Application of cyanamide waste residue carbon in extraction of lotus alkaloids, a solid-phase extraction adsorbent and its application

Abstract

This application belongs to the technical field of analytical chemistry, and specifically relates to the application of cyanamide waste residue carbon in the extraction of lotus alkaloids, a solid-phase extraction adsorbent and its application. The solid-phase extraction method using cyanamide waste residue carbon in this application can achieve the separation and purification of up to 32 alkaloids in lotus. Moreover, the test results show that the extraction recovery rates of 32 alkaloids in the diluted lotus mixed extract reach 83.09% - 98.54%, reflecting excellent balanced extraction effects, effectively solving the problems of few types of separation and purification of alkaloids caused by the influence of pigments in the plant lotus, complex extraction methods, and uneven extraction recovery rates of various components. At the same time, it also provides a new idea for the high-value utilization of cyanamide waste residue carbon.

Description

Technical Field

[0001] This application belongs to the technical field of analytical chemistry, and specifically relates to the application of cyanamide waste residue carbon in the extraction of lotus alkaloids, as well as a solid-phase extraction adsorbent containing cyanamide waste residue carbon. Background Art

[0002] Lotus (Nelumbo nucifera Gaertn.) is an aquatic herbaceous plant of the genus Nelumbo in the family Nelumbonaceae. Lotus contains a large number of active substances such as alkaloids and flavonoids, and is a natural plant resource with great development value. Lotus alkaloids are mainly divided into monobenzylisoquinoline, bisbenzylisoquinoline, aporphine, and organic amide alkaloids according to their structural characteristics, and have been found to have anti-inflammatory, anti-cancer, sedative, antioxidant and other effects. The composition of lotus is complex, and its pigment components will interfere with the separation and purification of alkaloids. Therefore, a suitable pretreatment method for separating and purifying lotus alkaloids is meaningful.

[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, less solvent consumption and good selectivity. Adsorbents play a crucial role in the SPE pretreatment process. The reported adsorbents for separating and purifying lotus alkaloids are mainly mixed strong cation exchange materials and macroporous adsorption resin materials. The solid-phase extraction method using a mixed strong cation exchange material as an adsorbent can separate 3 aporphine alkaloids and 1 monobenzylisoquinoline alkaloid in lotus leaves, and its recovery rate is 97.7%-99.7%. This method has high extraction efficiency and short analysis time, but it only targets 4 alkaloids in lotus leaves and has certain limitations. In addition, there is currently a method of first preliminarily purifying the lotus leaf / lotus core extract with macroporous adsorption resin, and then using a mixed strong cation exchange material as an adsorbent to extract alkaloids. This method improves the purification efficiency, but the pretreatment process is more cumbersome, and the cost is high due to the resin itself and the reasons for resin regeneration and maintenance. Summary of the Invention

[0004] To solve the above technical problems, this application proposes the application of cyanamide waste residue carbon in the extraction of lotus alkaloids, which is specifically realized through the following technical solutions:

[0005] In the first aspect, this application proposes the application of cyanamide waste residue carbon in the extraction of lotus alkaloids.

[0006] Cyanamide waste residue carbon is an existing product. For its preparation method and parameter characterization, please refer to the article "Application of Cyanamide Waste Residue Derived Functional Carbon Materials in the Treatment of Phenol-Containing Wastewater". The hydrophilic nano-graphite 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 has nitrogen doping, and its nitrogen species mainly include pyridine nitrogen, pyrrole nitrogen and graphitic nitrogen; and there are also oxygen-containing groups such as hydroxyl groups and carboxyl groups on its surface. Nitrogen doping and oxygen-containing functional groups endow cyanamide waste residue carbon with better hydrophilicity, manifested as a lower contact angle, enabling cyanamide waste residue carbon to fully contact with the lotus extract during the extraction process of lotus alkaloids, and then effectively adsorb the pigments in the lotus extract. Cyanamide waste residue carbon has a graphitized lamellar structure, and its existing rich π-electron system can undergo π-π interaction with the π-electron system in pigment molecules such as lutein and β-carotene in the lotus extract, thereby effectively adsorbing pigments and reducing their interference in the separation and purification process of alkaloids. In addition, the high specific surface area of cyanamide waste residue carbon itself provides more adsorption sites, further enhancing its adsorption capacity for pigments. In addition, the cyanamide waste residue carbon mentioned in this application is a hydrophilic nano-graphitized carbon with a mesoporous structure. Compared with graphitized carbon black, it has a larger specific surface area and pore volume, reducing the non-specific loss of alkaloids during the sample loading process.

