CN1560626A - Separation analyzing method for lipophilicity extraction in agricultural waste - Google Patents
Separation analyzing method for lipophilicity extraction in agricultural waste Download PDFInfo
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- CN1560626A CN1560626A CNA2004100155136A CN200410015513A CN1560626A CN 1560626 A CN1560626 A CN 1560626A CN A2004100155136 A CNA2004100155136 A CN A2004100155136A CN 200410015513 A CN200410015513 A CN 200410015513A CN 1560626 A CN1560626 A CN 1560626A
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Abstract
The invention discloses a separating and analyzing method for lipophilic extracted substances from the agricultural waste, introduces a method using double-trimethyl silicane group fluoroform acetamide and trimethyl chlorosilane to carry on methyl silicane process after the lipophilic extracted substances is extracted through organic solvent, then using high temperature Rtx-1 capillary to carry on gas phase chromatogram analysis, determining the content and composition of the lipophiltic extracted substances.
Description
Technical field
The invention belongs to the qualitative of lipides and quantitative measurement technical field, be specifically related to the method for separating and analyzing of lipophilicity extract in the agricultural wastes.
Background technology
The lipophilicity extract is meant the material that organic solvent extracting timber such as adopting ethanol, acetone or methylene chloride or paper pulp obtain.In general, extract accounts for 3～6% of timber weight.Nonpolar extract is resin usually again, mainly by fatty acid, geocerellite, fatty acid ester (as sterol ester, wax and triglyceride), and neutral compound such as compositions such as fatty alcohol and sterol.Except that the lipophilicity extract, also has the water wettability extract in the timber, as lignan.The chemical composition of extract and content are subjected to the influence of several factors, as different parts of seeds, the age of tree and tree etc.The lipophilicity extract is hydrophobic low molecular compound, the chemical behavior that different types of extract shows in pulping process and after the slurrying is different: some ester class hydrolysis in storage process, and most of ester class can be remaining following in the machinery pulping process; In neutral and acid slurrying, the lipophilicity extract is difficult to remove, and in alkaline pulp-making such as sulfate pulp-making, glyceride can be fully saponified, free fatty acid and geocerellite also are easy to saponification and dissolve, have only seldom amount to remain in the paper pulp, but sterol and some sterol esters and wax can not form soluble soap, be easy to form deposition and cause a series of problems.These extracts also can have negative effect to paper strength, and cause from the applying glue phenomenon, and extract still is the principal ingredient of paper-making industrial waste water toxicity.
The classic method that reduces the extract deposition is peeling or storage etc., is not enough to eliminate pitch prob-lems usually.The latest Progress of biotechnology shows that many kinds of wood parasitic fungies have the ability of degraded lipophilicity extract, but only is just effective under specific slurrying condition to specific tree kind.Along with the employing bleaching process more friendly, as adopt other to float agent such as H to environment
2O
2, O
3Deng replacement Cl
2, it is more serious that pitch prob-lems becomes.
Seek the method that solves pitch prob-lems and need identify the extract composition that causes pitch prob-lems in the wood raw material.The classic method cycle of extract fractionation and quantitative test is very long, classic method has a lot of steps, comprise separating, derive and gas chromatographic analysis of solvent extraction, saponification, acid and neutral component, this technology can be divided into lipides the fatty acid and the unsaponifiables of geocerellite, free and chemical combination.In addition, also have many other methods to be used for the analysis of extract, as paper chromatography, high pressure lipuid chromatography (HPLC) (HPLC), efficient size exclusion chromatography (SEC) and
13C nmr analysis method (
13C-NMR) etc.But most of method is very loaded down with trivial details, also has certain methods too high because of analyzing a large amount of sample expenses.In the past ten years, application along with modern short capillary post gas chromatographic technique, in same chromatographic run, free fatty acid and geocerellite, sterol, wax, sterol ester and triglyceride might be analyzed simultaneously, but the chemical constitution in each quasi-grease can not be analyzed.
