Application of cyanamide waste residue carbon in lotus alkaloid extraction, solid-phase extraction adsorbent and application thereof

By using cyanamide waste slag as solid-phase extraction adsorbent, the problems of pigment interference and non-specific loss during the separation and purification of alkaloids in lotus were solved, and efficient extraction of 32 alkaloids were achieved and the extraction recovery was significantly improved.

CN119656653AActive Publication Date: 2025-03-21ZHEJIANG UNIV OF TECH
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Patent Information

Application Number
CN202510175631.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-02-18
Publication Date
2025-03-21
Estimated Expiration
2045-02-18

AI Technical Summary

Technical Problem

The prior art has limitations in isolating and purifying alkaloids in lotus, such as few extraction types, complex methods and high cost, especially nonspecific loss problems due to pigment interference.

Method used

Cyanamide waste slag charcoal is used as a solid-phase extraction adsorbent. Through its mesoporous structure, hydrophilicity and π-π interaction, it effectively adsorbs the pigments in the lotus extract, reduce interference to alkaloids, and enhance the adsorption and retention of alkaloids through hydrogen bonds and electrostatic forces.

Benefits of technology

The separation and purification of up to 32 alkaloids was achieved, which significantly improved the extraction recovery rate. Especially in the extraction of alkaloids such as 4-methyl-N-methylbacilline and N-trans-feruloyl tyramine, the extraction recovery rate was improved by 35% and 30% compared with the comparative example graphitized carbon black GCB method.

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Abstract

The invention belongs to the technical field of analytical chemistry, and particularly relates to application of cyanamide waste residue carbon in lotus alkaloid extraction, a solid-phase extraction adsorbent and application of the solid-phase extraction adsorbent. The cyanamide waste residue carbon solid-phase extraction method can realize separation and purification of 32 alkaloids in the lotus, and test results show that the extraction recovery rate of the 32 alkaloids in the lotus mixed extraction diluent reaches 83.09%-98.54%, so that an excellent balanced extraction effect is reflected, and the method is suitable for industrial production. The problems that the separation and purification types of alkaloid are few, the extraction method is complex and the extraction recovery rates of all components are uneven due to the influence of pigments in the plant lotus at present are effectively solved. Meanwhile, a new thought is provided for high value-added utilization of the cyanamide waste residue carbon.
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Description

Technical Field

[0001] The present application belongs to the technical field of analytical chemistry, and specifically relates to the application of cyanamide waste residue charcoal in the extraction of lotus alkaloids, and a solid phase extraction adsorbent containing the cyanamide waste residue charcoal. Background Art

[0002] Lotus (Nelumbo nucifera Gaertn.) is an aquatic herbaceous plant of the genus Nelumbo of the family Nelumbo. It contains a large number of alkaloids, flavonoids and other active substances, and is a natural plant resource with great development value. According to their structural characteristics, the alkaloids in lotus are mainly divided into monobenzylisoquinoline, dibenzylisoquinoline, aporphine and organic amide alkaloids, which have been found to have anti-inflammatory, anti-cancer, sedative and antioxidant effects. Lotus has a complex composition, and the pigment components in it will interfere with the separation and purification of alkaloids, so it is meaningful to use appropriate pretreatment methods to separate and purify the alkaloids in lotus.

[0003] Solid phase extraction (SPE) is an efficient separation, purification and enrichment method. Compared with traditional solvent extraction, SPE has the advantages of high extraction efficiency, low solvent usage and good selectivity. Adsorbent plays a vital role in the pretreatment process of SPE. The adsorbents reported for separation and purification of alkaloids in lotus are mainly mixed strong cation exchange materials and macroporous adsorption resin materials. The solid phase extraction method using mixed strong cation exchange materials as adsorbents can separate three aporphine alkaloids and one monobenzylisoquinoline alkaloid in lotus leaves, with a recovery rate of 97.7%-99.7%. This method has high extraction efficiency and short analysis time, but it is only for four alkaloids in lotus leaves, which has certain limitations. In addition, there is currently a method that first uses macroporous adsorption resins to preliminarily purify the lotus leaf / lotus seed core extract, and then uses mixed strong cation exchange materials as adsorbents to extract alkaloids. This method improves the purification efficiency, but the pretreatment process is cumbersome, and the cost is high due to the resin itself and the regeneration and maintenance of the resin. Summary of the invention

[0004] In order to solve the above technical problems, the present application proposes the application of cyanamide waste residue charcoal in the extraction of lotus alkaloids, which is specifically achieved through the following technical solutions: In the first aspect, the present application proposes the use of cyanamide waste residue charcoal in the extraction of lotus alkaloids.

