Method for separating and purifying mogroside V by subcritical water desorption technology

10759827 ยท 2020-09-01

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Abstract

The invention relates to a method for separating and purifying mogroside V by subcritical water desorption technology. The macroporous adsorption resin enriched with mogroside V is subjected to desorption under a subcritical condition of water using water as a solvent, to give an aqueous solution rich in mogroside V. The method not only improves the content of mogroside V in product, but also effectively removes bitter impurities and residual pesticides, greatly improves the taste adaptability of the product, and improves the safety and quality of the product. The method reduces the processing steps and reduces the use of organic solvents in the prior art, and reduces total production costs.

Claims

1. A method for separating and purifying mogroside V by subcritical water desorption technology, comprising: crushing the raw material of Siraitia grosvenori fresh fruit or dried fruit, and then extracting with purified water as solvent using a continuous dynamic countercurrent extraction apparatus under the following conditions: a solid-liquid ratio of 50 to 250 g/L, a temperature of 60 to 90 C. a circulation velocity of the purified water of 1,500 to 4,000 L/h, a raw material feeding rate of 500 to 1,500 kg/h, and a time period for extraction of 30 to 180 min, so as to give a water extract of Siraitia grosvenori; (2) centrifuging the water extract of Siraitia grosvenori at a rotation speed of 10,000 to 13,000 r/min for 10 to 20 min so as to give a centrifuged liquid; (3) successively filtering the centrifuged liquid obtained from the centrifuging through a ceramic membrane having a pore size of 50 to 100 m and a ceramic membrane having a pore size of 5 to 20 m, so as to give a filtrate; and (4) absorbing the filtrate on a D101 macroporous adsorption resin with the mass ratio of the macroporous adsorption resin to the raw material of Siraitia grosvenori being 1:5 to 1:20, so as to give the macroporous adsorption resin enriched with mogroside V; (5) subjecting the macroporous adsorption resin enriched with mogroside V to desorption-extraction using 5 to 8 bed volumes (BV) purified water in a subcritical state under a pressure of 8 to 15 MPa and a temperature of 120 to 170 C. at a circulation velocity of 5 to 8 BV/h, to give a Siraitia grosvenori aqueous solution: and (6) concentrating the obtained Siraitia grosvenori aqueous solution containing mogroside V through a ceramic membrane with a relative molecular weight cutoff of 150 to 250 Daltons, to give a Siraitia grosvenori concentrated solution.

2. The method of claim 1, wherein the desorption-extraction is carried out on the macroporous adsorption resin enriched with mogroside V using 5 BV purified water in a subcritical state under a pressure of 10 MPa and a temperature of 160 C. at a circulation velocity of 5 BV/h, to give a Siraitia grosvenori aqueous solution.

3. The method of claim 1, wherein the macroporous adsorption resin enriched with mogroside V is prepared by a method comprising: (1) crushing the raw material of Siraitia grosvenori fresh fruit or dried fruit, and then extracting with purified water as solvent using a continuous dynamic countercurrent extraction apparatus under the following conditions: a solid-liquid ratio of 90 g/L, a temperature of 85 C., a circulation velocity of the purified water of 2,500 L/h, a raw material feeding rate of 1,100 kg/h, and a time period for extraction of 120 min, so as to give the water extract of Siraitia grosvenori; (2) centrifuging the water extract of Siraitia grosvenori at a rotation speed of 12,000 r/min for 15 min so as to give the centrifuged liquid; (3) successively filtering the centrifuged liquid through a ceramic membrane having a pore size of 80 m and a ceramic membrane having a pore size of 10 m, so as to give the filtrate; and (4) absorbing the filtrate on the D101 macroporous adsorption resin with the mass ratio of the used macroporous adsorption resin to the raw material of Siraitia grosvenori being 1:10, so as to give the macroporous adsorption resin enriched with mogroside V.

4. A method for preparing mogroside V, wherein the mogroside V is prepared by drying the Siraitia grosvenori concentrated solution prepared by the method of claim 1.

5. A method for preparing mogroside V, wherein the mogroside V is prepared by drying the Siraitia grosvenori concentrated solution prepared by the method of claim 2.

