CN104431841A - Method for reducing carbendazim in fructus momordicae extract - Google Patents
Method for reducing carbendazim in fructus momordicae extract Download PDFInfo
- Publication number
- CN104431841A CN104431841A CN201410657496.XA CN201410657496A CN104431841A CN 104431841 A CN104431841 A CN 104431841A CN 201410657496 A CN201410657496 A CN 201410657496A CN 104431841 A CN104431841 A CN 104431841A
- Authority
- CN
- China
- Prior art keywords
- activated
- deionized water
- activated carbon
- extract
- fructus monordicae
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- JNPZQRQPIHJYNM-UHFFFAOYSA-N carbendazim Chemical compound C1=C[CH]C2=NC(NC(=O)OC)=NC2=C1 JNPZQRQPIHJYNM-UHFFFAOYSA-N 0.000 title claims abstract description 29
- TWFZGCMQGLPBSX-UHFFFAOYSA-N Carbendazim Natural products C1=CC=C2NC(NC(=O)OC)=NC2=C1 TWFZGCMQGLPBSX-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000006013 carbendazim Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 167
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 54
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000008367 deionised water Substances 0.000 claims abstract description 44
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 44
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 36
- GHBNZZJYBXQAHG-KUVSNLSMSA-N (2r,3r,4s,5s,6r)-2-[[(2r,3s,4s,5r,6r)-6-[[(3s,8s,9r,10r,11r,13r,14s,17r)-17-[(2r,5r)-5-[(2s,3r,4s,5s,6r)-4,5-dihydroxy-3-[(2r,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxy-6-[[(2r,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxy Chemical compound C([C@H]1O[C@H]([C@@H]([C@@H](O)[C@@H]1O)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)O[C@H](CC[C@@H](C)[C@@H]1[C@]2(C[C@@H](O)[C@@]3(C)[C@H]4C(C([C@@H](O[C@H]5[C@@H]([C@@H](O)[C@H](O)[C@@H](CO[C@H]6[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O6)O)O5)O)CC4)(C)C)=CC[C@H]3[C@]2(C)CC1)C)C(C)(C)O)O[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O GHBNZZJYBXQAHG-KUVSNLSMSA-N 0.000 claims abstract description 23
- TVJXHJAWHUMLLG-UHFFFAOYSA-N mogroside V Natural products CC(CCC(OC1OC(COC2OC(CO)C(O)C(O)C2OC3OC(CO)C(O)C(O)C3O)C(O)C(O)C1O)C(C)(C)O)C4CCC5(C)C6CC=C7C(CCC(OC8OC(COC9OC(CO)C(O)C(O)C9O)C(O)C(O)C8O)C7(C)C)C6(C)C(O)CC45C TVJXHJAWHUMLLG-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000007787 solid Substances 0.000 claims abstract description 18
- 238000005406 washing Methods 0.000 claims abstract description 13
- 150000003839 salts Chemical class 0.000 claims abstract description 9
- 229940023032 activated charcoal Drugs 0.000 claims description 40
- 229910052799 carbon Inorganic materials 0.000 claims description 18
- 238000010612 desalination reaction Methods 0.000 claims description 16
- 239000003480 eluent Substances 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 239000003518 caustics Substances 0.000 claims description 8
- 239000000919 ceramic Substances 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 8
- 238000001728 nano-filtration Methods 0.000 claims description 8
- 238000005554 pickling Methods 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 238000005507 spraying Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000000575 pesticide Substances 0.000 abstract description 6
- 238000012856 packing Methods 0.000 abstract 1
- 238000001694 spray drying Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 9
- 241001409321 Siraitia grosvenorii Species 0.000 description 8
- 235000011171 Thladiantha grosvenorii Nutrition 0.000 description 8
- 239000006071 cream Substances 0.000 description 7
- 239000008187 granular material Substances 0.000 description 7
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 7
- 238000005070 sampling Methods 0.000 description 6
- 239000011347 resin Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 229930189775 mogroside Natural products 0.000 description 3
- KYVIPFHNYCKOMQ-YMRJDYICSA-N (2r,3s,4s,5r,6r)-2-(hydroxymethyl)-6-[[(2r,3s,4s,5r,6s)-3,4,5-trihydroxy-6-[(3r,6r)-2-hydroxy-6-[(3s,8s,9r,10r,11r,13r,14s,17r)-11-hydroxy-4,4,9,13,14-pentamethyl-3-[(2r,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxy-2,3,7,8,10,11,12,15,16,1 Chemical compound C([C@H]1O[C@H]([C@@H]([C@@H](O)[C@@H]1O)O)O[C@H](CC[C@@H](C)[C@@H]1[C@]2(C[C@@H](O)[C@@]3(C)[C@H]4C(C([C@@H](O[C@H]5[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O5)O)CC4)(C)C)=CC[C@H]3[C@]2(C)CC1)C)C(C)(C)O)O[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O KYVIPFHNYCKOMQ-YMRJDYICSA-N 0.000 description 2
