CN103623610B - Method for extracting and purifying finotoxin-1 and scallop toxin-2 from seawater - Google Patents
Method for extracting and purifying finotoxin-1 and scallop toxin-2 from seawater Download PDFInfo
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- CN103623610B CN103623610B CN201310633780.9A CN201310633780A CN103623610B CN 103623610 B CN103623610 B CN 103623610B CN 201310633780 A CN201310633780 A CN 201310633780A CN 103623610 B CN103623610 B CN 103623610B
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- NGNQZCDZXSOVQU-UHFFFAOYSA-N 8,16,18,26,34,36-hexahydroxyhentetracontane-2,6,10,14,24,28,32-heptone Chemical compound CCCCCC(O)CC(O)CC(=O)CCCC(=O)CC(O)CC(=O)CCCCCC(O)CC(O)CC(=O)CCCC(=O)CC(O)CC(=O)CCCC(C)=O NGNQZCDZXSOVQU-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 101000939689 Araneus ventricosus U2-aranetoxin-Av1a Proteins 0.000 title claims abstract description 24
- 101000633673 Buthacus arenicola Beta-insect depressant toxin BaIT2 Proteins 0.000 title claims abstract description 24
- 101000654318 Centruroides noxius Beta-mammal toxin Cn2 Proteins 0.000 title claims abstract description 24
- 101001028695 Chironex fleckeri Toxin CfTX-2 Proteins 0.000 title claims abstract description 24
- 241000237509 Patinopecten sp. Species 0.000 title claims abstract description 24
- 235000020637 scallop Nutrition 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000013535 sea water Substances 0.000 title claims abstract description 16
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000011347 resin Substances 0.000 claims abstract description 15
- 229920005989 resin Polymers 0.000 claims abstract description 15
- 239000011521 glass Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000741 silica gel Substances 0.000 claims abstract description 7
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 239000004744 fabric Substances 0.000 claims abstract description 4
- 239000000945 filler Substances 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims abstract description 4
- 229920000728 polyester Polymers 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000007789 sealing Methods 0.000 claims abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 108
- 239000002250 absorbent Substances 0.000 claims description 31
- 230000002745 absorbent Effects 0.000 claims description 31
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 27
- CLBIEZBAENPDFY-HNXGFDTJSA-N dinophysistoxin 1 Chemical compound C([C@H](O1)[C@H](C)/C=C/[C@H]2CC[C@@]3(CC[C@H]4O[C@@H](C([C@@H](O)[C@@H]4O3)=C)[C@@H](O)C[C@H](C)[C@@H]3[C@@H](CC[C@@]4(O3)[C@@H](CCCO4)C)C)O2)C(C)=C[C@]21O[C@H](C[C@@](C)(O)C(O)=O)CC[C@H]2O CLBIEZBAENPDFY-HNXGFDTJSA-N 0.000 claims description 22
- DLTYQVNXVIJKAZ-UHFFFAOYSA-N dinophysistoxin-1 Natural products CC1CCC2(OCCCC2C)OC1C(O)CC(O)C3OC4CCC5(CCC(O5)C=CCC6CC(=CC7(OC(CC(C)(O)C(=O)O)CCC7O)O6)C)OC4C(O)C3=C DLTYQVNXVIJKAZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000003480 eluent Substances 0.000 claims description 17
- 238000004587 chromatography analysis Methods 0.000 claims description 12
- 238000002390 rotary evaporation Methods 0.000 claims description 9
- 239000000287 crude extract Substances 0.000 claims description 7
- 239000000284 extract Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 229960001866 silicon dioxide Drugs 0.000 claims description 6
- 238000007664 blowing Methods 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 238000013329 compounding Methods 0.000 claims description 3
- 239000011159 matrix material Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229920003053 polystyrene-divinylbenzene Polymers 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- -1 sealing Substances 0.000 claims description 2
- 241000195493 Cryptophyta Species 0.000 abstract description 5
- 235000015170 shellfish Nutrition 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract 4
- 239000000203 mixture Substances 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
- 238000009958 sewing Methods 0.000 abstract 1
- 238000000746 purification Methods 0.000 description 7
- 239000003053 toxin Substances 0.000 description 7
- 231100000765 toxin Toxicity 0.000 description 7
- 108700012359 toxins Proteins 0.000 description 7
