing yang, soothing the mind and relieving fright, and improving eyesight and clearing away corneal opacity. It is used for headaches, dizziness, palpitations, insomnia, red eyes with corneal opacity, and blurred vision.

[0003] According to the Ministry of Health's "Standard for Sterilization Dosage of Traditional Chinese Medicine by Cobalt-60 Irradiation," calcined mother-of-pearl can be irradiated with a certain dose to kill microorganisms. However, there is currently no comprehensive method for quality analysis before and after irradiation. Summary of the Invention

[0004] Technical problem solved: To address the above-mentioned technical problem, this invention provides a method for determining the main components of calcined pearl powder before and after irradiation, thereby ensuring the efficacy of the product by conducting quality testing on calcined pearl powder before and after irradiation.

[0005] Technical solution: In a first aspect, the present invention provides a method for determining the main components of calcined mother-of-pearl before and after irradiation, comprising the following steps: (1) Preparation of test sample: Weigh the irradiated calcined mother-of-pearl, add potassium bromide, place it in an agate mortar, grind it evenly under an infrared lamp to obtain a mixed powder, transfer the mixed powder into a mold, transfer the mold to a tablet press, vacuum and pressurize to obtain the test sample; (2) Preparation of reference standard: Weigh the calcined mother-of-pearl before irradiation, add potassium bromide, place it in an agate mortar, grind it evenly under an infrared lamp to obtain a mixed powder, transfer the mixed powder into a mold, transfer the mold to a tablet press, vacuum and pressurize to obtain the reference standard; (3) The fingerprint spectra of the test sample and the reference sample were determined by infrared spectroscopy, and the changes in the fingerprint spectra were analyzed.

[0006] Preferably, the irradiation dose in step (1) is 8 kGy.

[0007] Preferably, in step (1), 1 mg of irradiated calcined mother-of-pearl is weighed and passed through a 200-mesh sieve; the ratio of potassium bromide added to the mass of irradiated calcined mother-of-pearl is 100:1, and the pressurization time is 1 min.

[0008] Preferably, in step (2), 1 mg of calcined mother-of-pearl before irradiation is weighed and passed through a 200-mesh sieve; the mass ratio of potassium bromide added to calcined mother-of-pearl before irradiation is 100:1, and the pressurization time is 1 min.

[0009] Preferably, in step (3), the infrared spectrometer has a measurement range of 4000–400 cm⁻¹. -1 .

[0010] Secondly, the present invention provides a fingerprint spectrum of calcined mother-of-pearl obtained using the determination method described in the first aspect, wherein the fingerprint spectrum has 7 common peaks, and the wavelengths of each common peak are as follows: Peak 1: 708 cm -1 ; Peak No. 2: 876 cm -1 ; Peak No. 3: 1419 cm -1 ; Peak No. 4: 1792 cm -1 ; Peak No. 5: 2516 cm -1 ; Peak No. 6: 2865 cm -1 ; Peak No. 7: 2976cm -1 .

[0011] Beneficial effects: The method of this invention confirms the authenticity of calcined mother-of-pearl, and the characteristic peaks in the spectrum represent the specific chemical components of calcined mother-of-pearl. Attached Figure Description

[0012] Figure 1 This is an infrared spectrum of sample S1 before irradiation in one embodiment of the present invention; Figure 2 This is the infrared spectrum of sample S1 after irradiation in one embodiment of the present invention; Figure 3 This is an infrared spectrum of samples S1-S6 before and after irradiation in one embodiment of the present invention. Detailed Implementation

[0013] The present invention will be described in detail below with reference to specific embodiments: Instruments: Fourier transform infrared spectrometer, WS70-1 infrared rapid dryer, YP-Z tablet press; Medicinal material: The sample of calcined mother-of-pearl was provided by Jiangsu 707 Natural Pharmaceutical Co., Ltd. Example

[0014] 1.1 Information on calcined mother-of-pearl samples is shown in Table 1 below: Table 1 Information on calcined mother-of-pearl samples

[0015] (1) Preparation of test sample: Weigh 1 mg of calcined mother-of-pearl after irradiation (irradiation dose of 8 kGy), pass it through a 200-mesh sieve; add 100 mg of potassium bromide, place it in an agate mortar, grind it evenly under an infrared lamp to obtain a mixed powder, transfer the mixed powder into a mold, transfer the mold to a tablet press, vacuum it, press it for 1 min to obtain the test sample; (2) Preparation of reference standard: Weigh 1 mg of calcined mother-of-pearl before irradiation and pass it through a 200-mesh sieve; add 100 mg of potassium bromide, place it in an agate mortar, grind it evenly under an infrared lamp to obtain a mixed powder, transfer the mixed powder into a mold, transfer the mold to a tablet press, vacuum it, press it for 1 min to obtain the reference standard; (3) Infrared spectroscopy at 4000–400 cm⁻¹ -1 The fingerprint spectra of the test sample and the reference sample were determined within the specified range, and the changes in the fingerprint spectra were analyzed.

