CN108658770B - Method for preparing chlorogenic acid monomer from black diamond potatoes - Google Patents
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Abstract
The invention discloses a method for preparing chlorogenic acid monomer from black diamond potato, which comprises the following steps: (1) adding the extracting solution into the black diamond potato powder to prepare chlorogenic acid extracting solution; (2) enabling the chlorogenic acid extracting solution to pass through a macroporous resin adsorption column at the flow rate of 1-3 mL/min, washing with water and eluting with ethanol to obtain a crude chlorogenic acid product; (3) preparing a chlorogenic acid crude product into a first chlorogenic acid solution, extracting the first chlorogenic acid solution for 1-2 times by using ethyl acetate, collecting an ethyl acetate layer, and concentrating and drying to obtain a chlorogenic acid refined product; (4) preparing a refined chlorogenic acid product into a second chlorogenic acid solution, separating the second chlorogenic acid solution by using semi-preparative liquid chromatography, and concentrating and drying collected samples to obtain chlorogenic acid monomers. The chlorogenic acid is extracted from the black-diamantine potatoes by a solvent extraction method, ethyl acetate extraction and semi-preparative high performance liquid chromatography, and the purity of the prepared chlorogenic acid monomer reaches 97-99%.
Description
Technical Field
The invention belongs to the technical field of chlorogenic acid monomer preparation, and particularly relates to a method for preparing chlorogenic acid monomer from black diamantane potatoes.
Background
Chlorogenic acid is an organic acid containing hydroxyl and O-diphenol hydroxyl, is chemically named as 5-O-caffeoyl quinic acid, and is a phenylpropanoid compound produced by plants in an aerobic respiration process through a shikimic acid pathway. Chlorogenic acid is an important bioactive substance, has wide pharmacological action and biological activity, is not only a main effective component of a plurality of medicinal materials and Chinese patent medicines for resisting bacteria, detoxifying, diminishing inflammation and benefiting gallbladder, but also has the effects of resisting viruses, increasing leucocytes, resisting tumors, reducing blood pressure, reducing blood fat, eliminating free radicals, exciting a central nervous system and the like. Chlorogenic acid is widely existed in plants, and is mainly extracted from the plants such as honeysuckle, eucommia bark and the like at present due to the high content of the honeysuckle and the eucommia bark.
The seed coats of the black king's rhizoma Solani Tuber osi are black, bright and rich in luster, and are black and purple due to the rich purple anthocyanin, so that the black king's rhizoma Solani Tuber osi is a rare potato variety which integrates the functions of introduction, cultivation and medicine and food in China. At present, the active ingredients in the black diamond potatoes are mainly researched at home and abroad by focusing on natural pigments, but the black diamond potatoes in Van county in the course of research by the subject group contain a substance with richer content of the pigment, and the substance is proved to be chlorogenic acid after monomer separation, purification and structure characterization. Chlorogenic acid is mainly extracted from honeysuckle, eucommia and other plants at present, for example: patent application No. 201710075147.0 discloses a method for extracting chlorogenic acid from green coffee beans, which mainly uses equipment for extraction; patent application No. 201711344050.1 discloses a method for extracting chlorogenic acid from eucommia ulmoides, which is mainly extracted by an enzymatic method; patent application No. 201810154455.7 discloses a method for extracting chlorogenic acid from fresh sweet potato leaves, which adopts an ultrasonic extraction method, a microwave-assisted ethanol extraction method and an enzymolysis-assisted ethanol extraction method to ensure the extraction efficiency. The report of extracting chlorogenic acid from the black-diamantine potatoes does not exist, a spray drying unit is required in the first invention, the requirement on equipment is high, the purity of extracted chlorogenic acid is only 70.3%, and the functional research of the extracted chlorogenic acid serving as a quantitative standard and the chlorogenic acid cannot be met; in the latter two inventions, an enzymolysis method is required, enzyme and enzymolysis products are introduced in the enzymolysis process, so that the difficulty of separation and purification is increased, and the purity of the extracted chlorogenic acid is still not high enough.
Disclosure of Invention
The invention aims to overcome the technical defects, provides an extraction method with high purity of chlorogenic acid monomer, and also aims to provide a method for extracting chlorogenic acid from black diamond potatoes.