[0005] Cyanamide waste residue carbon is an existing product. For its preparation method and parameter characterization, please refer to the paper (Liang Xiao. Application of cyanamide waste residue derived functional carbon materials in phenol-containing wastewater treatment [D]. Hangzhou: Zhejiang University of Technology, 2021). The hydrophilic nanographite carbon in the article is the cyanamide waste residue carbon in this application. Please refer to the relevant characterization of cyanamide waste residue carbon in the article. Cyanamide waste residue carbon is nitrogen-doped, and its nitrogen species mainly include pyridinic nitrogen, pyrrolic nitrogen and graphitic nitrogen; and there are oxygen-containing groups such as hydroxyl and carboxyl groups on its surface. Nitrogen doping and oxygen-containing functional groups give cyanamide waste residue carbon better hydrophilicity, which is manifested as a lower contact angle, so that the cyanamide waste residue carbon can fully contact with the lotus extract during the lotus alkaloid extraction process, and then effectively adsorb the pigments in the lotus extract. The cyanamide waste residue carbon has a graphitized lamellar structure, and the rich π electron system present therein can interact with the π electron system in the pigment molecules such as lutein and beta-carotene in the lotus extract, thereby effectively adsorbing the pigment and reducing its interference with the alkaloid separation and purification process. In addition, the high specific surface area possessed by the cyanamide waste residue carbon itself provides more adsorption sites, further enhancing its adsorption capacity for the pigment. In addition, the cyanamide waste residue carbon mentioned in the present application is a hydrophilic nanographitized carbon with a mesoporous structure, which has a larger specific surface area and pore volume than graphitized carbon black, reducing the nonspecific loss of alkaloids during the loading process.

[0006] Preferably, the alkaloids include nicotinamide, demethylcoclaurine-6-O-glucoside, N-methyl-O-demethylcoclaurine-7-O-glucoside, N-methylcoclaurine-7-O-glucoside, coclaurine-7-O-glucoside, isococlaurine-4-O-glucoside, N-methylcoclaurine-4-O-glucoside, glacivin, N-methylisococlaurine, coclaurine, N-methylcoclaurine, protococlaurine, metopramine, N-demethylcoclaurine, One or more of methylparaben, isoliensinine, pavone, methylneferine, O-demethylneferine, oxyneferine, 4-methyl-N-methylcoclaurine, liriodendrine, N-methoxypavone, liriodendrine, annonaine, N-demethylneferine, neferine, neferine, N-cis-feruloyltyramine, neferine-N-methanol, N-trans-feruloyltyramine, N-cis-cinnamoyltyramine, and N-trans-cinnamoyltyramine.

[0007] Preferably, the alkaloid comprises 4-methyl-N-methylcoclaurine and / or N-trans-feruloyltyramide.

[0008] Since cyanamide waste residue carbon is a hydrophilic nanographitized carbon with a mesoporous structure, it has a large specific surface area and pore volume. In addition, there are oxygen-containing groups such as hydroxyl and carboxyl on its surface. For alkaloids such as 4-methyl-N-methylcoclaurine and N-trans-feruloyltyramide that cannot be fully retained by the mixed strong cation exchange adsorbent during the sampling process, it can produce supplementary adsorption and retention through hydrogen bonding, electrostatic and other forces, thereby reducing the nonspecific loss of these alkaloids during the sampling process and significantly improving their extraction recovery rate.

[0009] Preferably, the extraction is solid phase extraction, and the solid phase extraction adopts a mixed strong cation exchange extraction column; cyanamide waste residue charcoal is arranged inside the extraction column; the cyanamide waste residue charcoal and the mixed strong cation exchange material are arranged in sequence in the loading direction of the extraction column.