- QATISCJMIITVAB-UHFFFAOYSA-N 2-[[17-[5-[4,5-dihydroxy-6-(hydroxymethyl)-3-[3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxyoxan-2-yl]oxy-6-hydroxy-6-methylheptan-2-yl]-11-hydroxy-4,4,9,13,14-pentamethyl-2,3,7,8,10,11,12,15,16,17-decahydro-1h-cyclopenta[a]phenanthren-3-yl]oxy]-6-(hydro Chemical compound C1CC2(C)C3CC=C(C(C(OC4C(C(O)C(O)C(CO)O4)O)CC4)(C)C)C4C3(C)C(O)CC2(C)C1C(C)CCC(C(C)(C)O)OC1OC(CO)C(O)C(O)C1OC1OC(CO)C(O)C(O)C1O QATISCJMIITVAB-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- KYVIPFHNYCKOMQ-UHFFFAOYSA-N Mogroside III Natural products C1CC2(C)C3CC=C(C(C(OC4C(C(O)C(O)C(CO)O4)O)CC4)(C)C)C4C3(C)C(O)CC2(C)C1C(C)CCC(C(C)(C)O)OC(C(C(O)C1O)O)OC1COC1OC(CO)C(O)C(O)C1O KYVIPFHNYCKOMQ-UHFFFAOYSA-N 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- LTDANPHZAHSOBN-IPIJHGFVSA-N (2R,3R,4S,5S,6R)-2-[[(2R,3S,4S,5R,6R)-6-[[(3S,8R,9R,10S,11R,13R,14S,17R)-17-[(2R,5R)-5-[(2S,3R,4S,5S,6R)-4,5-dihydroxy-3-[(2S,3R,4S,5S,6R)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxy-6-[[(2S,3R,4S,5S,6R)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxymethyl]oxan-2-yl]oxy-6-hydroxy-6-methylheptan-2-yl]-11-hydroxy-4,4,9,13,14-pentamethyl-2,3,7,8,10,11,12,15,16,17-decahydro-1H-cyclopenta[a]phenanthren-3-yl]oxy]-3,4-dihydroxy-5-[(2S,3R,4S,5S,6R)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxyoxan-2-yl]methoxy]-6-(hydroxymethyl)oxane-3,4,5-triol Chemical compound C([C@H]1O[C@H]([C@@H]([C@@H](O)[C@@H]1O)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)O[C@H](CC[C@@H](C)[C@@H]1[C@]2(C[C@@H](O)[C@@]3(C)[C@@H]4C(C([C@@H](O[C@H]5[C@@H]([C@@H](O)[C@H](O)[C@@H](CO[C@H]6[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O6)O)O5)O[C@H]5[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O5)O)CC4)(C)C)=CC[C@@H]3[C@]2(C)CC1)C)C(C)(C)O)O[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O LTDANPHZAHSOBN-IPIJHGFVSA-N 0.000 description 1
- 229930192771 11-oxomogroside Natural products 0.000 description 1
- 241000219104 Cucurbitaceae Species 0.000 description 1
- -1 Cucurbitane glycosides compounds Chemical class 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 240000005373 Panax quinquefolius Species 0.000 description 1
- 241001409305 Siraitia Species 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229930182478 glucoside Natural products 0.000 description 1
- 150000008131 glucosides Chemical class 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 235000021096 natural sweeteners Nutrition 0.000 description 1
- 239000000447 pesticide residue Substances 0.000 description 1
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 1
- 230000005070 ripening Effects 0.000 description 1
- 229930182490 saponin Natural products 0.000 description 1
- 150000007949 saponins Chemical class 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
Abstract
The invention relates to a method for reducing carbendazim in a fructus momordicae extract. The method comprises the following steps: taking the fructus momordicae extract, dissolving with deionized water, adjusting the pH to be 2-4 with 10% of hydrochloric acid, and thus obtaining a to-be-treated water solution of the fructus momordicae extract; taking activated carbon, and packing by a column; firstly, washing the activated carbon column with 1% of sodium hydroxide, then washing the column with the deionized water, and washing the activated carbon column with 1% of hydrochloric acid; finally washing the activated carbon column with the deionized water, so as to obtain processed activated carbon column; enabling the to-be-treated water solution of the fructus momordicae extract to flow through the activated carbon column, feeding a solution, and then washing the activated carbon column with the deionized water, mixing and collecting the eluant; adjusting the pH to be 5 with 10% of sodium hydroxide; and removing salt from the eluant of which the pH is adjusted, concentrating into 5% of solid matter, concentrating into 30% of solid matter in vacuum, and carrying out spray drying, so as to obtain an extract of which the carbendazim content is lower than 0.01mg/kg and the mogroside V content is higher than 40%. According to the method disclosed by the invention, the pesticide carbendazim content in the fructus momordicae extract can be lower than 0.01mg/kg; and the mogroside V content is higher than 40%.