In order to achieve the technical purpose, the technical scheme of the invention provides a method for preparing chlorogenic acid monomers from black diamantane potatoes, which comprises the following steps:
s1, adding an extracting solution into black diamond potato powder to prepare a chlorogenic acid extracting solution;
s2, enabling the chlorogenic acid extracting solution to pass through a macroporous resin adsorption column at the flow rate of 1-3 mL/min, washing the macroporous resin adsorption column with water after adsorption saturation, eluting chlorogenic acid with an ethanol solution, collecting an eluent, concentrating and drying to obtain a crude chlorogenic acid product;
s3, preparing the crude chlorogenic acid product into a first chlorogenic acid solution, extracting the first chlorogenic acid solution for 1-2 times by using ethyl acetate, collecting an ethyl acetate layer, and concentrating and drying to obtain a refined chlorogenic acid product;
s4, preparing the refined chlorogenic acid product into a second chlorogenic acid solution, separating the second chlorogenic acid solution by using semi-preparative liquid chromatography, performing gradient elution by using a formic acid solution-acetonitrile, collecting a sample with retention time of 13.3-14.3min, and concentrating and drying to obtain a chlorogenic acid monomer.
Compared with the prior art, the invention has the beneficial effects that:
1. the method comprises the steps of extracting chlorogenic acid in an extraction liquid by a solvent extraction method and ethyl acetate in one step, wherein the purity of the chlorogenic acid in the extraction liquid reaches 72-75%, extracting a chlorogenic acid monomer from the black diamondra and the potato by combining with a semi-preparative liquid chromatography, wherein the purity of the prepared chlorogenic acid monomer reaches 97-99%, which is obviously higher than that of the chlorogenic acid monomer extracted in the prior art, and the purity of the chlorogenic acid monomer prepared by the method meets the requirements of quantitative standards and functional research;
2. the chlorogenic acid monomer is extracted from the anthocyanin extracting solution of the black diamond potato by using ethyl acetate, and is a waste liquid part for preparing anthocyanin, and the chlorogenic acid is extracted by using the waste liquid part, so that the waste of resources is avoided, and the comprehensive utilization of the black diamond potato is realized;
3. china is advancing the industrialization plan of potatoes as staple food products, compared with the extraction of chlorogenic acid from traditional Chinese medicine raw materials such as honeysuckle and eucommia, the raw materials have wide sources and rich resources, and the extracted chlorogenic acid does not have the smell of Chinese herbal medicines;
4. the extraction method is simple, the process flow is easy to control, and the method is suitable for industrial automatic control production.
Drawings
FIG. 1 is a process flow diagram of chlorogenic acid monomer extraction from a black-eyed potato;
FIG. 2 is a high performance liquid chromatography analysis chart of chlorogenic acid of the extract of Solanum nigrum Linn;
FIG. 3 shows the hydrogen spectrum of chlorogenic acid of Solanum nigrum extract ((R))1HNMR) map;
FIG. 4 is a carbon spectrum of chlorogenic acid of Solanum nigrum extract ((C))13CNMR) map;
figure 5 is a DEPT135 spectrum of chlorogenic acid from Solanum nigra extract.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the following description, with reference to the accompanying drawings and examples, further details of the method for preparing chlorogenic acid monomer from black diamantane potato according to the present invention are provided. The experimental procedures in the following examples are conventional unless otherwise specified. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1:
embodiment 1 of the present invention provides a method for preparing chlorogenic acid monomer from black diamantane potatoes, comprising the following steps:
(1) extraction: cleaning and peeling rotten black king-kong potatoes, cutting the potatoes into strips, drying the potato strips at 50 ℃, crushing the dried potato strips, and sieving the potato strips with a 40-mesh sieve to obtain black king-kong potato powder; adding 2g of black diamond potato powder into 120mL of hydrochloric acid solution with the concentration of 0.3mol/L, then leaching at 70 ℃ for 2h, transferring the leaching solution into a centrifugal machine, and carrying out centrifugal separation for 10min under the condition that the rotating speed is 8000r/min to obtain supernatant, namely chlorogenic acid extracting solution;