[0010] In a second aspect, the present application provides a solid phase extraction adsorbent, which includes cyanamide waste residue charcoal and a mixed strong cation exchange material.

[0011] Preferably, the mass ratio of the cyanamide waste residue charcoal to the mixed strong cation exchange material is 1:(5-6).

[0012] In a third aspect, the present application proposes the use of the above-mentioned solid phase extraction adsorbent in the extraction of lotus alkaloids.

[0013] In a fourth aspect, the present application proposes the use of the above-mentioned solid phase extraction adsorbent in the identification of lotus-based products. The lotus-based products include products containing plant lotus ingredients such as lotus powder and lotus drinks. The identification includes identifying whether the lotus-based products contain any part of the lotus pod, lotus seed shell, lotus leaf, lotus flower, lotus seed core, lotus stamen, and lotus garment.

[0014] Compared with the prior art, this application has the following beneficial effects: The present application adopts the solid phase extraction method of cyanamide waste residue carbon to achieve the separation and purification of up to 32 alkaloids in lotus, and the test results of Example 1 show that the extraction recovery rate of 32 alkaloids in the lotus mixed extraction dilution reaches 83.09%-98.54%, reflecting an excellent balanced extraction effect, and effectively solving the current problems of few types of alkaloids, complex extraction methods, and uneven extraction recovery rates of various components caused by the influence of pigments in the plant lotus. Compared with the comparative example of graphitized carbon black GCB solid phase extraction method, the present application of cyanamide waste residue carbon has a better extraction recovery rate effect on 32 alkaloids, especially in the extraction of two alkaloids, 4-methyl-N-methylcoclaurine and N-trans-feruloyltyramine, the alkaloid extraction recovery rates of the present application are 35% and 30% higher than those of comparative example 1, respectively, reflecting unexpected technical effects. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 It is a solid phase extraction flow chart based on a combined solid phase extraction column; Figure 2 The effect of the amount of cyanamide waste residue carbon on the decolorization effect of the combined solid phase extraction column; Figure 3 The effect of PCX dosage on the extraction recovery of 32 alkaloids; Figure 4 The effect of sample loading on the extraction recovery of 32 alkaloids; Figure 5 The effect of elution solvent type on the extraction recovery of 32 alkaloids; Figure 6 The effect of the amount of ammonia added to methanol as the elution solvent on the extraction recovery of 32 alkaloids; Figure 7 The effect of elution solvent dosage on the extraction recovery of 32 alkaloids; Figure 8 The effect of different carbon materials on the color removal effect of combined solid phase extraction column; Fig. 9 The effect of the combined solid phase extraction column with different carbon materials on the extraction recovery of 32 alkaloids; Fig.10 This is a diagram showing the distribution of the main components of alkaloids in different parts of lotus. DETAILED DESCRIPTION

[0016] The present application will be further described below in the form of specific embodiments. Those of ordinary skill in the art will be able to implement the present application based on these descriptions. In addition, the embodiments of the present application involved in the following description are generally only embodiments of a part of the present application, rather than all embodiments. Therefore, based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without making creative work should fall within the scope of protection of the present application.

[0017] In the following examples, the sources of raw materials are as follows: the liquid chromatograph used is Waters' ACQUITYPREMIER UPLC, and the mass spectrometer is Waters' Xevo TQ-XS mass spectrometer. Reagents used: acetonitrile, chromatographically pure, Merck, Germany; ammonia, chromatographically pure, Aladdin Biochemical Technology Co., Ltd.; formic acid, chromatographically pure, Aladdin Biochemical Technology Co., Ltd.; ethanol, chromatographically pure, Sinopharm Chemical Reagent Co., Ltd.; ethyl lactate, analytically pure, Sinopharm Chemical Reagent Co., Ltd.; mechanical vacuum pressure dual-purpose pump, Millipore, USA; solid phase extraction device, Waters Technology Co., Ltd.; cyanamide waste residue, from Professor Li Ying's research group at Zhejiang University of Technology; graphitized carbon black GCB, Meizheng Detection Technology Co., Ltd.; mixed strong cation exchange material PCX, Tianjin Bona Aiger Technology Co., Ltd.