6. A method for preparing mogroside V, wherein the mogroside V is prepared by drying the Siraitia grosvenori concentrated solution prepared by the method of claim 3.

Description

Example 1

(1) (1) 1,000 kg of Siraitia grosvenori dried fruits were crushed, and then extracted by continuous dynamic countercurrent extraction apparatus with purified water as solvent under the following conditions: a solid-liquid ratio of 50 g/L, a temperature of 90 C., a circulation velocity of purified water of 4,000 L/h, a raw material feeding rate of 1,500 kg/h, and a time period for extraction of 180 min, so as to give a water extract of Siraitia grosvenori;

(2) (2) the water extract of Siraitia grosvenori obtained in step (1) was centrifuged at a rotation speed of 10,000 r/min for 20 min so as to give a centrifuged liquid;

(3) (3) the centrifuged liquid obtained in step (2) was filtered successively through a ceramic membrane having a pore size of 50 m and a ceramic membrane having a pore size of 5 m so as to give a filtrate;

(4) (4) the filtrate obtained in step (3) was absorbed by macroporous adsorption resin D101 with the mass ratio of the employed macroporous adsorption resin to the raw material of Siraitia grosvenori being 1:5, so as to give a macroporous adsorption resin enriched with mogroside V;

(5) (5) desorption-extraction was carried out on the macroporous adsorption resin enriched with mogroside V using 8 BV purified water in a subcritical state under a pressure of 15 Mpa and a temperature of 170 C. at a circulation velocity of 8 BV/h, to give a Siraitia grosvenori aqueous solution; and

(6) (6) the Siraitia grosvenori aqueous solution obtained in step (5) was concentrated through a ceramic membrane with a relative molecular weight cutoff of 150, to give a Siraitia grosvenori concentrated solution.

Example 2

(7) (1) 1,000 kg of Siraitia grosvenori dried fruits were crushed, and then extracted using a continuous dynamic countercurrent extraction apparatus with purified water as solvent under the following conditions: a solid-liquid ratio of 90 g/L, a temperature of 85 C., a circulation velocity of purified water of 2,500 L/h, a raw material feeding rate of 1,100 kg/h, and a time period for extraction of 120 min, so as to give a water extract of Siraitia grosvenori;

(8) (2) the water extract of Siraitia grosvenori obtained in step (1) was centrifuged at a rotation speed of 12,000 r/min for 15 min so as to give a centrifuged liquid;

(9) (3) the centrifuged liquid obtained in step (2) was filtered successively through a ceramic membrane having a pore size of 80 m and a ceramic membrane having a pore size of 10 m so as to give a filtrate;

(10) (4) the filtrate obtained in step (3) was absorbed by microspheric macroporous adsorption resin with the mass ratio of the microspheric macroporous adsorption resin to the raw material of Siraitia grosvenori being 1:10, so as to give a microspheric macroporous adsorption resin enriched with mogroside V;

(11) (5) desorption-extraction was carried out on the microspheric macroporous adsorption resin enriched with mogroside V using 5 BV purified water in a subcritical state under a pressure of 10 Mpa and a temperature of 160 C. at a circulation velocity of 5 BV/h, to give a Siraitia grosvenori aqueous solution; and

(12) (6) the Siraitia grosvenori aqueous solution obtained in step (5) was concentrated through a ceramic membrane with a relative molecular weight cutoff of 200, to give a Siraitia grosvenori concentrated solution.