Description
Technical field
The present invention relates to a kind of method reducing carbendazim in Fructus Monordicae extract, belong to medicinal chemistry arts.
Background technology
Momordica grosvenori is the famous special product in Guangxi, it is the ripening fruits of Curcurbitaceae (Cucurbitaceae) Genus Siraitia Merr (Siraitia grosvenorii (SwingIe) C.Jeffrey), is mainly the counties such as the Yongfu of northern Guangxi, Lingui, Xingan and Long Sheng main product.Up to now, scholar has been separated and has identified multiple Momordica grosvenori saponin monomer from Lo Han Guo fruit, respectively: Momordica grosvenori IV (mogrosideIV), mogroside V (mogroside V), mogroside III (mogroside III), mogroside lIE (mogrosid II E), mogroside III E (mogroside III E), mogroside V I (mogroside VI), mogroside A (mogrosideA), Momordica grosvenori Neogroside (neomogroside), Simon glucoside I (siamenside I), 11-is oxidized mogroside (11-oxomogroside), the Cucurbitane glycosides compounds such as Momordica grosvenori glycol benzoate (mogloester).Wherein mogroside V is that in Momordica grosvenori, content is high, sugariness large (sugariness is sucrose 256-344 times), has the features such as sugariness is high, heat is low, Heat stability is good.With the Fructus Monordicae extract that modernization of Chinese medicine technology is produced, can be used as natural sweetener, export to foreign countries in a large number every year.
In recent years, along with states such as Europe, Japan, the U.S., in succession most of Chinese medical extract Pesticide Residue standard is reduced to 0.01mg/kg from 0.05mg/kg.And the GB27630-2012 " Pesticide MRL " that Current Domestic uses, regulation is applicable to extract limitation at 0.1-0.2mg/kg.Foreign standard is higher than domestic requirements more than 10 times, and the difficulty that Fructus Monordicae extract is exported strengthens, and Momordica grosvenori persticide residue risk of exceeding criterion strengthens.Wherein pesticide carbendazim is one of agricultural chemicals wherein the most easily exceeded standard, and it is general more than 5 times to exceed standard.Therefore, study a kind of method effectively reducing carbendazim residues of pesticides, to the outlet ensureing Fructus Monordicae extract, there is very urgent meaning.
Present stage, also do not find that in a Fructus Monordicae extract, carbendazim is reduced to 0.01mg/kg reported in literature, the research of this patent, filled up the blank of this one side.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method reducing carbendazim in Fructus Monordicae extract, and the present invention can make Fructus Monordicae extract Pesticides carbendazim content lower than 0.01mg/kg, and mogroside V content is higher than 40%.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of method reducing carbendazim in Fructus Monordicae extract, comprising:
1) Fructus Monordicae extract (Guilin Laiyin Biotechnology Co., Ltd. commercially available prod is got, wherein, carbendazim content 0.085mg/kg, mogroside V content 41.21%), dissolve by the deionized water stirring at normal temperature of Fructus Monordicae extract 10 times of weight, adjust pH to 2-4 with 10% hydrochloric acid (analyzing pure), obtain the pending aqueous solution of Fructus Monordicae extract;
2) active carbon (purchased from American CALGON company is got, Filtrasorb-200, coarse granule type) fill post, first use 1% caustic washing activated-charcoal column, then being washed to efflux pH by deionized water is 7-8, use 1% salt pickling activated-charcoal column again, being finally washed to efflux pH by deionized water is 6-7, obtains the activated-charcoal column handled well;
3) pending for Fructus Monordicae extract water solution flow is crossed activated-charcoal column, flow velocity is 0.5BV/H, after having entered liquid, washes activated-charcoal column by deionized water, and flow velocity is 0.5BV/H, merges and collects eluent, adjusts pH to 5 with 10% NaOH;
4) the eluent desalination nanofiltration ceramic membrane desalination, concentrated of pH will be mixed up, be concentrated to 5% solid content (mass fraction), with Vacuum Concentration cream to solid content 30% (mass fraction), spraying dry, obtain carbendazim content lower than 0.01mg/kg, mogroside V content higher than 40% extract.