- 238000001819 mass spectrum Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- PTKFEDGHUVZLPL-LLUYWJARSA-N Pectenotoxin 2 Chemical compound O[C@@H]1[C@H](C)CCO[C@]1(O)[C@H]1O[C@@H]2/C=C/C(/C)=C/[C@H](C)C[C@](C)(O3)CC[C@@H]3[C@](O3)(O4)CC[C@@]3(C)C[C@@H]4[C@@H](O3)C(=O)C[C@]3(C)[C@@H](O)[C@@H](O3)CC[C@@]3(O3)CCC[C@H]3[C@@H](C)C(=O)O[C@@H]2C1 PTKFEDGHUVZLPL-LLUYWJARSA-N 0.000 description 2
- 238000005374 membrane filtration Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 101100313763 Arabidopsis thaliana TIM22-2 gene Proteins 0.000 description 1
- 206010012735 Diarrhoea Diseases 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- PTKFEDGHUVZLPL-UHFFFAOYSA-N Pectenotoxin 2 Natural products OC1C(C)CCOC1(O)C1OC2C=CC(C)=CC(C)CC(C)(O3)CCC3C(O3)(O4)CCC3(C)CC4C(O3)C(=O)CC3(C)C(O)C(O3)CCC3(O3)CCCC3C(C)C(=O)OC2C1 PTKFEDGHUVZLPL-UHFFFAOYSA-N 0.000 description 1
- 241000200248 Prorocentrum Species 0.000 description 1
- 208000004891 Shellfish Poisoning Diseases 0.000 description 1
- 241000719329 Trentepohlia Species 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000004292 cyclic ethers Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000741 diarrhetic effect Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 210000004916 vomit Anatomy 0.000 description 1
- 230000008673 vomiting Effects 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a method for extracting finotoxin-1 and scallop toxin-2 from seawater, which comprises the following steps: 1) sewing into an adsorption bag with 48 μm polyester mesh cloth, filling adsorption resin into the adsorption bag, sealing, and adsorbing; 2) using a glass sand core chromatographic column, firstly washing off the salt in the adsorption resin by using deionized water; 3) purifying by using a glass sand core chromatographic column filled with alumina filler with the particle size of 75-150 mu m; 4) purifying with glass sand core chromatographic column filled with reversed phase C18 silica gel to obtain mixture containing finphycotoxin-1 and scallop toxin-2. The invention has the beneficial effects that the invention can simultaneously prepare two substances of the fintoxin-1 and the scallop toxin-2, and can be used as mixed standard substances. The method is not limited by the quantity of the collected algae and shellfish, can be extracted and prepared from seawater in natural sea areas in large scale, and is simple and effective.
Description
Technical field
The present invention relates to a kind of method extracting dinophysistoxin-1 and scallop toxin-2 from seawater.
Background technology
Research of diarrhetic shellfish poisons (Diarrhetic Shellfish Poisoning, DSP) is the fat-soluble many cyclic ethers class bioactivator produced by some kinds of red tide algae fin Trentepohlia and Prorocentrum.DSP causes eater to suffer from diarrhoea, vomits, transference cure in the usual a few days, and patient can self-healing.DSP often occurs at China coast, is also one of primary toxins kind of countries in the world monitoring.No matter be that toxin is monitored reliably and analyzes, still develop new toxin monitoring analysis technology, especially prepare toxin quick detection kit, all must use a large amount of toxin standard items.
China does not also have dinophysistoxin-1(Dinophysistoxin-1 at present, DTX-1) and scallop toxin-2(Pectenotoxin-2, PTX-2) technology of preparing.
Abroad, the preparation of dinophysistoxin-1 and scallop toxin-2 has two kinds of methods usually, and one is extract from shellfish tissue.But because shellfish morphological element is complicated, in extract, lipid impurities is more, purification purification process process is more complicated.Another kind extracts from toxic algae.Owing to producing the algae more difficult cultivation in laboratory conditions of dinophysistoxin-1 and scallop toxin-2, the quantity of once cultivating also is restricted, and therefore preparation process is very difficult.
Summary of the invention
For the defect existed in prior art, the object of this invention is to provide the novel technical method that the present invention establishes a kind of extracting and developing and purification dinophysistoxin-1 and scallop toxin-2 from natural waters seawater, this technology can gather dinophysistoxin-1 and scallop toxin-2 in a large number from seawater, not by the restriction of collecting quantity.Owing to adopting special macroporous absorbent resin, the toxin impurity extracted from seawater is at first less, and when separation further, purification, technology is simple.