[0007] Preferably, the alkaloid includes one or more of 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-methylisococlaurine-4-O-glucoside, graziovine, N-methylisococlaurine, coclaurine, N-methylcoclaurine, protolimonine, armepavine, N-demethylarmepavine, isoliensinine, asimilobine, methyl liensinine, O-demethyllimonine, noroxyhydrastinine, 4-methyl-N-methylcoclaurine, liriodenine, N-methoxyasimilicin, tulipinolidine, anonaine, N-demethyllimonine, liensinine, noroxyhydrastinine, N-cis-feruloyltyramine, noroxyhydrastinine-N-methanol, N-trans-feruloyltyramine, N-cis-cinnamoyltyramine, N-trans-cinnamoyltyramine.

[0008] Preferably, the alkaloid includes 4-methyl-N-methylcoclaurine and / or N-trans-feruloyltyramine.

[0009] Since the cyanamide waste residue carbon is a hydrophilic nano-graphitized carbon with a mesoporous structure, having a large specific surface area and pore volume, and in addition, there are oxygen-containing groups such as hydroxyl groups and carboxyl groups on its surface, alkaloids such as 4-methyl-N-methylcoclaurine and N-trans-feruloyltyramine that cannot be fully retained by the mixed strong cation exchange adsorbent during the sample loading process can be supplemented and retained through hydrogen bonding, electrostatic and other forces, thereby reducing the non-specific loss of these alkaloids during the sample loading process and significantly improving their extraction recovery rate.

[0010] Preferably, the extraction is solid-phase extraction, and the solid-phase extraction uses a mixed strong cation exchange extraction column; the extraction column is internally provided with cyanamide waste residue carbon; the cyanamide waste residue carbon and the mixed strong cation exchange material are arranged in sequence in the sample loading direction in the extraction column.

[0011] In a second aspect, the present application provides a solid-phase extraction adsorbent, which includes cyanamide waste residue carbon and a mixed strong cation exchange material.

[0012] Preferably, the mass ratio of the cyanamide waste residue carbon to the mixed strong cation exchange material is 1:(5 - 6).

[0013] In a third aspect, the present application proposes the application of the above solid-phase extraction adsorbent in the extraction of lotus alkaloids.

[0014] In a fourth aspect, the present application proposes the application of the above solid-phase extraction adsorbent in the identification of lotus-based products. The lotus-based products include products containing plant lotus components such as lotus powder and lotus-based beverages. The identification includes identifying whether any part of lotus receptacle, lotus seed shell, lotus leaf, lotus flower, lotus seed core, lotus stigma, and lotus seed coat is contained in the lotus-based product.

[0015] Compared with the prior art, the present application has the following beneficial effects:

[0016] The solid-phase extraction method using cyanamide waste residue carbon in the present application can achieve the separation and purification of up to 32 alkaloids in lotus. Moreover, the test results of Example 1 show that the extraction recovery rates of 32 alkaloids in the diluted lotus mixed extract reach 83.09% - 98.54%, reflecting an excellent balanced extraction effect, effectively solving the problems of few types of separation and purification of alkaloids caused by the influence of pigments in plant lotus at present, complex extraction methods, and uneven extraction recovery rates of each component. Compared with the graphite carbon black GCB solid-phase extraction method of the comparative example, the cyanamide waste residue carbon in the present application 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 extraction recovery rates of the alkaloids in the present application are 35% and 30% higher than those of the comparative example 1 respectively, showing an unexpected technical effect. Description of the Drawings

[0017] Figure 1 It is a solid-phase extraction flow chart based on a combined solid-phase extraction column;

[0018] Figure 2 It is the influence of the amount of cyanamide waste residue carbon on the color removal effect of the combined solid-phase extraction column;

[0019] Figure 3 It is the influence of the amount of PCX on the extraction recovery rate of 32 alkaloids;

[0020] Figure 4 It is the influence of the sample loading amount on the extraction recovery rate of 32 alkaloids;

[0021] Figure 5 It is the influence of the type of elution solvent on the extraction recovery rate of 32 alkaloids;

[0022] Figure 6 It is the influence of the addition amount of ammonia water in methanol of the elution solvent on the extraction recovery rate of 32 alkaloids;

[0023] Figure 7 It is the influence of the amount of elution solvent on the extraction recovery rate of 32 alkaloids;

[0024] Figure 8 It is the influence of different carbon materials on the color removal effect of the combined solid-phase extraction column;

[0025] Figure 9 It is the influence of the combined solid-phase extraction column with different carbon materials on the extraction recovery rate of 32 alkaloids;

[0026] Figure 10 It is a diagram showing the distribution of the main components of alkaloids in different parts of lotus. Specific embodiments

[0027] The present application will be further described below by way 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 usually only a part of the embodiments of the present application, rather than all of the embodiments. Therefore, all other embodiments obtained by those of ordinary skill in the art without creative efforts based on the embodiments in the present application should fall within the scope of protection of the present application.