On the basis of technique scheme, the present invention can also do following improvement.
Further, 2) in, the consumption of described active carbon counts Fructus Monordicae extract in mass ratio: active carbon=2:1.
Further, 2) in, the consumption of described 1% NaOH is 2 times of quality of activated carbon.
Further, 2) in, the consumption of described 1% hydrochloric acid is 2 times of quality of activated carbon.
Further, 3) in, the consumption of described deionized water is 5 times of quality of activated carbon.
The invention has the beneficial effects as follows:
The present invention can make Fructus Monordicae extract Pesticides carbendazim content lower than 0.01mg/kg, and mogroside V content is higher than 40%.
Detailed description of the invention
Be described principle of the present invention and feature below, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment 1
1) Fructus Monordicae extract (Guilin Laiyin Biotechnology Co., Ltd. commercially available prod is got, wherein, carbendazim content 0.085mg/kg, mogroside V content 41.21%) 200g, dissolve by 2000ml deionized water stirring at normal temperature, be 2.0 with 10% hydrochloric acid (analyzing pure) adjust pH, obtain the pending aqueous solution of Fructus Monordicae extract;
2) active carbon (purchased from American CALGON company is got, Filtrasorb-200, coarse granule type), mass ratio fills post by (Fructus Monordicae extract: active carbon=2:1), first use 1% caustic washing activated-charcoal column, the consumption of 1% NaOH is 2 times of quality of activated carbon, then being washed to efflux pH by deionized water is 7-8, use 1% salt pickling activated-charcoal column again, the consumption of 1% hydrochloric acid is 2 times of quality of activated carbon, finally being washed to efflux pH by deionized water is 6-7, obtains the activated-charcoal column handled well;
3) pending for Fructus Monordicae extract water solution flow is crossed activated-charcoal column, flow velocity is 0.5BV/H, after having entered liquid, wash activated-charcoal column by deionized water, the consumption of deionized water is 5 times of quality of activated carbon, and flow velocity is 0.5BV/H, merge and collect eluent, adjust pH to 5 with 10% NaOH;
4) the eluent desalination nanofiltration ceramic membrane desalination, concentrated of pH will be mixed up, be concentrated to 5% solid content (mass fraction), with Vacuum Concentration cream to solid content 30% (mass fraction), spraying dry, yield 96.21%, detect through Agilent 1100 type high performance liquid chromatograph (Agilent Science and Technology Ltd. of the U.S.) sampling, the carbendazim 0.0095mg/kg of extract, mogroside V content 42.35%.
Embodiment 2
1) Fructus Monordicae extract (Guilin Laiyin Biotechnology Co., Ltd. commercially available prod is got, wherein, carbendazim content 0.085mg/kg, mogroside V content 41.21%) 200g, dissolve by 2000ml deionized water stirring at normal temperature, be 2.5 with 10% hydrochloric acid (analyzing pure) adjust pH, obtain the pending aqueous solution of Fructus Monordicae extract;
2) active carbon (purchased from American CALGON company is got, Filtrasorb-200, coarse granule type), mass ratio fills activated-charcoal column by (Fructus Monordicae extract: active carbon=2:1), first use 1% caustic washing activated-charcoal column, the consumption of 1% NaOH is 2 times of quality of activated carbon, then being washed to efflux pH by deionized water is 7-8, use 1% salt pickling resin column again, the consumption of 1% hydrochloric acid is 2 times of quality of activated carbon, finally being washed to efflux pH by deionized water is 6-7, obtains the activated-charcoal column handled well;
3) pending for Fructus Monordicae extract water solution flow is crossed activated-charcoal column, flow velocity is 0.5BV/H, after having entered liquid, wash activated-charcoal column by deionized water, the consumption of deionized water is 5 times of quality of activated carbon, and flow velocity is 0.5BV/H, merge and collect eluent, adjust pH to 5 with 10% NaOH;
4) the eluent desalination nanofiltration ceramic membrane desalination, concentrated of pH will be mixed up, be concentrated to 5% solid content (mass fraction), with Vacuum Concentration cream to solid content 30% (mass fraction), spraying dry, yield 94.28%, detect through Agilent 1100 type high performance liquid chromatograph (Agilent Science and Technology Ltd. of the U.S.) sampling, the carbendazim content 0.0084mg/kg of extract, mogroside V content 43.61%.