[0018] Example 1: Extraction of alkaloids from lotus plant This embodiment discloses a method for extracting alkaloids from lotus plants using cyanamide waste residue charcoal, which specifically comprises the following steps: S1. Preparation of lotus mixed extract diluent: Take lotus seed shell, lotus pod, lotus leaf, and lotus flower, freeze-dry and mechanically crush at -80°C, and then pass through a 100-mesh sieve to obtain lotus seed shell, lotus pod, lotus leaf, and lotus powder. Weigh 1g of lotus seed shell, lotus pod, lotus leaf, and lotus powder respectively in a 15ml centrifuge tube, add 10mL of ethyl lactate aqueous solution (ethyl lactate: water = 7:3, v / v) respectively for extraction, vortex for 1min, stand for 10min, ultrasonicate at 262W for 5min, centrifuge at 10000rpm at 4°C for 5min, take the supernatant, obtain lotus seed shell, lotus pod, lotus leaf, and lotus flower extract, and then mix these four extracts in a 50ml centrifuge tube to obtain a lotus mixed extract, which is diluted 20 times with ethanol / water solution (3:7, v / v) to obtain a lotus mixed extract diluent.

[0019] S2. Preparation of cyanamide waste residue carbon: Prepare 6.7 wt% HCl solution, add cyanamide waste residue and hydrochloric acid solution at a solid-liquid ratio of 1:10, react at room temperature for 0.5h, start stirring at 500 rpm, and filter under reduced pressure to obtain a crude product. Prepare 5wt% NaOH solution, add the crude product after pickling and sodium hydroxide solution at a solid-liquid ratio of 1:10, react in a 70℃ water bath for 1h, start stirring at 500 rpm, and filter under reduced pressure to obtain the material. Bake in an oven at 110℃ to constant weight to obtain cyanamide waste residue carbon, in which the C content is relatively high, which can reach more than 99%. The obtained carbon material has the advantages of good hydrophilicity, high specific surface area, acid and alkali resistance, and rich surface oxygen functional groups.

[0020] S3. Assembly of extraction column: Assemble 20 μm sieve plate, 15 mg cyanamide waste residue carbon, 10 μm sieve plate, 80 mg mixed strong cation exchange material PCX, and 20 μm sieve plate into a 6 ml empty column tube from top to bottom, and install the assembled extraction column on the solid phase extraction device, as shown in the attached Figure 1 As shown in the flow chart, the solid phase extraction steps are as follows: a) Initialization: Wash the balanced extraction column with 1 ml of ethanol solution and 1 ml of 0.1% formic acid aqueous solution in turn. b) Loading: Load 3 ml of lotus mixed extraction dilution at a flow rate of 3 ml / min. c) Elution: Elute with 1.5 ml of 5% ammonia methanol at a flow rate of 3 ml / min and collect the eluate. Of course, it can be understood that in other embodiments, the mass ratio between the cyanamide waste residue carbon and the mixed strong cation exchange material PCX can also be 1: (5-6).

[0021] S4. The collected eluate and the lotus mixed extract dilution that had not been treated by column were diluted 20 times with acetonitrile / water solution (1:9, v / v), centrifuged and then subjected to liquid chromatography-mass spectrometry detection. The UPLC detection conditions were as follows: mobile phase: phase A was acetonitrile, phase B was 0.1% formic acid water; elution gradient: 0-0.5 min, 94% B; 0.5-4 min, 94-90% B; 4-8 min, 90% B; 8-13 min, 90-85% B; 13-20 min, 85-40% B; 20.1-23 min, 5% B; 23.1-28 min, 94% B. The flow rate was 0.3 ml / min; the chromatographic column used was Waters ACQUITY Premier HSS T3 column (2.1×100 mm, 1.8 μm); the injection was 2 μl; the MS conditions were: capillary voltage (+ESI): 2.0 kV, cone voltage: 30 V, desolvation gas temperature: 450°C, desolvation gas flow rate: 1000 L / h, cone gas flow rate: 50 L / h, nebulizer gas: 7 Bar. The extraction recovery of alkaloids was calculated based on the peak area detected, and the extraction recovery of 32 alkaloids in the lotus mixed extract dilution reached 83.09%-98.54%.