Example 3

(13) (1) 1,000 kg of Siraitia grosvenori dried fruits were crushed, and then extracted using a continuous dynamic countercurrent extraction apparatus with purified water as solvent under the following conditions: a solid-liquid ratio of 250 g/L, a temperature of 60 C., a circulation velocity of purified water of 1,500 L/h, a raw material feeding rate of 500 kg/h, and a time period for extraction of 30 min, so as to give a water extract of Siraitia grosvenori;

(14) (2) the water extract of Siraitia grosvenori obtained in step (1) was centrifuged at a rotation speed of 13,000 r/min for 10 min so as to give a centrifuged liquid;

(15) (3) the centrifuged liquid obtained in step (2) was filtered successively through a ceramic membrane having a pore size of 100 m and a ceramic membrane having a pore size of 20 m so as to give a filtrate;

(16) (4) the filtrate obtained in step (3) was absorbed by macroporous adsorption resin D101 with the mass ratio of the macroporous adsorption resin to the raw material of Siraitia grosvenori being 1:20, so as to give a macroporous adsorption resin enriched with mogroside V;

(17) (5) desorption-extraction was carried out on the macroporous adsorption resin enriched with mogroside V using 5 BV purified water in a subcritical state under a pressure of 8 Mpa and a temperature of 120 C. at a circulation velocity of 5 BV/h, to give a Siraitia grosvenori aqueous solution; and

(18) (6) the Siraitia grosvenori aqueous solution obtained in step (5) was concentrated through a ceramic membrane with a relative molecular weight cutoff of 250, to give a Siraitia grosvenori concentrated solution.

Comparative Example 1

(19) This Comparative Example refers to the technical solution disclosed in the Reference document 1, and was used to evaluate the difference in technical effect between the technical solution of the Reference document 1 and that of the present invention. The specific steps were given as follows:

(20) (1) 1,000 kg of fresh Siraitia grosvenori were fed together with water at a ratio of 1:15 into a countercurrent extraction apparatus in three equal portions at three time points with an interval of 20 min, and extracted at a temperature of 60 C. for 75 min;

(21) (2) the extract solution was rough filtered and cooled to 40 to 50 C., and 0.5%0 of pectin complex enzyme was added to perform enzymolysis for 60 min.

(22) (3) the extract solution undergoing enzymolysis was filtered through a 0.5 m microfiltration membrane, rapidly cooled to 20 C., and centrifuged at 6,000 r/min, and then ultrafiltered with a hollow cellulose membrane with a relative molecular weight cutoff of 60,000 Daltons;

(23) (4) the filtrate was concentrated to 6 Brix by vacuum concentrator at a temperature of 50 to 55 C. under a vacuum degree of 0.06 to 0.1;

(24) (5) the concentrated solution was passed through macroporous adsorption resin D101 until a leak point was achieved, the effluent was discarded, and then the macroporous adsorption resin D101 was washed with deionized water;

(25) (6) the macroporous adsorption resin D101 was eluted with 50% ethanol until it has no sweetness, and the ethanol eluate was collected;

(26) (7) the ethanol eluate was decolorized with an anion exchange resin, and the decolorized solution was collected; and

(27) (8) ethanol was recovered from the decolorized solution, and the decolorized solution was concentrated in vacuum to give Siraitia grosvenori concentrated solution.

Comparative Example 2

(28) The technical solution of this Comparative Example adopts subcritical water in an extraction step, and macroporous resin adsorption and water-ethanol elution in a desorption step, so as to evaluate the difference in technical effect between the technical solution in which the subcritical water was used for extraction and the technical solution of the present invention in which the subcritical water was sued for desorption from macroporous resin. The specific steps were given as follows:

(29) (1) 1,000 kg of Siraitia grosvenori dried fruits were crushed, and then extracted using a continuous dynamic countercurrent extraction apparatus with purified water as solvent under the following conditions: a solid-liquid ratio of 90 g/L, a subcritical state with a temperature of 160 C. and a pressure of 10 Mpa, a circulation velocity of purified water of 2,500 L/h, a raw material feeding rate of 1,100 kg/h, and a time period for extraction of 120 min, so as to give a water extract of Siraitia grosvenori;

(30) (2) the water extract of Siraitia grosvenori obtained in step (1) was centrifuged at a rotation speed of 12,000 r/min for 15 min so as to give a centrifuged liquid;

(31) (3) the centrifuged liquid obtained in step (2) was filtered successively through a ceramic membrane having a pore size of 80 m and a ceramic membrane having a pore size of 10 m so as to give a filtrate;