Embodiment 3
1) Fructus Monordicae extract (Guilin Laiyin Biotechnology Co., Ltd. commercially available prod is got, wherein, carbendazim content 0.085mg/kg, mogroside V content 41.21%) 200g, dissolve by 2000ml deionized water stirring at normal temperature, adjust pH to be 3.0 with 10% hydrochloric acid (analyzing pure), obtain the pending aqueous solution of Fructus Monordicae extract;
2) active carbon (purchased from American CALGON company is got, Filtrasorb-200, coarse granule type), mass ratio fills activated-charcoal column by (Fructus Monordicae extract: active carbon=2:1), first use 1% caustic washing activated-charcoal column, the consumption of 1% NaOH is 2 times of quality of activated carbon, then being washed to efflux pH by deionized water is 7-8, use 1% salt pickling resin column again, the consumption of 1% hydrochloric acid is 2 times of quality of activated carbon, finally being washed to efflux pH by deionized water is 6-7, obtains the activated-charcoal column handled well;
3) pending for Fructus Monordicae extract water solution flow is crossed activated-charcoal column, flow velocity is 0.5BV/H, after having entered liquid, wash activated-charcoal column by deionized water, the consumption of deionized water is 5 times of quality of activated carbon, and flow velocity is 0.5BV/H, merge and collect eluent, adjust pH to 5 with 10% NaOH;
4) the eluent desalination nanofiltration ceramic membrane desalination, concentrated of pH will be mixed up, be concentrated to 5% solid content (mass fraction), with Vacuum Concentration cream to solid content 30% (mass fraction), spraying dry, yield 96.87%, detect through Agilent 1100 type high performance liquid chromatograph (Agilent Science and Technology Ltd. of the U.S.) sampling, the carbendazim 0.0055mg/kg of extract, mogroside V content 41.73%.
Embodiment 4
1) Fructus Monordicae extract (Guilin Laiyin Biotechnology Co., Ltd. commercially available prod is got, wherein, carbendazim content 0.085mg/kg, mogroside V content 41.21%) 200g, dissolve by 2000ml deionized water stirring at normal temperature, adjust pH to be 3.5 with 10% hydrochloric acid (analyzing pure), obtain the pending aqueous solution of Fructus Monordicae extract;
2) active carbon (purchased from American CALGON company is got, Filtrasorb-200, coarse granule type), mass ratio fills activated-charcoal column by (Fructus Monordicae extract: active carbon=2:1), first use 1% caustic washing activated-charcoal column, the consumption of 1% NaOH is 2 times of quality of activated carbon, then being washed to efflux pH by deionized water is 7-8, use 1% salt pickling resin column again, the consumption of 1% hydrochloric acid is 2 times of quality of activated carbon, finally being washed to efflux pH by deionized water is 6-7, obtains the activated-charcoal column handled well;
3) pending for Fructus Monordicae extract water solution flow is crossed activated-charcoal column, flow velocity is 0.5BV/H, after having entered liquid, wash activated-charcoal column by deionized water, the consumption of deionized water is 5 times of quality of activated carbon, and flow velocity is 0.5BV/H, merge and collect eluent, adjust pH to 5 with 10% NaOH;
4) the eluent desalination nanofiltration ceramic membrane desalination, concentrated of pH will be mixed up, be concentrated to 5% solid content (mass fraction), with Vacuum Concentration cream to solid content 30% (mass fraction), spraying dry, yield 95.45%, detect through Agilent 1100 type high performance liquid chromatograph (Agilent Science and Technology Ltd. of the U.S.) sampling, the carbendazim 0.0071mg/kg of extract, mogroside V content 42.33%.