Thereby, to use short-cut method and identify that extract has caused people's close attention, this helps to find the method that solves pitch prob-lems.At present, more to the research report that the extract of pulp and paper industry timber commonly used is analyzed, but seldom be used for the qualitative and quantitative analysis of agricultural wastes extract.Wheat straw, barley straw, rye bar and straw are most important material in the agricultural wastes, be widely used in pulp and paper industry in developing country, especially in Algeria, Argentina, China, Egypt, India, Indonesia, Mexico, Pakistan, Sri Lanka, Syria and Turkey.In these countries, fluting medium, paperboard and wrapping paper do not float straw pulp production by high yield, and bleaching straw pulp is the main slurry of production high-quality writing paper, printing paper and other paper kind.More than 900 ten thousand tons of straw pulps of the annual production of China account for 90% of the total straw pulp amount in the world.But this four kind of plant is the same with all grasses, is covered with the miocrystalline wax that one deck 1～2 μ m is wide, 2～3 μ m are long on stalk and leaf, and these waxes are mainly by long chain alkane, ester type waxes and pure wax, and a considerable amount of free fatty acid is formed.Although the wax in the agricultural wastes only accounts for 1.0～2.0%, the present annual whole world still has 1500～3,000 ten thousand tons of valuable secondary product waxes to produce, and this lipophilicity material also is many industrial potential raw materials.Report about wheat straw extract chemical composition mainly concentrates on the strong polar compound that contains phenol at present, and the research that relevant lipophilicity extract is formed seldom, has only the report of the qualitative examination aspect of some free fatty aciies and sterol aspect.
Summary of the invention
The object of the present invention is to provide the method for separating and analyzing of lipophilicity extract in a kind of agricultural wastes, it is extremely important to the influence of environment to the pitch trouble, the minimizing paper-making industrial waste water that solve in the slurrying.
The method for separating and analyzing of lipophilicity extract in the agricultural wastes of the present invention may further comprise the steps:
(1) extracting of lipophilicity extract
Agricultural wastes are cut into small pieces after drying, grind, get part by 4～6mm sieve aperture, place 45～65 ℃ of baking ovens, keep air circulation drying 15～25h, get dried agricultural wastes in cable-styled extractor with organic solvent methyl-tertbutyl ether (MTBE) extracting 12～15h, under 30～40 ℃, remove solvent with rotary evaporator, with residue at N
2Dry and weigh in the stream, calculate lipophilicity extract yield, the amount ratio of described agricultural wastes and organic solvent methyl-tertbutyl ether is 40～60: 1400～2200g/ml;
Described agricultural wastes are one or more the potpourris in wheat-straw, barley-straw, rye stalk, the straw stalk.
(2) silanization
Get dried lipophilicity extract, fluoridize acetamide and trimethyl chlorosilane carry out methyl-monosilaneization with two TMSs three, the reactant amount ratio is 2～4: 80～160: 40～80mg/ μ l/ μ l, be reflected in the closed container and carry out, keep 20～30min to finish to guarantee reaction down at 70～80 ℃, cooling adds 120～240 μ l toluene, shake up, be used for gas chromatographic analysis;
(3) gas chromatographic analysis
The sample of silanization is adopted gas chromatographic analysis, gas chromatography adopts the Rtx-1 capillary column, fill kapillary column length 15m, internal diameter 0.53mm with 100% crosslinked dimethyl silicone polymer, coating thickness is 0.10 μ m, and have flame ionization detector (FID), as carrier gas, syringe and detector temperature are set in 340 ℃ with helium, heating furnace is raised to 340 ℃ with the speed of 8 ℃/min from 70 ℃, obtains the composition and the content of lipophilicity extract by analysis.
Each compound all passes through residence time of gas chromatography and total ion detection mass spectrum and n-compound to evaluation recently in free fatty acid and geocerellite and the sterol, and the composition in wax, sterol ester and the triglyceride is only checked with the gas chromatography residence time.
This method for separating and analyzing can directly apply to the composition measurement of fatty acid and geocerellite, sterol, wax, sterol ester and the triglyceride of the wood extractive in agricultural wastes and the paper-making effluent.