[0028] 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.

[0029] Example 1: Extraction of alkaloids from lotus plant

[0030] This embodiment discloses a method for extracting alkaloids from lotus plants using cyanamide waste residue charcoal, which specifically comprises the following steps:

[0031] S1. Preparation of lotus mixed extract diluent: Take lotus seed shell, lotus pod, lotus leaf, lotus flower and freeze-dry and mechanically crush at -80°C, 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 in a 15ml centrifuge tube, add 10mL of ethyl lactate aqueous solution (ethyl lactate: water = 7:3, v / v) to extract, vortex for 1min, stand for 10min, ultrasonicate at 262W for 5min, centrifuge at 10000rpm for 5min at 4°C, take the supernatant, obtain lotus seed shell, lotus pod, lotus leaf, and lotus extract, and then mix these four extracts in a 50ml centrifuge tube to obtain a lotus mixed extract, which is diluted 20 times with an ethanol / water solution (3:7, v / v) to obtain a lotus mixed extract diluent.

[0032] S2, preparation of cyanamide waste residue carbon: prepare 6.7wt% HCl solution, add cyanamide waste residue and hydrochloric acid solution according to the solid-liquid ratio of 1:10, react at room temperature for 0.5h, start stirring at a speed of 500rpm, and filter under reduced pressure to obtain a crude product. Prepare 5wt% NaOH solution, add the crude product after pickling and sodium hydroxide solution according to the solid-liquid ratio of 1:10, react in a 70℃ water bath for 1h, start stirring at a speed of 500rpm, 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.

[0033] S3. Assembly of the extraction column: A 20-μm sieve plate, 15 mg of cyanamide waste residue carbon, a 10-μm sieve plate, 80 mg of the mixed strong cation exchange material PCX, and a 20-μm sieve plate are assembled into an empty column tube with a 6-ml specification from top to bottom in sequence. The assembled extraction column is installed on the solid-phase extraction device. As shown in the attached Figure 1 flow chart, the solid-phase extraction steps are as follows: a) Initialization: The extraction column is washed and balanced with 1 ml of ethanol solution and 1 ml of 0.1% formic acid aqueous solution in sequence. b) Sample loading: 3 ml of the mixed extract dilution of lotus is loaded at a flow rate of 3 ml / min. c) Elution: 1.5 ml of 5% ammonia methanol is used for elution at a flow rate of 3 ml / min, and the eluate is collected. 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).

[0034] S4. The above-mentioned collected eluate and the mixed extract dilution of lotus that has not been processed through the column are uniformly diluted 20 times with an acetonitrile / water solution (1:9, v / v), centrifuged, and then subjected to liquid chromatography-mass spectrometry detection. The UPLC detection conditions are as follows: Mobile phase: Phase A is acetonitrile, and phase B is 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 is 0.3 ml / min; The chromatographic column used is the Waters company ACQUITY Premier HSS T3 column (2.1×100 mm, 1.8 μm); The injection volume is 2 μl; The MS conditions are: 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, Nebulizing gas: 7 Bar. The extraction recovery rate of alkaloids is calculated according to the detected peak area, and the extraction recovery rate of 32 alkaloids in the mixed extract dilution of lotus reaches 83.09% - 98.54%.

[0035] S5. Mixed standard solutions with different concentrations are prepared and analyzed by UPLC-QQQ-MS / MS to obtain the linear regression equation. The 32 alkaloids in different parts of lotus and commercial beverage samples are determined. The peak area of the analyte is measured and substituted into the linear equation to calculate the content of the analyte in the sample; The names of the standards, linear regression equations, and linear ranges in the mixed standard solution are shown in the following table:

[0036] Table 1. Standard curves of 6 alkaloid standards

[0037]

[0038] Description of the quantitative methods for 32 alkaloids: Among them, asimilobine, lindera alkaloid, N - demethylnuciferine, nuciferine, nicotinamide, and liensinine are quantified by the external standard method. The content of monobenzylisoquinoline alkaloids is expressed in terms of the equivalent of lindera alkaloid (μg lindera alkaloid / g), the content of bisbenzylisoquinoline alkaloids is expressed in terms of the equivalent of liensinine (μg liensinine / g), the content of aporphine alkaloids is expressed in terms of the equivalent of asimilobine (μg asimilobine / g), and the content of organic amide alkaloids is expressed in terms of the equivalent of nicotinamide (μg nicotinamide / g). For the extraction and recovery of the 32 alkaloids obtained, please refer to Figure 7 。