(32) (4) the filtrate obtained in step (3) was absorbed by microspheric macroporous adsorption resin with the mass ratio of the microspheric macroporous adsorption resin to the raw material of Siraitia grosvenori being 1:10, so as to give a microspheric macroporous adsorption resin enriched with mogroside V;

(33) (5) the microspheric macroporous adsorption resin enriched with mogroside V was eluted with 5 BV purified water and 3 BV 50% (v/v) ethanol, the water eluate was discarded, and the ethanol eluate was collected;

(34) (6) the ethanol was completely recovered and Siraitia grosvenori aqueous solution was obtained;

(35) (7) the Siraitia grosvenori aqueous solution obtained in step (6) was successively passed through a residual pesticide-removing resin with a mass ratio to the raw material of Siraitia grosvenori being 1:100, a strongly acidic 001*1 resin with a mass ratio to the raw material of Siraitia grosvenori being 1:100, a decolorizing resin with a mass ratio to the raw material of Siraitia grosvenori being 1:40, and an activated carbon with a mass ratio to the raw material of Siraitia grosvenori being 1:10, to give a treated solution; and

(36) (8) the treated solution obtained in step (7) was concentrated through a ceramic membrane with a relative molecular weight cutoff of 200 to give Siraitia grosvenori concentrated solution.

Comparative Example 3

(37) This Comparative Example refers to the technical solution disclosed in the Reference document 2, and was used to evaluate the difference in technical effect between the technical solution of the Reference document 2 and that of the present invention. The specific steps were as follows:

(38) (1) 1,000 kg of fresh Siraitia grosvenori were taken and extracted for 3 times at a temperature of 90 C. or higher. The amount of water added was 5 times the weight of the raw material for the first extraction, 4 times the weight of the raw material for the second extraction and 3 times the weight of the raw material for the third extraction; and the extraction time was 1.5 h for the first extraction, 1.0 h for the second extraction and 0.5 h for the third extraction; after each extraction was completed, filtration was carried out, and filter residue was used as the raw material for the next extraction; the filtrates obtained from the three times of extraction were combined and concentrated under vacuum at a temperature of 75 C. or less to a weight 4 times the weight of the fed fruit;

(39) (2) the concentrated extract solution was sedimentation-centrifuged at 2,000 to 4,000 r/min for 2 h;

(40) (3) a resin column was loaded with strongly basic anion exchange resin D-201 which accounts for 1/10 of the weight of fresh Siraitia grosvenori, then the centrifugate was allowed to pass through the resin column, the effluent was collected, and the resin column was washed with purified water until it has no sweetness, and all effluents were combined;

(41) (4) a resin column was pre-loaded with macroporous adsorption resin ADS-17 which accounts for 0.4 times of the weight of fresh Siraitia grosvenori, and the eluate treated with the ion exchange resin was passed through the resin column; and the resin column was washed with purified water until the effluent was colorless and transparent, finally, the resin column was desorbed with 55% edible ethanol, and the desorption solution was collected until it has no sweetness;

(42) (5) the desorption solution was concentrated under vacuum-decompressed at a temperature of 75 C. or less to a weight of 0.5 times the weight of the fed Siraitia grosvenori;

(43) (6) a resin column was pre-loaded with alumina which accounts for 0.04 times of the weight of fresh Siraitia grosvenori, the concentrated solution was diluted by 30 to 60 times, and passed through the alumina column, the effluent was collected, and the column was washed with purified water, and all effluents were collected; and

(44) (7) the effluent was concentrated under reduced pressure at a temperature of 75 C. or less to obtain a Siraitia grosvenori concentrated solution.

(45) Detection Experiment for the Content of Mogroside V and Multiple Pesticide Residues

(46) 1. Instruments and Reagents

(47) Instruments: High Performance Liquid Chromatography (Agilent), Agilent 6495 Liquid series mass spectrometer LC-MS/MS, 0.45 m microfiltration membrane and Syringe Filter, Pesticide Residue Purification Kit, microfiltration membrane 0.22 m, oscillator, centrifuge, electronic balance ( 1/10,000), and ultrasonic cleaner.