Embodiment 5
1) Fructus Monordicae extract (Guilin Laiyin Biotechnology Co., Ltd. commercially available prod is got, wherein, carbendazim content 0.085mg/kg, mogroside V content 41.21%) 200g, dissolve by 2000ml deionized water stirring at normal temperature, adjust pH to be 3.8 with 10% hydrochloric acid (analyzing pure), obtain the pending aqueous solution of Fructus Monordicae extract;
2) active carbon (purchased from American CALGON company is got, Filtrasorb-200, coarse granule type), mass ratio fills activated-charcoal column by (Fructus Monordicae extract: active carbon=2:1), first use 1% caustic washing activated-charcoal column, the consumption of 1% NaOH is 2 times of quality of activated carbon, then being washed to efflux pH by deionized water is 7-8, use 1% salt pickling resin column again, the consumption of 1% hydrochloric acid is 2 times of quality of activated carbon, finally being washed to efflux pH by deionized water is 6-7, obtains the activated-charcoal column handled well;
3) pending for Fructus Monordicae extract water solution flow is crossed activated-charcoal column, flow velocity is 0.5BV/H, after having entered liquid, wash activated-charcoal column by deionized water, the consumption of deionized water is 5 times of quality of activated carbon, and flow velocity is 0.5BV/H, merge and collect eluent, adjust pH to 5 with 10% NaOH;
4) the eluent desalination nanofiltration ceramic membrane desalination, concentrated of pH will be mixed up, be concentrated to 5% solid content (mass fraction), with Vacuum Concentration cream to solid content 30% (mass fraction), spraying dry, yield 95.89%, detect through Agilent 1100 type high performance liquid chromatograph (Agilent Science and Technology Ltd. of the U.S.) sampling, the carbendazim 0.0078mg/kg of extract, mogroside V content 42.17%.
Embodiment 6
1) Fructus Monordicae extract (Guilin Laiyin Biotechnology Co., Ltd. commercially available prod is got, wherein, carbendazim content 0.085mg/kg, mogroside V content 41.21%) 200g, dissolve by 2000ml deionized water stirring at normal temperature, adjust pH to be 4.0 with 10% hydrochloric acid (analyzing pure), obtain the pending aqueous solution of Fructus Monordicae extract;
2) active carbon (purchased from American CALGON company is got, Filtrasorb-200, coarse granule type), mass ratio fills activated-charcoal column by (Fructus Monordicae extract: active carbon=2:1), first use 1% caustic washing activated-charcoal column, the consumption of 1% NaOH is 2 times of quality of activated carbon, then being washed to efflux pH by deionized water is 7-8, use 1% salt pickling resin column again, the consumption of 1% hydrochloric acid is 2 times of quality of activated carbon, finally being washed to efflux pH by deionized water is 6-7, obtains the activated-charcoal column handled well;
3) pending for Fructus Monordicae extract water solution flow is crossed activated-charcoal column, flow velocity is 0.5BV/H, after having entered liquid, wash activated-charcoal column by deionized water, the consumption of deionized water is 5 times of quality of activated carbon, and flow velocity is 0.5BV/H, merge and collect eluent, adjust pH to 5 with 10% NaOH;
4) the eluent desalination nanofiltration ceramic membrane desalination, concentrated of pH will be mixed up, be concentrated to 5% solid content (mass fraction), with Vacuum Concentration cream to solid content 30% (mass fraction), spraying dry, yield 96.24%, detect through Agilent 1100 type high performance liquid chromatograph (Agilent Science and Technology Ltd. of the U.S.) sampling, the carbendazim 0.0087mg/kg of extract, mogroside V content 41.37%.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. reduce a method for carbendazim in Fructus Monordicae extract, it is characterized in that, comprising:
1) get Fructus Monordicae extract, dissolve by the deionized water stirring at normal temperature of Fructus Monordicae extract 10 times of weight, adjust pH to 2-4 with 10% hydrochloric acid, obtain the pending aqueous solution of Fructus Monordicae extract;
2) get active carbon dress post, first use 1% caustic washing activated-charcoal column, being then washed to efflux pH by deionized water is 7-8, then uses 1% salt pickling activated-charcoal column, and being finally washed to efflux pH by deionized water is 6-7, obtains the activated-charcoal column handled well;
3) pending for Fructus Monordicae extract water solution flow is crossed activated-charcoal column, flow velocity is 0.5BV/H, after having entered liquid, washes activated-charcoal column by deionized water, and flow velocity is 0.5BV/H, merges and collects eluent, adjusts pH to 5 with 10% NaOH;
4) will the eluent desalination nanofiltration ceramic membrane desalination, concentrated of pH be mixed up, and be concentrated to 5% solid content, with being concentrated in vacuo to solid content 30%, spraying dry, obtaining carbendazim content lower than 0.01mg/kg, mogroside V content higher than 40% extract.
2. method according to claim 1, is characterized in that, 2) in, the consumption of described active carbon counts Fructus Monordicae extract in mass ratio: active carbon=2:1.
3. method according to claim 1, is characterized in that, 2) in, the consumption of described 1% NaOH is 2 times of quality of activated carbon.
4. method according to claim 1, is characterized in that, 2) in, the consumption of described 1% hydrochloric acid is 2 times of quality of activated carbon.