The present invention compared with prior art has following advantage and beneficial effect: the method for separating and analyzing that the present invention adopts, and easy and simple to handle, step is few, and the time is short, the use amount of having saved chemicals.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail:
Embodiment 1
(1) wheat-straw is cut into small pieces after drying, grind, get part by the 4mm sieve aperture, place 45 ℃ of baking ovens to keep the dry 15h of air circulation, get 40g and in cable-styled extractor, use 1400ml organic solvent methyl-tertbutyl ether extracting 12h, under 30 ℃, remove solvent with rotary evaporator, with residue at N
2Dry and weigh in the stream, calculate the extract yield;
(2) dried lipophilicity extract 2mg fluoridizes acetamide with the two TMSs three of 80 μ l and 40 μ l trimethyl chlorosilanes carry out methyl-monosilaneizations, is reflected in the closed container and carries out, and keeps reaction 20min down at 75 ℃, cooling, add 120 μ l toluene, shake up, be used for gas chromatographic analysis;
(3) sample of silanization adopts gas chromatographic analysis, gas chromatography adopts the Rtx-1 capillary column, fill with 100% crosslinked dimethyl silicone polymer, kapillary column length 15m, internal diameter 0.53mm, coating thickness is 0.10 μ m, and have a flame ionization detector (FID), with helium as carrier gas, syringe and detector temperature are set in 340 ℃, heating furnace is raised to 340 ℃ with the speed of 8 ℃/min from 70 ℃, obtains the composition and the content of wheat-straw extract by analysis, its productive rate and chemical composition 1 sample F of seeing attached list
1
Embodiment 2
(1) barley-straw is cut into small pieces after drying, grind, get part by the 4.75mm sieve aperture, place 50 ℃ of baking ovens to keep the dry 22h of air circulation, get 60g and in cable-styled extractor, use 2200ml organic solvent methyl-tertbutyl ether extracting 15h, under 35 ℃, remove solvent with rotary evaporator, with residue at N
2Dry and weigh in the stream, calculate the extract yield;
(2) dried lipophilicity extract 3mg fluoridizes acetamide with the two TMSs three of 120 μ l and 60 μ l trimethyl chlorosilanes carry out methyl-monosilaneizations, be reflected in the closed container and carry out, keep reaction 20min down at 75 ℃, cooling, add 150 μ l toluene, shake up, be used for gas chromatographic analysis;
(3) sample of silanization adopts gas chromatographic analysis, gas chromatography adopts the Rtx-1 capillary column, fill with 100% crosslinked dimethyl silicone polymer, kapillary column length 15m, internal diameter 0.53mm, coating thickness is 0.10 μ m, and have a flame ionization detector (FID), with helium as carrier gas, syringe and detector temperature are set in 340 ℃, heating furnace is raised to 340 ℃ with the speed of 8 ℃/min from 70 ℃, obtains the composition and the content of rye stalk extract by analysis, its productive rate and chemical composition 1 sample F of seeing attached list
2
Embodiment 3
(1) the rye stalk is cut into small pieces after drying, grind, get part by the 5mm sieve aperture, place 50 ℃ of baking ovens to keep the dry 20h of air circulation, get 50g and in cable-styled extractor, use 1800ml organic solvent methyl-tertbutyl ether (MTBE) extracting 14h, under 35 ℃, remove solvent with rotary evaporator, with residue at N
2Dry and weigh in the stream, calculate the extract yield;
(2) dried lipophilicity extract 3mg fluoridizes acetamide with the two TMSs three of 120 μ l and 60 μ l trimethyl chlorosilanes carry out methyl-monosilaneizations, be reflected in the closed container and carry out, keep reaction 25min down at 75 ℃, cooling, add 200 μ l toluene, shake up, be used for gas chromatographic analysis;
(3) sample of silanization adopts gas chromatographic analysis, gas chromatography adopts the Rtx-1 capillary column, fill with 100% crosslinked dimethyl silicone polymer, kapillary column length 15m, internal diameter 0.53mm, coating thickness is 0.10 μ m, and have a flame ionization detector (FID), with helium as carrier gas, syringe and detector temperature are set in 340 ℃, heating furnace is raised to 340 ℃ with the speed of 8 ℃/min from 70 ℃, obtains the composition and the content of rye stalk extract by analysis, its productive rate and chemical composition 1 sample F of seeing attached list
3
Embodiment 4
(1) the straw stalk is cut into small pieces after drying, grind, get part by the 6mm sieve aperture, place 65 ℃ of baking ovens to keep the dry 25h of air circulation, get 60g and in cable-styled extractor, use 2200ml organic solvent methyl-tertbutyl ether extracting 15h, under 40 ℃, remove solvent with rotary evaporator, with residue at N