(48) Reagents: mogroside V standard substance (purchased from Chromadex), acetonitrile (chromatography grade), formic acid (mass spectrometry grade), ammonium formate (mass spectrometry grade), anhydrous magnesium sulfate (AR), sodium chloride (AR), methanol (AR), acetonitrile (chromatographically pure), and ultrapure water.

(49) 2. Method

(50) 2.1 Chromatographic Conditions and Operating Steps for the Determination of Mogroside V

(51) Chromatographic conditions: chromatographic column: LUNAC18, 250 mm4.6 mm, 5 m; mobile phase: acetonitrile (B)-0.1% phosphoric acid aqueous solution (A) being taken as mobile phase for gradient elution (0 to 17 min, 17.fwdarw.20%, phase B; 17 to 50 min, 20.fwdarw.26%, phase B), flow rate: 0.8 ml/min, detection wavelength: 203 nm; injection volume: 5 l; and column temperature: 25 C.

(52) Preparation of the test solution: about 60 mg (30%) of the sample was precisely weighed, placed in a 25 ml volumetric flask, dissolved by adding methanol, ultrasonically extracted for 15 min, cooled to room temperature, diluted with methanol to 25 mL, the mixture was shake up and passed through a 0.45 m filter membrane.

(53) Preparation of the standard solution: an appropriate amount of mogroside V standard substance was weighed precisely and prepared into a solution with a concentration of about 0.7 mg/ml by adding methanol. 5 l of the standard substance solution and 5 l of test solution were injected into the HPLC instrument respectively.

(54) 2.2 Chromatographic Conditions and Mass Spectrum Conditions for the Determination of Multiple Pesticide Residues

(55) Chromatographic conditions: chromatographic column: Agilent ZORBAX Eclipse Plus-C18 2.1 mm100 mm, 1.8 m; column temperature: 35 C.; needle washing: washing needle by needle seat with acetonitrile: water=10:90 for 3s; mobile phase: A: 0.1% formic acid and 0.1 mM ammonium formate aqueous solution, B: 0.1% formic acid in acetonitrile as mobile phase for gradient elution (0 to 10 min, 10.fwdarw.85%, phase B; 10 to 12 min, 85.fwdarw.95%, phase B), flow rate: 0.4 mL/min; stop time: 12 min; and post-run time: 3 min.

(56) Conditions for mass spectrometry: Dry gas temperature: 250 C.; flow rate of dry gas: 11 L/min; pressure of atomization gas: 40 psi; capillary voltage: 3,500 V; sheath gas temperature: 350 C., and flow rate of sheath gas: 12 L/min.

(57) 3. Results

(58) 3.1 Effect of Different Processes on the Content Mogroside V in Siraitia grosvenori Concentrated Solution

(59) TABLE-US-00001 TABLE 1 Effect of different processes on the content of mogroside V in Siraitia grosvenori concentrated solution Groups mass fraction % of mogroside V Example 1 59.26% 1.08% Example 2 72.40% 1.26% Example 3 55.07% 0.92% Comparative Example 1 35.37% 2.15% Comparative Example 2 42.18% 1.58% Comparative Example 3 46.34% 1.74%

(60) 3.2 Effect of Different Processes on the Residual Degree of Multiple Pesticides in Siraitia grosvenori Concentrated Solution

