CN104431841B - A kind of method of carbendazim in reduction Fructus Monordicae extract - Google Patents
A kind of method of carbendazim in reduction Fructus Monordicae extract Download PDFInfo
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- CN104431841B CN104431841B CN201410657496.XA CN201410657496A CN104431841B CN 104431841 B CN104431841 B CN 104431841B CN 201410657496 A CN201410657496 A CN 201410657496A CN 104431841 B CN104431841 B CN 104431841B
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- TWFZGCMQGLPBSX-UHFFFAOYSA-N Carbendazim Natural products C1=CC=C2NC(NC(=O)OC)=NC2=C1 TWFZGCMQGLPBSX-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000006013 carbendazim Substances 0.000 title claims abstract description 29
- 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
- 238000000034 method Methods 0.000 title claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 181
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229940023032 activated charcoal Drugs 0.000 claims abstract description 45
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000008367 deionised water Substances 0.000 claims abstract description 29
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 29
- 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
- 238000010612 desalination reaction Methods 0.000 claims abstract description 17
- 239000003480 eluent Substances 0.000 claims abstract description 12
- 238000005554 pickling Methods 0.000 claims abstract description 9
- 150000003839 salts Chemical class 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 239000003518 caustics Substances 0.000 claims abstract description 8
- 239000000919 ceramic Substances 0.000 claims description 8
- 238000002242 deionisation method Methods 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 8
- 238000001728 nano-filtration Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000001694 spray drying Methods 0.000 claims description 2
- 238000000605 extraction Methods 0.000 claims 1
- 239000000575 pesticide Substances 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 description 12
- 241001409321 Siraitia grosvenorii Species 0.000 description 10
- 235000011171 Thladiantha grosvenorii Nutrition 0.000 description 8
- 235000021028 berry Nutrition 0.000 description 7
- 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
- 238000001514 detection method Methods 0.000 description 6
- 238000010828 elution Methods 0.000 description 6
- 238000005070 sampling Methods 0.000 description 6
- 239000003643 water by type Substances 0.000 description 6
- 239000011347 resin Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 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 4
- 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 4
- 235000013399 edible fruits Nutrition 0.000 description 3
- 229930182478 glucoside Natural products 0.000 description 3
- 150000008131 glucosides Chemical class 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 239000003905 agrochemical Substances 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
- XJIPREFALCDWRQ-UYQGGQRHSA-N (2r,3r,4s,5s,6r)-2-[[(2r,3s,4s,5r,6s)-3,4-dihydroxy-6-[(3r,6r)-2-hydroxy-6-[(3s,8s,9r,10r,11r,13r,14s,17r)-11-hydroxy-4,4,9,13,14-pentamethyl-3-[(2s,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxy-2,3,7,8,10,11,12,15,16,17-decahydro-1h-cyclop 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)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 XJIPREFALCDWRQ-UYQGGQRHSA-N 0.000 description 1
- 229930192771 11-oxomogroside Natural products 0.000 description 1
- 241000219104 Cucurbitaceae Species 0.000 description 1
- -1 Cucurbitane glycosides Chemical class 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 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
- 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
- 150000001875 compounds Chemical class 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 235000021096 natural sweeteners Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 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
- XJIPREFALCDWRQ-UHFFFAOYSA-N siamenoside I 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)OC2C(C(O)C(O)C(CO)O2)O)OC1COC1OC(CO)C(O)C(O)C1O XJIPREFALCDWRQ-UHFFFAOYSA-N 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
Landscapes
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Medicines Containing Plant Substances (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Saccharide Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention relates to a kind of method for reducing carbendazim in Fructus Monordicae extract, including：Fructus Monordicae extract is taken, with deionized water dissolving, adjusts pH to 24 with 10% hydrochloric acid, obtains Fructus Monordicae extract accessing pending water solution；Take activated carbon to fill post, first with 1% caustic washing activated-charcoal column, post is then washed with deionized water, then with 1% salt pickling activated-charcoal column, activated-charcoal column is finally washed with deionized water, the activated-charcoal column handled well；Fructus Monordicae extract accessing pending water solution is flowed through into activated-charcoal column, entered after decoction, activated-charcoal column is washed with deionized water, merges and collects eluent, pH to 5 is adjusted with 10% sodium hydroxide；PH eluent desalination will be mixed up, 5% solid content is concentrated to, with solid content 30% is concentrated in vacuo to, be spray-dried, carbendazim content is obtained less than 0.01mg/kg, mogroside V content is higher than 40% extract.The inventive method can make Fructus Monordicae extract Pesticides carbendazim content be less than 0.01mg/kg, and mogroside V content is higher than 40%.