[0022] S5. Prepare mixed standard solutions of different concentrations, analyze them by UPLC-QQQ-MS / MS, obtain a linear regression equation, and measure 32 alkaloids in different parts of lotus and commercial beverage samples. Measure the peak area of ​​the analyte, substitute it into the linear equation, and calculate the content of the analyte in the sample; the name of the standard substance, linear regression equation and linear range in the mixed standard solution are shown in the following table: Table 1. Standard curves of six alkaloid standards Quantitative methods for 32 alkaloids: Among them, pavlova, linderpine, N-demethylnucleine, linderpine, nicotinamide, and neferine were quantified by external standard method. The content of monobenzylisoquinoline alkaloids is expressed as linderpine equivalent (μg linderpine / g), the content of bisbenzylisoquinoline alkaloids is expressed as neferine equivalent (μg neferine / g), the content of aporphine alkaloids is expressed as pavlova equivalent (μg pavlova / g), and the content of organic amide alkaloids is expressed as nicotinamide equivalent (μg nicotinamide / g). Please refer to the extraction recovery of the 32 alkaloids obtained. Figure 7 .

[0023] Example 2: Effect of adsorbent on alkaloid extraction recovery Based on Example 1, this example tests the effect of adsorbent dosage on alkaloid extraction recovery. Specifically, weigh 0-20 mg of cyanamide waste charcoal and 50-120 mg of mixed strong cation exchange material PCX on weighing paper, assemble the extraction column and install it on the solid phase extraction device. The solid phase extraction steps are as follows: a) Initialization: wash the equilibrium extraction column with 1 ml of ethanol solution and 1 ml of 0.1% formic acid aqueous solution in turn; b) Loading: load 3 ml of lotus mixed extraction dilution at a flow rate of 3 ml / min; c) Elution: elute with 3 ml of 3% ammonia methanol at a flow rate of 3 ml / min and collect the eluate. According to the attached Figure 2 , 3 The results showed that the best alkaloid extraction recovery was achieved when 15 mg of cyanamide waste residue charcoal and 80 mg of mixed strong cation exchange material PCX were used as the final adsorbent dosage.

[0024] Example 3: Effect of sample loading on alkaloid extraction recovery Based on Example 2, this example tests the effect of sample loading on the alkaloid extraction recovery rate. Specifically, 15 mg of cyanamide waste charcoal and 80 mg of mixed strong cation exchange material PCX were weighed on weighing paper, and the extraction column was assembled and installed on the solid phase extraction device. The solid phase extraction steps are as follows: a) Initialization: Wash the equilibrium extraction column with 1 ml of ethanol solution and 1 ml of 0.1% formic acid aqueous solution in turn. b) Loading: Load 1-5 ml of lotus mixed extraction dilution at a flow rate of 3 ml / min. c) Elution: Elute with 3 ml of 3% ammonia methanol at a flow rate of 3 ml / min and collect the eluate. According to the attached Figure 4 The results showed that the extraction recovery rate of 32 alkaloids was optimal when the loading volume of the mixed extract dilution of lotus was 3 ml.

[0025] Example 4: Effect of elution conditions on alkaloid extraction recovery Based on Example 3, this example tests the effect of the type of eluent on the alkaloid extraction recovery rate. Specifically, weigh 15 mg of cyanamide waste charcoal and 80 mg of mixed strong cation exchange material PCX on weighing paper, assemble the extraction column and install it on the solid phase extraction device. The solid phase extraction steps are as follows: a) Initialization: Wash the equilibrium extraction column with 1 ml of ethanol solution and 1 ml of 0.1% formic acid aqueous solution in turn. b) Loading: Load 3 ml of lotus mixed extraction dilution at a flow rate of 3 ml / min. c) Elution: Elute with 3 ml of 3% ammonia methanol / acetonitrile / ethanol at a flow rate of 3 ml / min and collect the eluate. According to the attached Figure 5 The results showed that the extraction recovery rate was optimal when methanol was selected as the elution solvent.