(2) preparing a crude chlorogenic acid powder: allowing the chlorogenic acid extracting solution obtained in the step (1) to pass through an adsorption column filled with macroporous resin D101 at the flow rate of 1mL/min, after dynamic adsorption saturation, washing the macroporous resin adsorption column with deionized water at the flow rate of 1mL/min until effluent is colorless, eluting chlorogenic acid adsorbed by the macroporous resin with an ethanol solution with the volume fraction of 60% at the flow rate of 1mL/min, collecting ethanol eluate until no chlorogenic acid flows out, concentrating the collected eluate at 50 ℃ under reduced pressure to paste to obtain a chlorogenic acid concentrated solution, and freeze-drying the chlorogenic acid concentrated solution to obtain crude chlorogenic acid powder of 14.2 mg;
(3) preparing refined chlorogenic acid powder: adding a proper amount of deionized water into the crude chlorogenic acid powder to completely dissolve the crude chlorogenic acid powder to obtain a first chlorogenic acid solution, adding 2 times of ethyl acetate into the first chlorogenic acid solution, extracting for 1 time, collecting an ethyl acetate layer, concentrating and drying to obtain refined chlorogenic acid powder 5.7mg with a purity of 72%;
(4) separation and purification: mixing 0.3% formic acid and acetonitrile according to a volume ratio of 1: 9 preparing a solvent, adding a proper amount of solvent into the refined chlorogenic acid powder to completely dissolve the chlorogenic acid powder to obtain a second chlorogenic acid solution, and separating and purifying the second chlorogenic acid solution by using a semi-preparative liquid chromatograph under the conditions of: the chromatographic column is Daisogel C18Column (20 mm. times.250 mm, 10 μm), detection wavelength 324nm, mobile phase 0.3% formic acid (A)And acetonitrile (B), gradient elution procedure as follows:
at 0min, the mobile phase A is 80% and the mobile phase B is 20%;
at 5min, the mobile phase A is 80% and the mobile phase B is 20%;
at 13min, the mobile phase A is 70%, and the mobile phase B is 30%;
at 17min, the mobile phase A is 65%, and the mobile phase B is 35%;
at 20min, the mobile phase A is 65%, and the mobile phase B is 35%;
at 21min, the mobile phase A is 70%, and the mobile phase B is 30%;
at 30min, mobile phase A was 80% and mobile phase B was 20%.
The flow rate is 15mL/min, the sample amount is 2mL, a sample with the retention time of 13.3-14.3min is collected, and the chlorogenic acid monomer 3.3mg with the purity of 97% is obtained after the solvent is removed by decompression concentration and freeze drying.
Example 2:
(1) extraction: cleaning and peeling rotten black king-kong potatoes, cutting the potatoes into strips, drying the potato strips at 50 ℃, crushing the dried potato strips, and sieving the potato strips with a 40-mesh sieve to obtain black king-kong potato powder; adding 2g of black diamond potato powder into 160mL of hydrochloric acid solution with the concentration of 0.1mol/L, then leaching for 1h at 70 ℃, transferring the leaching solution into a centrifugal separator, and carrying out centrifugal separation for 10min at the rotation speed of 8000r/min to obtain supernatant, namely chlorogenic acid extracting solution;
(2) preparing a crude chlorogenic acid powder: allowing the chlorogenic acid extracting solution obtained in the step (1) to pass through an adsorption column filled with macroporous resin AB-8 type at the flow rate of 1mL/min, after dynamic adsorption saturation, washing the macroporous resin adsorption column with deionized water at the flow rate of 3mL/min until effluent is colorless, eluting chlorogenic acid adsorbed by the macroporous resin with an ethanol solution with the volume fraction of 60% at the flow rate of 1mL/min, collecting ethanol eluate until no chlorogenic acid flows out, concentrating the collected eluate at 50 ℃ under reduced pressure to paste to obtain a chlorogenic acid concentrated solution, and freeze-drying the chlorogenic acid concentrated solution to obtain crude chlorogenic acid powder of 12.8 mg;
(3) preparing refined chlorogenic acid powder: adding a proper amount of deionized water into the crude chlorogenic acid powder to completely dissolve the crude chlorogenic acid powder to obtain a first chlorogenic acid solution, then adding 2 times volume of ethyl acetate into the first chlorogenic acid solution to extract for 2 times, collecting, combining ethyl acetate layers, concentrating and drying to obtain refined chlorogenic acid powder 5.1mg with purity of 73%;
(4) separation and purification: mixing 0.3% formic acid and acetonitrile according to a volume ratio of 1: 9 preparing a solvent, adding a proper amount of solvent into the refined chlorogenic acid powder to completely dissolve the chlorogenic acid powder to obtain a second chlorogenic acid solution, separating and purifying the second chlorogenic acid solution by using a semi-preparative liquid chromatograph, separating and purifying under the same separation and purification conditions as those in the example 1, collecting a monomer peak with retention time of 13.3-14.3min, removing the solvent by concentration under reduced pressure, and freeze-drying to obtain 2.96mg of chlorogenic acid monomer with purity of 98%.