Description
Technical field
The present invention relates to a kind of method for reducing carbendazim in Fructus Monordicae extract, belong to medicinal chemistry arts.
Background technology
Momordica grosvenori is the famous special product in Guangxi, and it is Curcurbitaceae (Cucurbitaceae) Genus Siraitia Merr (Siraitia
Grosvenorii (SwingIe) C.Jeffrey) ripening fruits, main product predominantly northern Guangxi Yongfu, Lingui, Xingan
With Long Shengdeng counties.So far, scholar separates from Lo Han Guo fruit and identifies a variety of Momordica grosvenori saponin monomers, respectively
It is：Momordica grosvenori IV (mogrosideIV), mogroside V (mogroside V), mogroside III (mogroside III), arhat
Fruit glucoside lIE (mogrosid II E), the E of mogroside III (E of mogroside III), mogroside V I (mogroside VI), arhat
Fruit glucoside A (mogrosideA), Momordica grosvenori Neogroside (neomogroside), siamenoside I (siamenside I), 11- oxidation arhats
The Cucurbitane glycosides class compounds such as fruit glucoside (11-oxomogroside), Momordica grosvenori glycol benzoate (mogloester).Its
Middle mogroside V is big (sugariness is 256-344 times of sucrose) for content height, sugariness in Momordica grosvenori, with sugariness is high, heat is low, heat
The features such as stability is good.The Fructus Monordicae extract produced with modernization of Chinese medicine technology, can be annual big as natural sweetener
Amount exports to foreign countries.
In recent years, with states such as Europe, Japan, the U.S., in succession most of Chinese medical extract Pesticide Residue standard
0.01mg/kg is reduced to from 0.05mg/kg.And the GB27630-2012 that Current Domestic is used《Pesticide maximum residual
Limitation》, regulation is suitable for extract limitation in 0.1-0.2mg/kg.Foreign standard is higher than domestic requirements more than 10 times so that sieve
The difficulty of Chinese berry extract outlet is increased, and Momordica grosvenori persticide residue risk of exceeding criterion is increased.Wherein pesticide carbendazim is wherein most
Easily one of exceeded agricultural chemicals, and exceeded general more than 5 times.Therefore, to effectively reduce carbendazim agricultural chemicals residual for research one kind
The method stayed, the outlet to ensureing Fructus Monordicae extract, with very urgent meaning.