(61) TABLE-US-00002 TABLE 2 Effect of different processes on the residual degree of multiple pesticides in Siraitia grosvenori concentrated solution Reporting Test results threshold Comparative Comparative Comparative Test items (mg/kg) Example 1 Example 2 Example 3 Example 1 Example 2 Example 3 Acephate 0.001 less than less than less than 0.1270 less than less than reporting reporting reporting reporting reporting threshold threshold threshold threshold threshold Propamocarb 0.001 less than less than 0.0076 0.4053 0.0258 0.0863 reporting reporting threshold threshold Carbendazim 0.001 0.0276 0.0381 0.0952 4.6881 5.2012 3.2916 Imidacloprid 0.001 0.0015 0.0126 0.0098 2.8129 1.6251 1.2965 acetamiprid 0.001 0.0013 less than 0.0157 0.3437 0.1685 0.3817 reporting threshold Tricyclazole 0.001 less than less than less than less than less than less than reporting reporting reporting reporting reporting reporting threshold threshold threshold threshold threshold threshold Oxadixyl 0.001 less than less than less than less than 0.1267 0.0985 reporting reporting reporting reporting threshold threshold threshold threshold Thiophanate- 0.001 less than less than less than less than less than less than methyl reporting reporting reporting reporting reporting reporting threshold threshold threshold threshold threshold threshold Ametryn 0.001 less than 0.0056 0.0126 0.7486 0.0514 0.0483 reporting threshold Metalaxyl 0.001 0.0018 less than 0.0282 0.4288 0.1592 0.0942 reporting threshold Pyrimethanil 0.001 less than less than less than 0.0082 less than less than reporting reporting reporting reporting reporting threshold threshold threshold threshold threshold Isoprocarb 0.001 less than less than less than less than less than less than reporting reporting reporting reporting reporting reporting threshold threshold threshold threshold threshold threshold Triadimenol 0.001 less than less than less than less than less than less than reporting reporting reporting reporting reporting reporting threshold threshold threshold threshold threshold threshold Paclobutrazol 0.001 0.0032 less than less than 0.0572 0.1659 0.1365 reporting reporting threshold threshold Dimethomorph 0.001 less than less than less than less than less than less than reporting reporting reporting reporting reporting reporting threshold threshold threshold threshold threshold threshold Methidathion 0.001 less than less than less than less than less than less than reporting reporting reporting reporting reporting reporting threshold threshold threshold threshold threshold threshold Diethofencarb 0.001 less than less than less than less than less than less than reporting reporting reporting reporting reporting reporting threshold threshold threshold threshold threshold threshold Myclobutanil 0.001 less than less than less than less than less than less than reporting reporting reporting reporting reporting reporting threshold threshold threshold threshold threshold threshold Iprovalicarb 0.001 less than less than less than less than less than less than reporting reporting reporting reporting reporting reporting threshold threshold threshold threshold threshold threshold Azoxystrobin 0.001 less than less than 0.0085 0.2652 0.0125 0.0688 reporting reporting threshold threshold Triadimefon 0.001 0.0018 less than less than 0.0964 0.1351 less than reporting reporting reporting threshold threshold threshold Tebuconazole 0.001 less than less than less than less than less than less than reporting reporting reporting reporting reporting reporting threshold threshold threshold threshold threshold threshold Fluorosilazole 0.001 less than less than less than less than less than less than reporting reporting reporting reporting reporting reporting threshold threshold threshold threshold threshold threshold Hexaconazole 0.001 less than less than less than 0.0284 less than less than reporting reporting reporting reporting reporting threshold threshold threshold threshold threshold Metolachlor 0.001 less than less than less than 0.0197 less than less than reporting reporting reporting reporting reporting threshold threshold threshold threshold threshold Diniconazole 0.001 less than less than less than less than less than less than reporting reporting reporting reporting reporting reporting threshold threshold threshold threshold threshold threshold Propiconazole 0.001 less than less than less than less than less than less than reporting reporting reporting reporting reporting reporting threshold threshold threshold threshold threshold threshold Difenoconazole 0.001 0.0023 less than 0.0249 less than 0.1529 0.1647 reporting reporting threshold threshold Teflubenzuron 0.001 less than less than less than less than less than less than reporting reporting reporting reporting reporting reporting threshold threshold threshold threshold threshold threshold Chlorpyrifos 0.001 less than less than less than less than less than less than reporting reporting reporting reporting reporting reporting threshold threshold threshold threshold threshold threshold
Experiments for Mouthfeel Test

(62) 1. Experimental subjects: 20 subjects, 10 males and 10 females, aged from 18 to 40.

(63) 2. Exclusion criteria: those who has been suffered from oral diseases in the past three months or for a long-term; pregnant women, or women in physiological period; those who have parageusia caused by other situations.