Example 3:
embodiment 3 of the present invention provides a method for preparing chlorogenic acid monomer from black diamantane potatoes, comprising the following steps:
(1) extraction: cleaning and peeling rotten black king-kong potatoes, cutting the potatoes into strips, drying the potato strips at 40 ℃, crushing the dried potato strips, and sieving the dried potato strips with a 80-mesh sieve to obtain black king-kong potato powder; adding 20g of black diamond potato powder into 1200mL of 2 wt% citric acid solution, leaching at 60 ℃ for 2h, transferring the leaching solution into a centrifugal separator, and performing centrifugal separation for 10min at the rotation speed of 6000r/min to obtain a supernatant, namely chlorogenic acid extracting solution;
(2) preparing a crude chlorogenic acid powder: allowing the chlorogenic acid extracting solution obtained in the step (1) to pass through an X-5 type adsorption column filled with macroporous resin at the flow rate of 1mL/min, after dynamic adsorption saturation, washing the macroporous resin adsorption column with deionized water at the flow rate of 3mL/min until effluent is colorless, eluting chlorogenic acid adsorbed by the macroporous resin with 80% ethanol solution in volume fraction at the flow rate of 3mL/min, collecting ethanol eluate until no chlorogenic acid flows out, concentrating the collected eluate at 50 ℃ under reduced pressure to paste to obtain a chlorogenic acid concentrated solution, and freeze-drying the chlorogenic acid concentrated solution to obtain crude chlorogenic acid powder of 136.2 mg;
(3) preparing refined chlorogenic acid powder: adding a proper amount of deionized water into the crude chlorogenic acid powder to completely dissolve the crude chlorogenic acid powder to obtain a first chlorogenic acid solution, adding 1 volume of ethyl acetate into the first chlorogenic acid solution, extracting for 1 time, collecting an ethyl acetate layer, concentrating and drying to obtain refined chlorogenic acid powder 54.8mg with a purity of 74%;
(4) separation and purification: mixing 0.3% formic acid and acetonitrile according to a volume ratio of 1: 9 preparing a solvent, adding a proper amount of solvent into the refined chlorogenic acid powder to completely dissolve the chlorogenic acid powder to obtain a second chlorogenic acid solution, separating and purifying the second chlorogenic acid solution by using a semi-preparative liquid chromatograph, separating and purifying under the same separation and purification conditions as those in the example 1, collecting a monomer peak with retention time of 13.3-14.3min, removing the solvent by concentration under reduced pressure, and freeze-drying to obtain 31.5mg of chlorogenic acid monomer with purity of 98%.