[0026] Furthermore, methanol was selected as the elution solvent, and the elution solvent was adjusted to 1-15% ammonia methanol to test the effect of different ammonia addition amounts in methanol on the alkaloid extraction recovery rate. Figure 6 The results showed that when 1%-3% ammonia in methanol was added, some alkaloids were still in an ionized state and would be adsorbed and retained. When the ammonia ratio continued to be added to 5%, the extraction recovery rate of 32 alkaloids was optimal.

[0027] Furthermore, based on the selection of methanol with 5% ammonia as the elution solvent, the effect of the amount of elution solvent on the alkaloid extraction recovery rate was tested by adjusting the amount of elution solvent to 1-3 ml of 5% ammonia methanol. Figure 7 The results showed that the extraction recovery rate was optimal when 1.5 ml of methanol with 5% ammonia was selected as the final elution solvent.

[0028] Example 5: Feasibility test of identification of lotus matrix alkaloids In order to verify the feasibility and effectiveness of the solid phase extraction method for screening 32 alkaloids in the lotus matrix, in this example, four alkaloid standards of three different concentrations (10 ng / ml, 100 ng / ml, 500 ng / ml) were added to the lotus mixed extract dilution sample, and the lotus mixed extract dilution added with the standard was treated by the solid phase extraction method of the present invention and then subjected to UPLC-QQQ-MS / MS analysis. The recovery rate was calculated according to the recovery rate = (spiked sample concentration - unspiked sample concentration) / spiked concentration × 100%.

[0029] S1. Prepare three different concentrations of four alkaloid standard mixed solutions, namely, monobenzylisoquinoline alkaloids: linaline (10ng / ml, 100ng / ml, 500ng / ml), bisbenzylisoquinoline alkaloids: neferine (10ng / ml, 100ng / ml, 500ng / ml), aporphine alkaloids: pavloline (10ng / ml, 100ng / ml, 500ng / ml), organic amide alkaloids: nicotinamide (10ng / ml, 100ng / ml, 500ng / ml).

[0030] S2. Prepare four 3 ml samples of lotus mixed extract dilution solution, and add standard mixed solutions with concentrations of 10 ng / ml, 100 ng / ml, and 500 ng / ml to three of them, respectively.

[0031] S3. After applying the solid phase extraction of the present invention to the four samples of the lotus mixed extract dilution, the collected eluate was diluted 20 times with acetonitrile / water solution (1:9, v / v), centrifuged and subjected to liquid chromatography tandem mass spectrometry analysis, and each sample was measured twice. The recovery rate was calculated at three spiked concentrations. The detailed recovery rate results are shown in Table 2.

[0032] Table 2. Recovery of solid phase extraction method in lotus matrix From the results in Table 2, it can be seen that at three spiked concentrations, the recoveries of the four alkaloids ranged from 82.29% to 110.38%, indicating that the solid phase extraction method described in the present invention can be used for screening analysis of alkaloids in lotus products.

[0033] Example 6: Lotus-based product identification test Based on Example 5, this example proposes a method for identifying the source of lotus ingredients in lotus-based products, specifically, comprising the following steps: S1. The seven parts of lotus (lotus pod, lotus seed shell, lotus leaf, lotus flower, lotus seed core, lotus stamen, and lotus garment) from three different batches stored in a -80°C refrigerator were mechanically crushed and then passed through a 100-mesh sieve to obtain three batches of sample powders of seven parts of lotus. 1 g of lotus pod, lotus seed shell, lotus leaf, lotus flower, lotus seed core, lotus stamen, and lotus garment powder were weighed respectively, and 10 mL of ethyl lactate aqueous solution (ethyl lactate: water = 7:3, v / v) was added to extract, vortexed for 1 min, allowed to stand for 10 min, ultrasonicated at 262 W for 5 min, centrifuged at 10000 rpm at 4°C for 5 min, and the supernatant was taken to obtain extracts of seven parts of lotus from three batches. The obtained extracts were diluted 20 times with ethanol / water solution (3:7, v / v) to obtain lotus part extract dilutions.