The present invention adopts following technical scheme:
From seawater, extract a method for dinophysistoxin-1 and scallop toxin-2, concrete steps are as follows:
1) absorbent packet is sewn into the polyester screen cloth that aperture is 48 μm, the macroporous absorbent resin that to load with nonpolar polystyrene-divinylbenzene in absorbent packet be matrix, sealing, absorbent packet is hung over cursory on, absorbent packet is positioned at below seawater surface 0.5 ~ 1m place, soaks and takes out after 7 days;
2) each for the macroporous absorbent resin in absorbent packet 10g being proceeded to nothing mark mouth 4F piston has in core glass chromatography column, with 50 ~ 70mL deionized water drip washing core filter post, wash away the salinity in macroporous absorbent resin, moisture positive pressure blowing in core filter post, and then add 20mL methanol-eluted fractions, filter in 50ml rotary evaporation bottle with the speed of 1 per second; Add 20mL methyl alcohol again, repeat to extract, merge eluent in rotary evaporation bottle; Eluent, in 40 DEG C of water-bath rotating pressure-decreasing removing methyl alcohol, during to remaining 1 ~ 2mL water, then adds 5mL carrene, then centrifugal, take out dichloromethane layer, then repeat once with 5mL carrene, merge the carrene of secondary, then dry up with nitrogen, finally dissolve with the methyl alcohol of 1.0mL80%; By above-mentioned steps, multi-pass operation is repeated to the macroporous absorbent resin in absorbent packet, obtains crude extract;
3) by 10g, through the aluminium oxide of 650 DEG C of calcinations, (chromatography is used, granularity 75 ~ 150um) load and have in core glass chromatography column without mark mouth 4F piston, first infiltrate, until liquid by when draining off to the greatest extent with methylene chloride/methanol (volume ratio, 5/5), add above-mentioned crude extract 10ml, again with 20ml methylene chloride/methanol (volume ratio, 5/5) wash-out, collect eluent, after eluent rotary evaporation is concentrated, with 5ml80% methyl alcohol dissolved residue;
4) with the methyl alcohol dissolved matter of anti-phase C18 silica gel (particle diameter 40 ~ 60 μm) the further purified treatment of post after above-mentioned alumina column process; Anti-phase for 10g C18 silica filler is respectively charged into and has in core glass chromatography column without mark mouth 4F piston, first add 10ml100% methyl alcohol to infiltrate, in post, methyl alcohol is by when draining off to the greatest extent, add the methyl alcohol dissolved matter after the above-mentioned alumina column process of 30ml again, with 80% methanol/water wash-out, collect eluent, with 2ml80% methanol/water dissolved residue after concentrated, obtain the compounding substances containing dinophysistoxin-1 and scallop toxin-2.
The invention has the beneficial effects as follows:
The present invention can prepare dinophysistoxin-1 and scallop toxin-2 two kinds of materials simultaneously, can as hybrid standard substance migration.The algae do not gathered and the quantitative limitation of shellfish number, can extract preparation in enormous quantities from natural waters seawater, and method is simple, effectively, the splitter particularly used in separation, purifying step and eluent, effectively can improve the effect of separation, purification.
Accompanying drawing explanation
The present invention has following accompanying drawing:
The mass spectrogram of Fig. 1 dinophysistoxin-1 standard items;
The goods figure of Fig. 2 scallop toxin-2 standard items;
The mass spectrogram of the dinophysistoxin-1 obtained after the process of Fig. 3 alumina column;
The mass spectrogram of the scallop toxin-2 obtained after the process of Fig. 4 alumina column;
The mass spectrogram of the dinophysistoxin-1 obtained after Fig. 5 C18 silicagel column purified treatment;
The mass spectrogram of the scallop toxin-2 obtained after Fig. 6 C18 silicagel column purified treatment.