At this stage, it has not been found that carbendazim in Fructus Monordicae extract is reduced to 0.01mg/kg reported in literature, this patent
Research, filled up the blank of this aspect.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of method for reducing carbendazim in Fructus Monordicae extract, this hair
Bright that Fructus Monordicae extract Pesticides carbendazim content can be made to be less than 0.01mg/kg, mogroside V content is higher than 40%.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：The side of carbendazim in a kind of reduction Fructus Monordicae extract
Method, including：
1) take Fructus Monordicae extract (Guilin Laiyin Biotechnology Co., Ltd. commercially available prod, wherein, carbendazim content
0.085mg/kg, mogroside V content 41.21%), the deionized water stirring at normal temperature with 10 times of weight of Fructus Monordicae extract is molten
Solution, adjusts pH to 2-4, obtains Fructus Monordicae extract accessing pending water solution with 10% hydrochloric acid (analysis is pure)；
2) activated carbon (being purchased from CALGON companies of the U.S., Filtrasorb-200, coarse granule type) dress post is taken, 1% hydrogen is first used
Sodium oxide molybdena washes activated-charcoal column, and it is 7-8 that efflux pH is then washed to deionized water, then with 1% salt pickling activated-charcoal column, finally
It is 6-7 that efflux pH is washed to deionized water, the activated-charcoal column handled well；
3) Fructus Monordicae extract accessing pending water solution is flowed through into activated-charcoal column, flow velocity is 0.5BV/H, has been entered after decoction, used
Deionization washes activated-charcoal column, and flow velocity is 0.5BV/H, merges and collects eluent, and pH to 5 is adjusted with 10% sodium hydroxide；
4) pH eluent desalination nanofiltration ceramic membrane desalination, concentration will be mixed up, 5% solid content (quality point is concentrated to
Number), with cream processed is concentrated in vacuo to solid content 30% (mass fraction), spray drying obtains carbendazim content less than 0.01mg/
Kg, mogroside V content is higher than 40% extract.
On the basis of above-mentioned technical proposal, the present invention can also do following improvement.
Further, in 2), the consumption of the activated carbon is calculated as Fructus Monordicae extract in mass ratio：Activated carbon=2:1.
Further, in 2), the consumption of 1% sodium hydroxide is 2 times of quality of activated carbon.
Further, in 2), the consumption of 1% hydrochloric acid is 2 times of quality of activated carbon.
Further, in 3), the consumption of the deionized water is 5 times of quality of activated carbon.
The beneficial effects of the invention are as follows：
The present invention can make Fructus Monordicae extract Pesticides carbendazim content be less than 0.01mg/kg, and mogroside V content is higher than
40%.
Embodiment
The principles and features of the present invention are described below, and the given examples are served only to explain the present invention, is not intended to limit
Determine the scope of the present invention.
Embodiment 1
1) take Fructus Monordicae extract (Guilin Laiyin Biotechnology Co., Ltd. commercially available prod, wherein, carbendazim content
0.085mg/kg, mogroside V content 41.21%) 200g, is dissolved with 2000ml deionized waters stirring at normal temperature, uses 10% hydrochloric acid
It is 2.0 that (analysis is pure), which adjusts pH value, obtains Fructus Monordicae extract accessing pending water solution；
2) activated carbon (being purchased from CALGON companies of the U.S., Filtrasorb-200, coarse granule type) is taken, mass ratio presses (sieve
Chinese berry extract：Activated carbon=2:1) post is filled, first with 1% caustic washing activated-charcoal column, the consumption of 1% sodium hydroxide is 2 times
Quality of activated carbon, it is 7-8 that efflux pH is then washed to deionized water, then with 1% salt pickling activated-charcoal column, 1% hydrochloric acid
Consumption is 2 times of quality of activated carbon, and it is 6-7 that efflux pH is finally washed to deionized water, the activated-charcoal column handled well；
3) Fructus Monordicae extract accessing pending water solution is flowed through into activated-charcoal column, flow velocity is 0.5BV/H, has been entered after decoction, used
Deionization washes activated-charcoal column, and the consumption of deionized water is 5 times of quality of activated carbon, and flow velocity is 0.5BV/H, merges and collects elution
Liquid, pH to 5 is adjusted with 10% sodium hydroxide；
4) pH eluent desalination nanofiltration ceramic membrane desalination, concentration will be mixed up, 5% solid content (quality point is concentrated to
Number), with cream processed is concentrated in vacuo to solid content 30% (mass fraction), it is spray-dried, yield 96.21%, through Agilent 1100
Type high performance liquid chromatograph (Agilent Science and Technology Ltd.s of the U.S.) sampling detection, the carbendazim 0.0095mg/kg of extract,
Mogroside V content 42.35%.