5. method according to claim 1, is characterized in that, 3) in, the consumption of described deionized water is 5 times of quality of activated carbon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410657496.XA CN104431841B (en) | 2014-11-18 | 2014-11-18 | A kind of method of carbendazim in reduction Fructus Monordicae extract |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410657496.XA CN104431841B (en) | 2014-11-18 | 2014-11-18 | A kind of method of carbendazim in reduction Fructus Monordicae extract |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104431841A true CN104431841A (en) | 2015-03-25 |
| CN104431841B CN104431841B (en) | 2017-09-19 |
Family
ID=52879189
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410657496.XA Active CN104431841B (en) | 2014-11-18 | 2014-11-18 | A kind of method of carbendazim in reduction Fructus Monordicae extract |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104431841B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106306991A (en) * | 2016-08-23 | 2017-01-11 | 湖南华诚生物资源股份有限公司 | Method for removing pesticide residues and plasticizer from fructus momordicae extract at the same time |
| CN107708440A (en) * | 2015-05-29 | 2018-02-16 | 莎罗雅株式会社 | Fructus Monordicae extract without agricultural chemicals and preparation method thereof |
| WO2018157335A1 (en) * | 2017-03-01 | 2018-09-07 | 桂林莱茵生物科技股份有限公司 | Method for increasing content of mogroside v in siraitia grosvenorii suspended cells |
| WO2018196476A1 (en) * | 2017-04-25 | 2018-11-01 | 广西甙元植物制品有限公司 | Process for preparing decolored concentrated fresh momordica grosvenori juice |
| CN112028960A (en) * | 2020-08-13 | 2020-12-04 | 赣州禾绿康健生物技术有限公司 | Low-cost acidification removal equipment and process for ginsenoside extract carbendazim |
| CN113680102A (en) * | 2021-08-27 | 2021-11-23 | 湖南绿蔓生物科技股份有限公司 | Method for preparing plant extract without exogenous pollutant |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1119407A (en) * | 1993-02-16 | 1996-03-27 | 普罗克特和甘保尔公司 | Sweet beverages and sweetening compositions |
| CN101007042A (en) * | 2007-02-06 | 2007-08-01 | 桂林莱茵生物科技股份有限公司 | A preparation method of debittered and discolored siraitia grosvenorii extracts |
| CN101570352A (en) * | 2009-05-28 | 2009-11-04 | 张金松 | Water purifier active carbon filter element provided with folding protective layer |
| CN101711926A (en) * | 2009-11-24 | 2010-05-26 | 天津市尖峰天然产物研究开发有限公司 | Method for removing residual pesticide in plant extract |
| CN103402374A (en) * | 2011-01-28 | 2013-11-20 | 泰特&莱尔组分美国公司 | Rebaudioside-mogroside V blends |
| US20140044843A1 (en) * | 2012-08-07 | 2014-02-13 | Guilin Gfs Bio-Technology Co. Limited | Methods of producing sweet juice compositions |
-
2014
- 2014-11-18 CN CN201410657496.XA patent/CN104431841B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1119407A (en) * | 1993-02-16 | 1996-03-27 | 普罗克特和甘保尔公司 | Sweet beverages and sweetening compositions |
| CN101007042A (en) * | 2007-02-06 | 2007-08-01 | 桂林莱茵生物科技股份有限公司 | A preparation method of debittered and discolored siraitia grosvenorii extracts |
| CN101570352A (en) * | 2009-05-28 | 2009-11-04 | 张金松 | Water purifier active carbon filter element provided with folding protective layer |
| CN101711926A (en) * | 2009-11-24 | 2010-05-26 | 天津市尖峰天然产物研究开发有限公司 | Method for removing residual pesticide in plant extract |
| CN103402374A (en) * | 2011-01-28 | 2013-11-20 | 泰特&莱尔组分美国公司 | Rebaudioside-mogroside V blends |
| US20140044843A1 (en) * | 2012-08-07 | 2014-02-13 | Guilin Gfs Bio-Technology Co. Limited | Methods of producing sweet juice compositions |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107708440A (en) * | 2015-05-29 | 2018-02-16 | 莎罗雅株式会社 | Fructus Monordicae extract without agricultural chemicals and preparation method thereof |
| JPWO2016194809A1 (en) * | 2015-05-29 | 2018-03-01 | サラヤ株式会社 | Luohan fruit extract containing no pesticide and method for preparing the same |
| AU2016271765B2 (en) * | 2015-05-29 | 2019-05-09 | Saraya Co., Ltd. | Agrochemical-free siraitia grosvenorii extract, and method for preparing same |
| JP2019165728A (en) * | 2015-05-29 | 2019-10-03 | サラヤ株式会社 | Momordicae fruit extract containing no agricultural chemical, and preparation method thereof |