[0034] S2. The diluted extracts of the lotus parts were treated with the solid phase extraction method of the present invention respectively, and the collected eluents were diluted 20 times with acetonitrile / water solution (1:9, v / v). After centrifugation, liquid chromatography tandem mass spectrometry analysis was performed according to the mobile phase and analysis conditions described in the scheme of the present invention.

[0035] S3. The contents of 32 alkaloids in seven parts of lotus of three batches were calculated respectively according to the constructed standard curve, and the determination method was the same as that in Example 1.

[0036] S4. Principal component analysis (PCA) was used to perform differential analysis on seven parts of three batches of lotus. Fig.10 .observe Fig.10 It can be seen that the two main components of nuciferine and pavarine can be used to distinguish the seven parts of lotus, among which the contribution rate of the main component one nuciferine is 48.8%, and the contribution rate of the main component two pavarine is 22.8%. Therefore, in the process of identifying the source parts of lotus components in lotus-based products, the alkaloid extraction method of the present application can be used to obtain the content of the two main components of nuciferine and pavarine, and finally combined with the measured content and Fig.10 Identify the source of lotus ingredients.

[0037] Comparative Example 1: Solid Phase Extraction Using Graphitized Carbon Black GCB The difference between the lotus alkaloid extraction method in this comparative example and that in Example 1 is that graphitized carbon black GCB is used instead of cyanamide waste residue carbon. Figure 8 , 9 The results show that the decolorization effect of cyanamide waste residue carbon and the extraction recovery rate of 32 alkaloids are significantly better than those of graphitized carbon black GCB. In particular, in the extraction of 4-methyl-N-methylcoclaurine, the extraction recovery rate obtained by the solid phase extraction method using graphitized carbon black GCB as one of the adsorbents is only 54%, while when the cyanamide waste residue carbon of the present application is used, the extraction recovery rate is as high as 89%, an increase of 35%; in the extraction of N-trans-feruloyltyramine alkaloids, the extraction recovery rate obtained by the solid phase extraction method using graphitized carbon black GCB as one of the adsorbents is only 58%, while when the cyanamide waste residue carbon of the present application is used, the extraction recovery rate is as high as 88%, an increase of 30%, reflecting unexpected technical effects.

Claims

1. Application of cyanamide waste residue charcoal in the extraction of lotus alkaloids.

2. The use according to claim 1, characterized in that: The alkaloids include nicotinamide, demethylcoclaurine-6-O-glucoside, N-methyl-O-demethylcoclaurine-7-O-glucoside, N-methylcoclaurine-7-O-glucoside, coclaurine-7-O-glucoside, isococlaurine-4-O-glucoside, N-methylcoclaurine-4-O-glucoside, glacivin, N-methylisococlaurine, coclaurine, N-methylcoclaurine, protococlaurine, metopramine, N-demethyl One or more of papaverine, isoliensinine, pavone, methyl neferine, O-demethylneferine, oxyneferine, 4-methyl-N-methylcoclaurine, liriodendrine, N-methoxypavone, liriodendrine, annonaine, N-demethylneferine, neferine, neferine, N-cis-feruloyltyramine, neferine-N-methanol, N-trans-feruloyltyramine, N-cis-cinnamoyltyramine, and N-trans-cinnamoyltyramine.

3. The use according to claim 2, characterized in that: The alkaloids include 4-methyl-N-methylcoclaurine and / or N-trans-feruloyltyramide.

4. The use according to claim 1, characterized in that: The extraction is solid phase extraction, and the solid phase extraction adopts a mixed strong cation exchange extraction column; cyanamide waste residue charcoal is arranged inside the extraction column; the cyanamide waste residue charcoal and the mixed strong cation exchange material are arranged in sequence in the loading direction of the extraction column.

5. A solid phase extraction adsorbent, characterized in that: The solid phase extraction adsorbent comprises cyanamide waste residue carbon and mixed strong cation exchange material.

6. A solid phase extraction adsorbent according to claim 5, characterized in that: The mass ratio of the cyanamide waste residue charcoal to the mixed strong cation exchange material is 1:(5-6).

7. Use of the solid phase extraction adsorbent according to claim 6 in the extraction of lotus alkaloids.

8. Use of the solid phase extraction adsorbent according to claim 5 or 6 in the identification of lotus-based products.

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