Embodiment 2
1) take Fructus Monordicae extract (Guilin Laiyin Biotechnology Co., Ltd. commercially available prod, wherein, carbendazim content
0.085mg/kg, mogroside V content 41.21%) 200g, is dissolved with 2000ml deionized waters stirring at normal temperature, uses 10% hydrochloric acid
It is 2.5 that (analysis is pure), which adjusts pH value, obtains Fructus Monordicae extract accessing pending water solution；
2) activated carbon (being purchased from CALGON companies of the U.S., Filtrasorb-200, coarse granule type) is taken, mass ratio presses (sieve
Chinese berry extract：Activated carbon=2:1) activated-charcoal column is filled, first with 1% caustic washing activated-charcoal column, the consumption of 1% sodium hydroxide
For 2 times of quality of activated carbon, it is 7-8 that efflux pH is then washed to deionized water, then with 1% salt pickling resin column, 1% hydrochloric acid
Consumption be 2 times of quality of activated carbon, it is 6-7 that efflux pH is finally washed to deionized water, the activated-charcoal column handled well；
3) Fructus Monordicae extract accessing pending water solution is flowed through into activated-charcoal column, flow velocity is 0.5BV/H, has been entered after decoction, used
Deionization washes activated-charcoal column, and the consumption of deionized water is 5 times of quality of activated carbon, and flow velocity is 0.5BV/H, merges and collects elution
Liquid, pH to 5 is adjusted with 10% sodium hydroxide；
4) pH eluent desalination nanofiltration ceramic membrane desalination, concentration will be mixed up, 5% solid content (quality point is concentrated to
Number), with cream processed is concentrated in vacuo to solid content 30% (mass fraction), it is spray-dried, yield 94.28%, through Agilent 1100
Type high performance liquid chromatograph (Agilent Science and Technology Ltd.s of the U.S.) sampling detection, the carbendazim content 0.0084mg/ of extract
Kg, mogroside V content 43.61%.
Embodiment 3
1) take Fructus Monordicae extract (Guilin Laiyin Biotechnology Co., Ltd. commercially available prod, wherein, carbendazim content
0.085mg/kg, mogroside V content 41.21%) 200g, is dissolved with 2000ml deionized waters stirring at normal temperature, uses 10% hydrochloric acid
It is 3.0 that (analysis is pure), which adjusts pH, obtains Fructus Monordicae extract accessing pending water solution；
2) activated carbon (being purchased from CALGON companies of the U.S., Filtrasorb-200, coarse granule type) is taken, mass ratio presses (sieve
Chinese berry extract：Activated carbon=2:1) activated-charcoal column is filled, first with 1% caustic washing activated-charcoal column, the consumption of 1% sodium hydroxide
For 2 times of quality of activated carbon, it is 7-8 that efflux pH is then washed to deionized water, then with 1% salt pickling resin column, 1% hydrochloric acid
Consumption be 2 times of quality of activated carbon, it is 6-7 that efflux pH is finally washed to deionized water, the activated-charcoal column handled well；
3) Fructus Monordicae extract accessing pending water solution is flowed through into activated-charcoal column, flow velocity is 0.5BV/H, has been entered after decoction, used
Deionization washes activated-charcoal column, and the consumption of deionized water is 5 times of quality of activated carbon, and flow velocity is 0.5BV/H, merges and collects elution
Liquid, pH to 5 is adjusted with 10% sodium hydroxide；
4) pH eluent desalination nanofiltration ceramic membrane desalination, concentration will be mixed up, 5% solid content (quality point is concentrated to
Number), with cream processed is concentrated in vacuo to solid content 30% (mass fraction), it is spray-dried, yield 96.87%, through Agilent 1100
Type high performance liquid chromatograph (Agilent Science and Technology Ltd.s of the U.S.) sampling detection, the carbendazim 0.0055mg/kg of extract,
Mogroside V content 41.73%.