| CN106306991A (en) * | 2016-08-23 | 2017-01-11 | 湖南华诚生物资源股份有限公司 | Method for removing pesticide residues and plasticizer from fructus momordicae extract at the same time |
| CN106306991B (en) * | 2016-08-23 | 2020-06-05 | 湖南华诚生物资源股份有限公司 | Method for simultaneously removing pesticide residues and plasticizer in fructus momordicae extract |
| WO2018157335A1 (en) * | 2017-03-01 | 2018-09-07 | 桂林莱茵生物科技股份有限公司 | Method for increasing content of mogroside v in siraitia grosvenorii suspended cells |
| WO2018196476A1 (en) * | 2017-04-25 | 2018-11-01 | 广西甙元植物制品有限公司 | Process for preparing decolored concentrated fresh momordica grosvenori juice |
| CN112028960A (en) * | 2020-08-13 | 2020-12-04 | 赣州禾绿康健生物技术有限公司 | Low-cost acidification removal equipment and process for ginsenoside extract carbendazim |
| CN113680102A (en) * | 2021-08-27 | 2021-11-23 | 湖南绿蔓生物科技股份有限公司 | Method for preparing plant extract without exogenous pollutant |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104431841B (en) | 2017-09-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104431841A (en) | Method for reducing carbendazim in fructus momordicae extract | |
| CN107033209A (en) | It is a kind of at the same extract the method without the residual mogroside of agriculture and water-soluble dietary fiber | |
| CN102526161B (en) | Preparation method for high-activity lepidium meyenii extract | |
| CN106967142B (en) | Method that is a kind of while extracting momordica glycoside V, VI and 11-O base glycosides V | |
| CN102816193B (en) | A kind of method of resin column method extraction purification steviol glycoside from stevia rebaudiana water extract of connecting | |
| CN101747388B (en) | Method for simultaneously extracting punicalagin and ellagic acid from pomegranate bark | |
| CN1854149A (en) | Extraction of Momordica grosvenori beet aglucone V | |
| CN106220747B (en) | Ultrasonic assistant Vacuum cavitation extracts the preparation technology of Dendrobium officinale polysaccharide and its instant powder | |
| CN105267275B (en) | Method for extracting flavone from chrysanthemum | |
| CN105032282A (en) | Preparation method for high-purity gleditsia sinensis natural surfactant | |
| CN109265346A (en) | The industrialized utilization method and its chlorogenic acid and steviol glycoside of a kind of STEVIA REBAUDIANA | |
| CN109394811A (en) | The method and its marigold flavones of marigold flavones are extracted in a kind of industrialization | |
| CN104610417B (en) | A kind of method of extracting ursolic acid and oleanolic acid from hawthorn | |
| CN105601694B (en) | A method of extraction ginsenoside Rg 5 | |
| CN103275175B (en) | The preparation method of dandelion small molecule glycoprotein | |
| CN104366165A (en) | Preparation method of total oil tea saponins | |
| CN104926767A (en) | Method of purification preparation of citrus flavones by adopting macroporous adsorption resin | |
| CN102702286A (en) | Method for separating and purifying aucubin from leaves of eucommia ulmoides oliv with NKA-2 macroporous adsorption resin | |
| CN101987856B (en) | Preparation method of anthocyanin monomer cornflower-3-glucoside | |
| CN106432394A (en) | Method for extracting siraitia grosvenorii total saponin in siraitia grosvenorii | |
| CN106543158A (en) | A kind of method that chimonin is extracted from Folium mangiferae | |
| CN107383126A (en) | A kind of rebaudioside dynamic microwave adverse current extraction production technology | |
| CN106117284A (en) | The method of six kinds of iridoid glycoside constituents in Extraction and enrichment Flos Lonicerae while of a kind of | |
| CN102772452A (en) | Method for producing ultra-low-acid ginkgo leaf extract | |
| JP2017210443A (en) | Method of extracting triterpenoid, and method of separating triterpenoid and carotenoid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A method for reducing carbendazim in Momordica grosvenorii extract Effective date of registration: 20231212 Granted publication date: 20170919 Pledgee: China Postal Savings Bank Co.,Ltd. Guilin Branch Guangxi Zhuang Autonomous Region Pledgor: GUILIN LAYN NATURAL INGREDIENTS Corp. Registration number: Y2023980071101 |