(64) 3. Experimental method: each subject was successively administrated with the Siraitia grosvenori concentrated solutions obtained in Examples 1 to 3 and Comparative Examples 1 to 3 as the test samples, and each test sample was in a total amount of 10 ml, and consumed within 10 min twice or 3 times. The waiting time after each test sample was consumed was 15 minutes, and the next test sample was consumed after the waiting time. Before the experiment and during the waiting time, the taste of the subjects was cleaned with purified water and inorganic salt biscuits. The mouthfeel of each test sample was evaluated from 11 aspects including characteristic odor, characteristic taste, raw taste, sweetness, bitterness, astringency, duration of sweet aftertaste, duration of bitter aftertaste, duration of astringent aftertaste, characteristic aftertaste and overall consistency. For each indicator, 0 represented the minimum feeling value, 6 represented the maximum feeling value, and each result was represented by the average score.

(65) 4. Results

(66) TABLE-US-00003 TABLE 3 Effect of different processes on the mouthfeel of Siraitia grosvenori concentrated solution Comparative Comparative Comparative Example 1 Example 2 Example 3 Example 1 Example 2 Example 3 characteristic odor 2.8 2.5 3.0 4.8 3.5 3.8 characteristic taste 2.1 1.9 2.6 4.6 3.8 4.2 raw taste 3.2 3.4 3.6 5.2 4.2 4.5 sweetness 5.1 5.6 5.7 3.5 4.2 4.0 bitterness 1.5 0.8 1.4 3.5 2.8 3.0 astringency 1.4 1.2 2.2 2.4 2.6 2.3 duration of sweet 4.5 4.2 4.6 5.5 4.6 4.8 aftertaste duration of bitter 1.6 0.5 1.2 2.4 2.5 1.6 aftertaste duration of astringent 1.0 0.4 1.5 2.2 2.8 2.6 aftertaste characteristic aftertaste 2.8 2.0 3.0 3.5 3.8 3.9 overall consistency 4.2 4.1 4.6 5.8 5.5 5.2

CONCLUSION

(67) The test results of the content of mogroside V show that, the contents of mogroside V in the Siraitia grosvenori concentrated solutions obtained in Examples 1 to 3 are higher than those obtained in Comparative Examples 1 to 3 by 20.95% on average. Among them, the contents in Example 2 are 37.03%, 30.22%, and 26.06% higher than those in Comparative Examples 1 to 3, respectively. It is shown that the method for separating and purifying mogro side V by subcritical water desorption technology is superior to the prior art.

(68) The detection results of the multiple pesticide residues show that, plural pesticide residue indexes in the Siraitia grosvenori concentrated solutions of Examples 1 to 3 are lower than those of Comparative Examples 1 to 3. It is shown that the efficiency of the removal of multiple pesticide residues by subcritical water desorption technology is superior to the prior art.

(69) The results of the mouthfeel test experiment show that, the mouthfeel effects of Examples 1 to 3 are all superior to those of Comparative Examples 1 to 3, wherein the sweetness effect is significantly improved, and the indicators that reduce mouthfeel pleasure such as raw taste, bitterness, astringency are all significantly improved. It is shown that the mouthfeel of the mogroside V-containing Siraitia grosvenori concentrated solution separated and purified by subcritical water desorption technology is superior to the prior art.

(70) Although the present invention has been described in detail by general descriptions, specific embodiments, and tests, the present invention can be modified or improved on the basis of the present invention, which will be obvious to a person skilled in the art. Therefore, these modifications or improvements made without departing from the spirit of the present invention all fall within the protection scope of the present invention.

INDUSTRIAL APPLICABILITY

(71) The invention provides a method for separating and purifying mogroside V by subcritical water desorption technology, in which desorption is carried out on the macroporous adsorption resin enriched with mogroside V using water as solvent under a subcritical condition of water, to give an aqueous solution rich in mogro side V. The method provided by the invention improves the content of mogroside V in product, effectively removes bitter impurities and residual pesticides, greatly improves the mouthfeel adaptability of the product, improves the safety and quality of the product, reduces the processing steps and the use of the organic solvents employed in the prior art, and decreases total production costs. The method provided by the invention has good economic value and broad application prospect.