Example 4:
(1) extraction: cleaning and peeling rotten black king-kong potatoes, cutting the potatoes into strips, drying the potato strips at 50 ℃, crushing the dried potato strips, and sieving the potato strips with a 40-mesh sieve to obtain black king-kong potato powder; adding 20g of black diamond potato powder into 1600mL of 4wt% citric acid solution, leaching at 50 ℃ for 2h, transferring the leaching solution into a centrifugal separator, and performing centrifugal separation for 15min at the rotation speed of 4000r/min to obtain supernatant, namely chlorogenic acid extracting solution;
(2) preparing a crude chlorogenic acid powder: allowing the chlorogenic acid extracting solution obtained in the step (1) to pass through an adsorption column filled with macroporous resin DM130 at the flow rate of 3mL/min, after dynamic adsorption saturation, washing the macroporous resin adsorption column with deionized water at the flow rate of 3mL/min until effluent is colorless, eluting chlorogenic acid adsorbed by the macroporous resin with 80% ethanol solution at the flow rate of 3mL/min, collecting ethanol eluate until no chlorogenic acid flows out, concentrating the collected eluate at 50 ℃ under reduced pressure to obtain a chlorogenic acid concentrated solution, and freeze-drying the chlorogenic acid concentrated solution to obtain crude chlorogenic acid powder of 136.7 mg;
(3) preparing refined chlorogenic acid powder: adding a proper amount of deionized water into the crude chlorogenic acid powder to completely dissolve the crude chlorogenic acid powder to obtain a first chlorogenic acid solution, adding 1 volume of ethyl acetate into the first chlorogenic acid solution, extracting for 1 time, collecting an ethyl acetate layer, concentrating and drying to obtain refined chlorogenic acid powder 54.9mg with a purity of 75%;
(4) separation and purification: mixing 0.3% formic acid and acetonitrile according to a volume ratio of 1: 9 preparing a solvent, adding a proper amount of solvent into the refined chlorogenic acid powder to completely dissolve the chlorogenic acid powder to obtain a second chlorogenic acid solution, separating and purifying the second chlorogenic acid solution by using a semi-preparative liquid chromatograph, separating and purifying under the same separation and purification conditions as those in the example 1, collecting a monomer peak with retention time of 13.3-14.3min, removing the solvent by concentration under reduced pressure, and freeze-drying to obtain 37.1mg of chlorogenic acid monomer with purity of 99%.
The chlorogenic acid monomers extracted in the embodiments 1-4 of the invention are analyzed and identified by the following methods:
(1) analyzing the purity of chlorogenic acid monomer by analytical liquid chromatography, and separating by the following method: the chromatographic column is DaisoglelC18Column (20 mm. times.250 mm, 10 μm), detection wavelength 324nm, mobile phase 0.3% formic acid (A) and acetonitrile (B), gradient elution procedure as follows:
at 0min, the mobile phase A is 90%, and the mobile phase B is 10%;
at 5min, the mobile phase A is 88%, and the mobile phase B is 12%;
at 13min, the mobile phase A is 79%, and the mobile phase B is 21%;
at 14min, the mobile phase A is 90%, and the mobile phase B is 10%;
at 16min, the mobile phase A is 90%, and the mobile phase B is 10%;
the flow rate is 1mL/min, the sample amount is 10 muL, and the volume ratio of the sample to the sample is 1: 0.3% of formic acid and acetonitrile of 9 were dissolved and the analysis results are shown in FIG. 2.
(2) Identification of chlorogenic acid monomer: after the sample was dissolved in tetradeuteromethanol (CD3OD), the hydrogen spectrum (1HNMR), the carbon spectrum (13CNMR) and the DEPT135 spectrum of the sample solution were measured on a Bruker 400MHZ (Avance III HD 400, Bruker, switzerland) nuclear magnetic resonance apparatus using Tetramethylsilane (TMS) as an internal standard, and the measurement results are shown in fig. 3 to 5.
As can be seen from FIG. 2, the retention time of the chlorogenic acid monomer peak is 5.358min, and the purity of the chlorogenic acid monomer is 97-99%.
It can be seen from FIGS. 3 to 5 that the results of the nuclear magnetic resonance measurement are as follows:
1H-NMR(CD3OD)：δ7.55(1H，d，J＝15.8Hz，H-7′)，7.04(1H，br.S，H-2′)，6.94(1H，br.D，J＝8.1Hz，H-6′)，6.77(1H，d，J＝8.1Hz,H-5′)，6.25(1H，d，J＝15.8Hz，H-8′)，5.33(1H，br.Dd，J＝10.2，8.0Hz，H-5)，4.17(1H，br.S，H-3)，3.72(1H，br.D，J＝8.0Hz，H-4)，1.98–2.28(4H，m，H-2and H-6)；
13C-NMR(CD3OD)：δ177.3(s，C-7)，168.7(s，C-9′)，149.5(s，C-4′)，147.1(d,C-7′)，146.8(s，C-3′)，127.8(s，C-1′)，123.0(d，C-6′)，116.5(d，C-5′)，115.3(d，C-2′)，115.2(d，C-8′)，76.3(s，C-1)，73.6(d，C-4)，72.0(d，C-5)，71.4(d，C-3)，38.9(t，C-6)，38.2(t，C-2)。
the results of nuclear magnetic resonance measurements are consistent with the chemical component studies of Panax notoginseng [ J ]. Chinese herbal medicine, 41(8): 1236-.