Detailed description of the invention
From seawater, extract the method preparing dinophysistoxin-1 and scallop toxin-2, concrete steps are as follows:
1) adsorb: be sewn into absorbent packet with the polyester screen cloth that aperture is 48 μm, the length of side is the square bag of 10cm × 10cm, take the macroporous absorbent resin (HP20 that 100g is matrix with nonpolar polystyrene-divinylbenzene, Mitsubishi chemical Co., Ltd) in absorbent packet, seal afterwards, and fix nylon at absorbent packet one jiao and buckle.20 absorbent packets, June, hang over sea area, gulf, the Huanghai Sea Lingshan cursory on, 0.5 ~ 1m place below seawater surface, soaks and takes out after 7 days;
2) each for the macroporous absorbent resin in absorbent packet 10g is proceeded to nothing mark mouth 4F piston and have core glass chromatography column (internal diameter 22mm, length 200mm-300mm, Shanghai Chu Bai laboratory equipment Co., Ltd) in, with 50 ~ 70mL deionized water drip washing core filter post, wash away the salinity in macroporous absorbent resin, moisture positive pressure blowing in core filter post, and then add 20mL methanol-eluted fractions, filter in 50ml rotary evaporation bottle with the speed of 1 per second; Add 20mL methyl alcohol again, repeat to extract, merge eluent in rotary evaporation bottle; Eluent, in 40 DEG C of water-bath rotating pressure-decreasing removing methyl alcohol, during to remaining 1-2mL water, then adds 5mL carrene, then centrifugal, take out dichloromethane layer, then repeat once with 5mL carrene, merge the carrene of secondary, then dry up with nitrogen, finally dissolve with the methyl alcohol of 1.0mL80%; By above-mentioned steps, multi-pass operation is repeated to the macroporous absorbent resin in absorbent packet, obtains crude extract;
3) crude extract is removed pigment impurity through alumina column purification.By 10g, through the aluminium oxide of 650 DEG C of calcinations, (chromatography is used, granularity 75 ~ 150 μm, land, Shanghai all chemical reagent factories) load and have core glass chromatography column (internal diameter 22mm without mark mouth 4F piston, length 200mm-300mm, Shanghai Chu Bai laboratory equipment Co., Ltd) in, first with methylene chloride/methanol (volume ratio, 5/5) infiltrate, until liquid by when draining off to the greatest extent, add above-mentioned crude extract 10ml, then with 20ml methylene chloride/methanol (volume ratio, 5/5) wash-out, collect eluent, after eluent rotary evaporation is concentrated, with 5ml80% methyl alcohol dissolved residue.
Repeat above-mentioned purification run, merge repeatedly the methyl alcohol dissolved matter of gained;
The effect of this step utilizes alumina column to purify the pigment impurity of removing from seawater in thick extracting toxin.
Meanwhile, get 1ml after 0.22 μm of membrane filtration, analyzed by high pressure liquid chromatography-tandem mass spectrometer (TSQ Quantum Access, Thermo Fischer Scient Inc. of the U.S.).As shown in Figure 3, concentration is 106.6ng/ml to dinophysistoxin-1 mass spectrum; Scallop toxin-2 mass spectrum as shown in Figure 4 concentration is 418.1ng/ml.
4) with the methyl alcohol dissolved matter of anti-phase C18 silica gel (particle diameter 40 ~ 60 μm) the further purified treatment of post after above-mentioned alumina column process.Anti-phase for 10g C18 silica filler is respectively charged into and has core glass chromatography column (internal diameter 22mm without mark mouth 4F piston, length 200mm-300mm, Shanghai Chu Bai laboratory equipment Co., Ltd) in, first add 10ml methyl alcohol to infiltrate, in post, methyl alcohol is by when draining off to the greatest extent, then adds the methyl alcohol dissolved matter after the above-mentioned alumina column process of 30ml, with 80% methanol/water wash-out, collect eluent, dissolve with 2ml80% methyl alcohol after eluent is concentrated, obtain the compounding substances containing dinophysistoxin-1 and scallop toxin-2.
The effect of this step utilizes C18 silicagel column isolation of purified to remove various non polar impurities.
Meanwhile, get 1ml after 0.22 μm of membrane filtration, by high pressure liquid chromatography-tandem mass spectrometer analysis, as shown in Figure 5, concentration is 24.7ng/ml to dinophysistoxin-1 mass spectrum; As shown in Figure 6, concentration is 24.5ng/ml to scallop toxin-2 mass spectrum.
By high pressure liquid chromatography-tandem mass spectrometer analysis, concentration be the mass spectrum of dinophysistoxin-1 standard items of 200ng/ml as shown in Figure 1, concentration be the mass spectrum of scallop toxin-2 standard items of 200ng/ml as shown in Figure 2.