[0016] 1.2 Methodological Examination 1.2.1 Precision Five consecutive measurements were performed on the same sample (S1), and the resulting infrared spectra were completely identical. The wavenumbers of the seven common peaks in the sample had a maximum RSD of 0.27% and a minimum of 0.05%.

[0017] 1.2.2 Stability The same sample (S1) was used for testing, and measurements were taken every 2 hours. The spectral lines obtained within 8 hours were basically identical. The wavenumbers of the 7 common peaks in the sample had a maximum RSD of 0.08% and a minimum of 0.01%.

[0018] 1.2.3 Repeatability Five samples (S1) were taken and pressed into pellets. The resulting infrared spectra were completely identical. The RSD of the seven common peaks in the samples ranged from a maximum of 0.97% to a minimum of 0.32%. These results indicate that the wavenumbers of the common peaks in the fingerprint spectrum are basically consistent, with a high degree of similarity, which meets the technical requirements for fingerprint spectrum research.

[0019] 1.3 Establishment of fingerprint map Table 2 shows the wavenumbers of the seven common peaks in 12 samples from 6 batches of calcined mother-of-pearl before and after irradiation. Table 2. Wavenumbers of the 7 common peaks in calcined mother-of-pearl

[0020] The fingerprint spectrum of the sample (before S1 irradiation) is as follows: Figure 1 As shown, the fingerprint spectrum of the sample (after S1 irradiation) is as follows: Figure 2 As shown; the fingerprint spectra of samples S1-S6 before and after irradiation are as follows. Figure 3As shown: from top to bottom, the images are: S1 before irradiation, S1 after irradiation, S2 before irradiation, S2 after irradiation, S3 before irradiation, S3 after irradiation, S4 before irradiation, S4 after irradiation, S5 before irradiation, S5 after irradiation, S6 before irradiation, and S6 after irradiation.

[0021] 1.3.1 Calculation of similarity of infrared fingerprint spectra of calcined mother-of-pearl Using OMNIC 6.0 software, and taking the average transmittance of common peaks in the infrared spectra of 12 samples (6 batches of calcined mother-of-pearl samples before and after irradiation) as a reference, the correlation coefficient and similarity (cosine of the included angle) of each sample were calculated. The analysis results are shown in Table 3. Table 3. Similarity analysis of infrared fingerprint spectra of calcined mother-of-pearl

[0022] The results above show that the similarity of the samples in each batch is in the range of 0.845 to 0.989. Therefore, the results indicate that there is basically no change in the types of components in the samples before and after irradiation. Irradiation has little effect on the overall chemical composition of calcined mother-of-pearl, and the overall consistency of different batches of calcined mother-of-pearl samples is good.

[0023] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A method for determining the main components of calcined mother-of-pearl before and after irradiation, characterized in that, Includes the following steps: (1) Preparation of test sample: Weigh the irradiated calcined mother-of-pearl, add potassium bromide, place it in an agate mortar, grind it evenly under an infrared lamp to obtain a mixed powder, transfer the mixed powder into a mold, transfer the mold to a tablet press, vacuum and pressurize to obtain the test sample; (2) Preparation of reference standard: Weigh the calcined mother-of-pearl before irradiation, add potassium bromide, place it in an agate mortar, grind it evenly under an infrared lamp to obtain a mixed powder, transfer the mixed powder into a mold, transfer the mold to a tablet press, vacuum and pressurize to obtain the reference standard; (3) The fingerprint spectra of the test sample and the reference sample were determined by infrared spectroscopy, and the changes in the fingerprint spectra were analyzed.

2. The method for determining the main components of calcined mother-of-pearl before and after irradiation according to claim 1, characterized in that: The irradiation dose in step (1) is 8 kGy.

3. The method for determining the main components of calcined mother-of-pearl before and after irradiation according to claim 1, characterized in that: In step (1), 1 mg of irradiated calcined mother-of-pearl was weighed and passed through a 200-mesh sieve; the ratio of potassium bromide added to the mass of irradiated calcined mother-of-pearl was 100:1, and the pressurization time was 1 min.

4. The method for determining the main components of calcined mother-of-pearl before and after irradiation according to claim 1, characterized in that: In step (2), 1 mg of calcined mother-of-pearl before irradiation is weighed and passed through a 200-mesh sieve; the mass ratio of potassium bromide added to calcined mother-of-pearl before irradiation is 100:1, and the pressurization time is 1 min.

5. The method for determining the main components of calcined mother-of-pearl before and after irradiation according to claim 1, characterized in that: In step (3), the infrared spectrometer has a measurement range of 4000–400 cm⁻¹. -1 .

6. A fingerprint spectrum of calcined mother-of-pearl obtained using the determination method according to any one of claims 1-5, characterized in that: The fingerprint spectrum contains 7 common peaks, and the wavelengths of each common peak are as follows: Peak 1: 708 cm -1 ; Peak No. 2: 876 cm -1 ; Peak No. 3: 1419 cm -1 ; Peak No. 4: 1792 cm -1 ; Peak No. 5: 2516 cm -1 ; Peak No. 6: 2865 cm -1 ; Peak No. 7: 2976cm -1 .

Images