The above-described embodiments of the present invention should not be construed as limiting the scope of the present invention. Any other corresponding changes and modifications made according to the technical idea of the present invention should be included in the protection scope of the claims of the present invention.
Claims (8)
1. A method for preparing chlorogenic acid monomers from a black diamantane potato is characterized by comprising the following steps:
s1, adding an extracting solution into black diamond potato powder to prepare a chlorogenic acid extracting solution;
s2, enabling the chlorogenic acid extracting solution to pass through a macroporous resin adsorption column at the flow rate of 1-3 mL/min, washing the macroporous resin adsorption column with water after adsorption saturation, eluting chlorogenic acid with an ethanol solution, collecting an eluent, concentrating and drying to obtain a crude chlorogenic acid product;
s3, preparing the crude chlorogenic acid product into a first chlorogenic acid solution, extracting the first chlorogenic acid solution for 1-2 times by using ethyl acetate, collecting an ethyl acetate layer, and concentrating and drying to obtain a refined chlorogenic acid product;
s4, preparing the refined chlorogenic acid product into a second chlorogenic acid solution, separating the second chlorogenic acid solution by using semi-preparative liquid chromatography, performing gradient elution by using a formic acid solution-acetonitrile, collecting a sample with retention time of 13.3-14.3min, and concentrating and drying to obtain a chlorogenic acid monomer;
the chlorogenic acid extracting solution prepared in the step S1 is prepared by the following method: adding an extracting solution into the black diamondback potato powder, leaching for 1-2 hours at 50-70 ℃, and then centrifugally separating the leaching solution to obtain a chlorogenic acid extracting solution;
the extracting solution is hydrochloric acid solution with the concentration of 0.1-0.3 mol/L or citric acid solution with the concentration of 2-4 wt%.
2. The method for preparing chlorogenic acid monomer from black diamantane potato as claimed in claim 1, wherein semi-preparative liquid chromatography separation conditions in step S4 are as follows: daisogel C18Chromatographic column, phi 20 × 250mm, 10 μm; the flow rate is 15 mL/min; the detection wavelength is 324 nm; mobile phase: performing gradient elution on 0.3 percent formic acid solution A and acetonitrile B; the sample volume is 2 mL.
3. The method for preparing chlorogenic acid monomer from black diamantane potato according to claim 2, characterized in that the gradient elution is performed by the following method: 0-13 min, 70-80% A; 13-21 min, 65-70% A; 21-30 min, 70-80% A.
4. The method for preparing chlorogenic acid monomers from black diamantane potatoes as claimed in claim 1, wherein the volume ratio of the first chlorogenic acid solution to the ethyl acetate in step S3 is 1: 1 to 2.
5. The method of preparing chlorogenic acid monomer from black diamond potato according to claim 1,
the macroporous resin adsorption column in the step S2 is any one of AB-8 type, D101 type, DM130 type or X-5 type macroporous resin.
6. The method for preparing chlorogenic acid monomer from black diamantane potato according to claim 1, wherein chlorogenic acid is eluted by ethanol solution with a flow rate of 1-3 mL/min in step S2, and the volume fraction of the ethanol solution is 60-80%.
7. The method for preparing chlorogenic acid monomer from black diamondoid potato according to claim 1, wherein the feed-liquid ratio of black diamondoid potato powder to extract in step S1 is 1 g: 60-80 mL.
8. The method for preparing chlorogenic acid monomer from black diamantane potato according to claim 1, wherein step S1 further comprises: cleaning and peeling the rotten black diamond potatoes, cutting the potatoes into strips, drying the potato strips at 40-50 ℃, crushing the dried potato strips, and sieving the dried potato strips with a 40-80-mesh sieve to obtain black diamond potato powder.
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| D201树脂对绿原酸的吸附、解析性能研究;赵升强等;《食品工业科技》;20131231;第34卷(第7期);第61-63、67页 * |
| 绿原酸提取分离及检测研究进展;周舟等;《长江大学学报(自然科学版)》;20110228(第02期);第243-246页 * |
| 马铃薯皮中绿原酸提取工艺优化;李次力等;《食品科学》;20141231;第35卷(第12期);第70-74页 * |
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