[0039] Example 2: Influence of adsorbents on the extraction recovery rate of alkaloids

[0040] Based on Example 1, in this example, the influence of the adsorbent dosage on the extraction recovery rate of alkaloids was detected. Specifically, 0 - 20 mg of cyanamide waste residue carbon and 50 - 120 mg of the 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: The extraction column was washed and balanced successively with 1 ml of ethanol solution and 1 ml of 0.1% formic acid aqueous solution; b) Sample loading: 3 ml of the diluted mixed extract of lotus was loaded at a flow rate of 3 ml / min; c) Elution: 3 ml of 3% ammonia - methanol was used for elution at a flow rate of 3 ml / min, and the eluate was collected. According to the attached Figure 2 、 3 The results show that when 15 mg of cyanamide waste residue carbon and 80 mg of the mixed strong cation exchange material PCX are selected as the final adsorbent dosage, the extraction and recovery of alkaloids are the best.

[0041] Example 3: Influence of the sample loading amount on the extraction recovery rate of alkaloids

[0042] Based on Example 2, in this example, the influence of the sample loading amount on the extraction recovery rate of alkaloids was detected. Specifically, 15 mg of cyanamide waste residue carbon and 80 mg of the 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: The extraction column was washed and balanced successively with 1 ml of ethanol solution and 1 ml of 0.1% formic acid aqueous solution. b) Sample loading: 1 - 5 ml of the diluted mixed extract of lotus was loaded at a flow rate of 3 ml / min. c) Elution: 3 ml of 3% ammonia - methanol was used for elution at a flow rate of 3 ml / min, and the eluate was collected. According to the attached Figure 4 The results show that when the sample loading volume of the diluted mixed extract of lotus is 3 ml, the extraction recovery rates of 32 alkaloids are optimal.

[0043] Example 4: Influence of elution conditions on the extraction recovery rate of alkaloids

[0044] On the basis of Example 3, this example detects the influence of the type of eluent on the extraction recovery rate of alkaloids. Specifically, weigh 15 mg of cyanamide waste residue carbon and 80 mg of mixed strong cation exchange material PCX on a 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 and balance the extraction column with 1 ml of ethanol solution and 1 ml of 0.1% formic acid aqueous solution in sequence. b) Loading: Load 3 ml of the mixed extract dilution of lotus 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 appendix Figure 5 The results show that the extraction recovery rate is optimal when the elution solvent type is methanol.

[0045] Furthermore, select methanol as the elution solvent, adjust the elution solvent to 1-15% ammonia methanol, and test the influence of different ammonia addition amounts in methanol on the extraction recovery rate of alkaloids. According to the appendix Figure 6 The results show that when methanol with 1%-3% ammonia is added, some alkaloids are still in the ionized state and will still be adsorbed and retained. When the ammonia ratio is continuously increased to 5%, the extraction recovery rate of 32 alkaloids is optimal.

[0046] Still further, on the basis of selecting methanol with 5% ammonia as the elution solvent, elute by adjusting the elution solvent amount to 1-3 ml of 5% ammonia methanol, and test the influence of the elution solvent amount on the extraction recovery rate of alkaloids. According to the appendix Figure 7 The results show that the extraction recovery rate is optimal when 1.5 ml of methanol with 5% ammonia is selected as the final elution solvent.

[0047] Example 5: Feasibility test for the identification of alkaloids in lotus matrix

[0048] 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 with three different concentrations (10 ng / ml, 100 ng / ml, 500 ng / ml) are added to the mixed extract dilution sample of lotus. After treating the mixed extract dilution of lotus added with the standards by the solid-phase extraction method of the present invention, UPLC-QQQ-MS / MS analysis is carried out. Calculate the recovery rate according to the formula: recovery rate = (spiked sample concentration - unspiked sample concentration) / spiked concentration × 100%.

[0049] S1. Prepare standard mixed solutions of 4 alkaloids at three different concentrations, namely, monobenzylisoquinoline alkaloids: corydine (10 ng / ml, 100 ng / ml, 500 ng / ml), bisbenzylisoquinoline alkaloids: liensinine methyl ester (10 ng / ml, 100 ng / ml, 500 ng / ml), aporphine alkaloids: asimilobine (10 ng / ml, 100 ng / ml, 500 ng / ml), and organic amide alkaloids: nicotinamide (10 ng / ml, 100 ng / ml, 500 ng / ml).