Embodiment 4
1) take Fructus Monordicae extract (Guilin Laiyin Biotechnology Co., Ltd. commercially available prod, wherein, carbendazim content
0.085mg/kg, mogroside V content 41.21%) 200g, is dissolved with 2000ml deionized waters stirring at normal temperature, uses 10% hydrochloric acid
It is 3.5 that (analysis is pure), which adjusts pH, obtains Fructus Monordicae extract accessing pending water solution；
2) activated carbon (being purchased from CALGON companies of the U.S., Filtrasorb-200, coarse granule type) is taken, mass ratio presses (sieve
Chinese berry extract：Activated carbon=2:1) activated-charcoal column is filled, first with 1% caustic washing activated-charcoal column, the consumption of 1% sodium hydroxide
For 2 times of quality of activated carbon, it is 7-8 that efflux pH is then washed to deionized water, then with 1% salt pickling resin column, 1% hydrochloric acid
Consumption be 2 times of quality of activated carbon, it is 6-7 that efflux pH is finally washed to deionized water, the activated-charcoal column handled well；
3) Fructus Monordicae extract accessing pending water solution is flowed through into activated-charcoal column, flow velocity is 0.5BV/H, has been entered after decoction, used
Deionization washes activated-charcoal column, and the consumption of deionized water is 5 times of quality of activated carbon, and flow velocity is 0.5BV/H, merges and collects elution
Liquid, pH to 5 is adjusted with 10% sodium hydroxide；
4) pH eluent desalination nanofiltration ceramic membrane desalination, concentration will be mixed up, 5% solid content (quality point is concentrated to
Number), with cream processed is concentrated in vacuo to solid content 30% (mass fraction), it is spray-dried, yield 95.45%, through Agilent 1100
Type high performance liquid chromatograph (Agilent Science and Technology Ltd.s of the U.S.) sampling detection, the carbendazim 0.0071mg/kg of extract,
Mogroside V content 42.33%.
Embodiment 5
1) take Fructus Monordicae extract (Guilin Laiyin Biotechnology Co., Ltd. commercially available prod, wherein, carbendazim content
0.085mg/kg, mogroside V content 41.21%) 200g, is dissolved with 2000ml deionized waters stirring at normal temperature, uses 10% hydrochloric acid
It is 3.8 that (analysis is pure), which adjusts pH, obtains Fructus Monordicae extract accessing pending water solution；
2) activated carbon (being purchased from CALGON companies of the U.S., Filtrasorb-200, coarse granule type) is taken, mass ratio presses (sieve
Chinese berry extract：Activated carbon=2:1) activated-charcoal column is filled, first with 1% caustic washing activated-charcoal column, the consumption of 1% sodium hydroxide
For 2 times of quality of activated carbon, it is 7-8 that efflux pH is then washed to deionized water, then with 1% salt pickling resin column, 1% hydrochloric acid
Consumption be 2 times of quality of activated carbon, it is 6-7 that efflux pH is finally washed to deionized water, the activated-charcoal column handled well；
3) Fructus Monordicae extract accessing pending water solution is flowed through into activated-charcoal column, flow velocity is 0.5BV/H, has been entered after decoction, used
Deionization washes activated-charcoal column, and the consumption of deionized water is 5 times of quality of activated carbon, and flow velocity is 0.5BV/H, merges and collects elution
Liquid, pH to 5 is adjusted with 10% sodium hydroxide；
4) pH eluent desalination nanofiltration ceramic membrane desalination, concentration will be mixed up, 5% solid content (quality point is concentrated to
Number), with cream processed is concentrated in vacuo to solid content 30% (mass fraction), it is spray-dried, yield 95.89%, through Agilent 1100
Type high performance liquid chromatograph (Agilent Science and Technology Ltd.s of the U.S.) sampling detection, the carbendazim 0.0078mg/kg of extract,
Mogroside V content 42.17%.