Claims (1)
1. from seawater, extract a method for dinophysistoxin-1 and scallop toxin-2, it is characterized in that concrete steps are as follows:
1) absorbent packet is sewn into the polyester screen cloth that aperture is 48 μm, the macroporous absorbent resin that to load with nonpolar polystyrene-divinylbenzene in absorbent packet be matrix, sealing, absorbent packet is hung over cursory on, absorbent packet is positioned at below seawater surface 0.5 ~ 1m place, soaks and takes out after 7 days;
2) each for the macroporous absorbent resin in absorbent packet 10g being proceeded to nothing mark mouth 4F piston has in core glass chromatography column, with 50 ~ 70mL deionized water drip washing core filter post, wash away the salinity in macroporous absorbent resin, moisture positive pressure blowing in core filter post, and then add 20mL methanol-eluted fractions, filter in 50ml rotary evaporation bottle with the speed of 1 per second; Add 20mL methyl alcohol again, repeat to extract, merge eluent in rotary evaporation bottle; Eluent, in 40 DEG C of water-bath rotating pressure-decreasing removing methyl alcohol, during to remaining 1 ~ 2mL water, then adds 5mL carrene, then centrifugal, take out dichloromethane layer, then repeat once with 5mL carrene, merge the carrene of secondary, then dry up with nitrogen, finally dissolve with the methyl alcohol of 1.0mL80%; By above-mentioned steps, multi-pass operation is repeated to the macroporous absorbent resin in absorbent packet, obtains crude extract;
3) 10g is had in core glass chromatography column through the chromatography aluminium oxide loading of the granularity 75 ~ 150um of 650 DEG C of calcinations without mark mouth 4F piston, the methylene chloride/methanol being first 5/5 with volume ratio infiltrates, until liquid by when draining off to the greatest extent, add above-mentioned crude extract 10ml, be the methylene chloride/methanol wash-out of 5/5 again with 20ml volume ratio, collect eluent, after eluent rotary evaporation is concentrated, with 5ml80% methyl alcohol dissolved residue;
4) with particle diameter be the methyl alcohol dissolved matter of the further purified treatment of anti-phase C18 silicagel column after above-mentioned alumina column process of 40 ~ 60 μm; Anti-phase for 10g C18 silica filler is respectively charged into and has in core glass chromatography column without mark mouth 4F piston, first add 10ml100% methyl alcohol to infiltrate, in post, methyl alcohol is by when draining off to the greatest extent, add the methyl alcohol dissolved matter after the above-mentioned alumina column process of 30ml again, use 80% methanol-eluted fractions, collect eluent, with 2ml80% methyl alcohol dissolved residue after concentrated, obtain the compounding substances containing dinophysistoxin-1 and scallop toxin-2.
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| CN105198900A (en) * | 2015-09-22 | 2015-12-30 | 国家海洋环境检测中心 | Pure yessotoxin (YTX) extracting and preparing method |
| CN105561958B (en) * | 2016-03-01 | 2018-05-11 | 中国水产科学研究院黄海水产研究所 | Ionic liquid bonded silica gel for enrichment and purification of shellfish toxins and preparation method thereof |
| CN107941968B (en) * | 2017-07-21 | 2023-07-25 | 浙江大学 | Method for preparing scallop toxin-2 standard sample from large-scale fin algae culture algae liquid |
| CN108469480A (en) * | 2018-03-20 | 2018-08-31 | 上海泰坦科技股份有限公司 | A kind of detection method of saxitoxin and its application |
| CN108977504B (en) * | 2018-08-06 | 2022-03-22 | 浙江海洋大学 | Method for rapidly screening microbial strains generating finotoxin |
| CN115343378A (en) * | 2021-09-06 | 2022-11-15 | 国家海洋环境监测中心 | Method for separating and purifying okadaic acid and finotoxin homologues in prorocentrum lima |
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| CN102928529A (en) * | 2012-10-15 | 2013-02-13 | 中国水产科学研究院黄海水产研究所 | High performance liquid chromatography mass spectrometry detecting method of 16 fat soluble saxitoxins in seawater |
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| CN102928529A (en) * | 2012-10-15 | 2013-02-13 | 中国水产科学研究院黄海水产研究所 | High performance liquid chromatography mass spectrometry detecting method of 16 fat soluble saxitoxins in seawater |
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| Title |
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| 液相色谱-串联质谱法同时测定贝类中大田软海绵酸、鳍藻毒素、蛤毒素和虾夷扇贝毒素;郭萌萌等;《色谱》;20120331;第30卷(第3期);第1.2节 * |
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