[0050] S2. Prepare four 3-ml lotus mixed extraction and dilution liquid samples, and add standard mixed solutions at concentrations of 10 ng / ml, 100 ng / ml, and 500 ng / ml to three of them respectively.

[0051] S3. After subjecting the above four lotus mixed extraction and dilution liquid samples to solid-phase extraction using the present invention, dilute the collected eluate 20 times with an acetonitrile / water solution (1:9, v / v), perform liquid chromatography-tandem mass spectrometry analysis after centrifugation, and measure each sample twice. Calculate the recovery rates at three spiked concentrations. The detailed recovery rate results are shown in Table 2.

[0052] Table 2. Recovery rates of the solid-phase extraction method in lotus matrix

[0053]

[0054]

[0055] As can be seen from the results in Table 2: at three spiked concentrations, the recovery rates of these 4 alkaloids range from 82.29% to 110.38%, indicating that the solid-phase extraction method described in the present invention can be used for the screening and analysis of alkaloids in lotus products.

[0056] Example 6: Identification test of lotus-based products

[0057] Based on Example 5, this example proposes a method for identifying the source parts of lotus components in lotus-based products. Specifically, it includes the following steps:

[0058] S1. Mechanically pulverize seven parts of lotus (lotus receptacle, lotus seed shell, lotus leaf, lotus flower, lotus plumule, lotus stigma, lotus seed coat) from three different batches stored in an -80°C refrigerator, and then pass through a 100-mesh sieve to obtain powder samples of seven parts of lotus from three batches. Weigh 1 g of powder of lotus receptacle, lotus seed shell, lotus leaf, lotus flower, lotus plumule, lotus stigma, and lotus seed coat respectively, add 10 mL of an aqueous solution of ethyl lactate (ethyl lactate: water = 7:3, v / v) for extraction, vortex for 1 min, let stand for 10 min, ultrasonicate at 262 W for 5 min, centrifuge at 10,000 rpm for 5 min at 4°C, take the supernatant to obtain the extraction solutions of seven parts of lotus from three batches, and dilute the obtained extraction solutions 20 times with an ethanol / water solution (3:7, v / v) to obtain diluted extraction solutions of lotus parts.

[0059] S2. Treat the diluted extraction solutions of lotus parts using the solid-phase extraction method of the present invention respectively, and dilute the collected eluate 20 times with an acetonitrile / water solution (1:9, v / v), and perform liquid chromatography-tandem mass spectrometry analysis according to the mobile phase and analysis conditions described in the scheme of the present invention after centrifugation.

[0060] S3. Calculate the contents of 32 alkaloids in seven parts of lotus from three batches respectively according to the constructed standard curve, and the determination method is the same as that in Example 1.

[0061] S4. Perform differential analysis on seven parts of lotus from three batches using principal component analysis (PCA) to obtain Figure 10 . Observe Figure 10 It can be seen that seven parts of lotus can be distinguished by using two principal components, PC1 and PC2, among which the contribution rate of the first principal component is 48.8% and the contribution rate of the second principal component is 22.8%. Therefore, in the process of identifying the source parts of lotus components in lotus-based products, the extraction method of alkaloids of the present application can be adopted, combined with ultra-high performance liquid chromatography-tandem mass spectrometry to determine the content distribution of 32 alkaloids in lotus-based products, and then confirm the source parts of lotus components through chemometric principal component analysis.

[0062] Comparative Example 1: Use graphitized carbon black GCB for solid-phase extraction

[0063] The difference between the lotus alkaloid extraction method of this comparative example and that of Example 1 is only that graphitized carbon black GCB is used to replace cyanamide waste residue carbon. According to the appendix Figure 8 、 9The results show that the decolorization effect of cyanamide waste residue carbon and the extraction recovery rates of 32 alkaloids are significantly better than those of graphitized carbon black GCB. Especially 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 using the cyanamide waste residue carbon of this application, the extraction recovery rate is as high as 89%, an increase of 35%; in the extraction of N-trans-feruloyltyramine alkaloid, 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 using the cyanamide waste residue carbon of this application, the extraction recovery rate is as high as 88%, an increase of 30%, demonstrating unexpected technical effects.

Claims

1. Application of cyanamide waste residue charcoal in lotus alkaloid extraction, characterized in that: The following steps are involved: The pigment in the lotus extract is adsorbed by cyanamide waste residue charcoal to obtain a pre-treated solution; the alkaloid in the pre-treated solution is adsorbed by a mixed strong cation exchange material; Elution to obtain 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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