Embodiment 6
1) take Fructus Monordicae extract (Guilin Laiyin Biotechnology Co., Ltd. commercially available prod, wherein, carbendazim content
0.085mg/kg, mogroside V content 41.21%) 200g, is dissolved with 2000ml deionized waters stirring at normal temperature, uses 10% hydrochloric acid
It is 4.0 that (analysis is pure), which adjusts pH, obtains Fructus Monordicae extract accessing pending water solution；
2) activated carbon (being purchased from CALGON companies of the U.S., Filtrasorb-200, coarse granule type) is taken, mass ratio presses (sieve
Chinese berry extract：Activated carbon=2:1) activated-charcoal column is filled, first with 1% caustic washing activated-charcoal column, the consumption of 1% sodium hydroxide
For 2 times of quality of activated carbon, it is 7-8 that efflux pH is then washed to deionized water, then with 1% salt pickling resin column, 1% hydrochloric acid
Consumption be 2 times of quality of activated carbon, it is 6-7 that efflux pH is finally washed to deionized water, the activated-charcoal column handled well；
3) Fructus Monordicae extract accessing pending water solution is flowed through into activated-charcoal column, flow velocity is 0.5BV/H, has been entered after decoction, used
Deionization washes activated-charcoal column, and the consumption of deionized water is 5 times of quality of activated carbon, and flow velocity is 0.5BV/H, merges and collects elution
Liquid, pH to 5 is adjusted with 10% sodium hydroxide；
4) pH eluent desalination nanofiltration ceramic membrane desalination, concentration will be mixed up, 5% solid content (quality point is concentrated to
Number), with cream processed is concentrated in vacuo to solid content 30% (mass fraction), it is spray-dried, yield 96.24%, through Agilent 1100
Type high performance liquid chromatograph (Agilent Science and Technology Ltd.s of the U.S.) sampling detection, the carbendazim 0.0087mg/kg of extract,
Mogroside V content 41.37%.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.
Claims (4)
1. a kind of method for reducing carbendazim in Fructus Monordicae extract, it is characterised in that including：
1) Fructus Monordicae extract is taken, is dissolved with the deionized water stirring at normal temperature of 10 times of weight of Fructus Monordicae extract, uses 10% hydrochloric acid
Adjust pH to 2-4, obtain Fructus Monordicae extract accessing pending water solution；
2) activated carbon is taken to fill post, first with 1% caustic washing activated-charcoal column, it is 7- to be then washed to efflux pH with deionized water
8, then with 1% salt pickling activated-charcoal column, it is 6-7 that efflux pH is finally washed to deionized water, the activated carbon handled well
Post；
3) Fructus Monordicae extract accessing pending water solution is flowed through into activated-charcoal column, flow velocity is 0.5BV/H, has been entered after decoction, spend from
Son washing activated-charcoal column, flow velocity is 0.5BV/H, merges and collects eluent, adjusts pH to 5 with 10% sodium hydroxide, the deionization
The consumption of water is 5 times of quality of activated carbon；
4) pH eluent desalination nanofiltration ceramic membrane desalination, concentration will be mixed up, 5% solid content is concentrated to, with being concentrated in vacuo to
Solid content 30%, spray drying obtains carbendazim content less than 0.01mg/kg, mogroside V content is higher than 40% extraction
Thing.
2. according to the method described in claim 1, it is characterised in that in 2), the consumption of the activated carbon is calculated as in mass ratio
Fructus Monordicae extract：Activated carbon=2:1.
3. according to the method described in claim 1, it is characterised in that in 2), the consumption of 1% sodium hydroxide is 2 times of work
Property carbonaceous amount.
4. according to the method described in claim 1, it is characterised in that in 2), the consumption of 1% hydrochloric acid is 2 times of activated carbons
Quality.
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| 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 |
| SG11201809025YA (en) * | 2017-03-01 | 2018-11-29 | Guilin Layn Natural Ingredients Corp | Method for increasing content of mogroside v in siraitia grosvenorii suspended cells |
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| 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 |
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