2Dry and weigh in the stream, calculate the extract yield;
(2) dried lipophilicity extract 4mg fluoridizes acetamide with the two TMSs three of 160 μ l and 80 μ l trimethyl chlorosilanes carry out methyl-monosilaneizations, be reflected in the closed container and carry out, keep reaction 30min down at 70 ℃, cooling, add 240 μ l toluene, shake up, be used for gas chromatographic analysis;
(3) sample of silanization adopts gas chromatographic analysis, gas chromatography adopts the Rtx-1 capillary column, fill with 100% crosslinked dimethyl silicone polymer, kapillary column length 15m, internal diameter 0.53mm, coating thickness is 0.10 μ m, and have a flame ionization detector (FID), with helium as carrier gas, syringe and detector temperature are set in 340 ℃, heating furnace is raised to 340 ℃ with the speed of 8 ℃/min from 70 ℃, obtains the composition and the content of straw stalk extract by analysis, its productive rate and chemical composition 1 sample F of seeing attached list
4
Embodiment 5
(1) wheat-straw, rye stalk, straw stalk are cut into small pieces respectively after drying, grind, get part by the 5mm sieve aperture, place 50 ℃ of baking ovens to keep the dry 22h of air circulation, get 20g, 15g, 15g respectively and mix back 1800ml organic solvent methyl-tertbutyl ether (MTBE) extracting 14h in cable-styled extractor, under 35 ℃, remove solvent with rotary evaporator, with residue at N
2Dry and weigh in the stream, calculate the extract yield;
(2) dried lipophilicity extract 3mg fluoridizes acetamide with the two TMSs three of 120 μ l and 60 μ l trimethyl chlorosilanes carry out methyl-monosilaneizations, be reflected in the closed container and carry out, keep reaction 25min down at 75 ℃, cooling, add 180 μ l toluene, shake up, be used for gas chromatographic analysis;
(3) sample of silanization adopts gas chromatographic analysis, gas chromatography adopts the Rtx-1 capillary column, fill with 100% crosslinked dimethyl silicone polymer, kapillary column length 15m, internal diameter 0.53mm, coating thickness is 0.10 μ m, and have a flame ionization detector (FID), with helium as carrier gas, syringe and detector temperature are set in 340 ℃, heating furnace is raised to 340 ℃ with the speed of 8 ℃/min from 70 ℃, obtains the composition and the content of the extract of mixed straw by analysis, its productive rate and chemical composition 1 sample F of seeing attached list
5
Yield of table 1 wheat straw, barley straw, rye bar, straw and mixed straw extract (to the over dry sample) and chemical composition (to the over dry extract)
Yield/chemical composition F
1 aF
2 aF
3 aF
4 aF
5 a
Yield 1.12 1.19 1.01 0.97 1.05
Chemical composition
Free fatty acid/geocerellite/other acid (P1-26)
b31.08 24.77 23.65 20.30 25.04
Eicosenoic acid, C20:1 (P15) 0.19 0.07 0.18 0.21 0.19
Arachic acid, C20:0 (P16) 0.48 0.30 0.70 0.60 0.59
Heneicosanoic acid, C21:0 (P18) 0.15 N 0.20 0.18 0.18
Docosanoic acid, C22:0 (P20) 0.41 0.38 0.66 0.47 0.51
Lignoceric acid, C24:0 (P23) 0.32 0.26 1.20 0.98 0.83
Sterol (P27～31) 13.79 10.42 12.54 14.60 13.62
The potpourri of analyzing 13.79 10.42 12.54 14.60 13.62
Cholesterol (P27) 1.46 0.52 0.84 0.32 0.86
Ergosterol (P28) 0.28 N 1.18 0.49 0.65
Stigmasterol (P30) 0.31 0.30 N
cT
d0.15
P-sitosterol (P29～31) 13.20 9.60 10.52 13.79 12.53
Wax (P32～37) 17.20 11.22 27.14 9.53 17.96
The potpourri of analyzing 10.81 8.77 15.06 4.34 10.07
Palmitic acid palm ester (P32) 4.88 6.36 10.51 3.04 6.14
Palmitic acid grease (P34) 5.72 2.05 4.39 0.96 3.69
Oleyl oleate (P36) 0.21 0.36 0.16 0.34 0.24
Diglyceride (P38～39) 0.31 0.65 0.23 0.42 0.32
The potpourri of analyzing 0.16 0.34 0.05 0.22 0.14
Glycerol-1,3-dipalmitate (P38) 0.16 0.34 0.05 0.22 0.14
Sterol ester (P40～48) 13.25 24.70 16.20 18.19 15.88
The potpourri of analyzing 8.74 18.25 10.70 10.83 10.09
Sterol laurate (P42) 0.62 4.25 0.95 0.29 0.62
Sterol myristinate (P44) 2.65 7.24 3.56 3.20 3.14
Sterol palmitate (P46) 1.83 2.70 1.86 2.28 1.99
Sterol margarate (P47) 2.12 1.60 2.20 2.93 2.42
Sterol oleate (P48) 1.52 2.46 2.13 2.13 1.93
Triglyceride (P49～56) 9.72 10.03 5.72 11.38 8.94
The potpourri of analyzing 3.56 6.65 2.06 5.33 3.65
Tripalmitin (P50) 0.32 2.64 0.23 1.64 0.73
Two palmitic acids-olein (P51) 1.56 1.68 1.06 2.08 1.57
Olein (P54) 1.68 2.33 0.77 1.61 1.35
Total content 85.35 81.79 85.30 74.42 81.69
Total oily matter 80.37 81.04 84.65 73.28 79.43
aRepresentative methyl tert-butyl ether difference extracting wheat straw (F in cable-styled extractor
1), barley straw (F
2), rye bar (F
3), straw (F
4) and mixed straw (F
5) the extract component that obtains.
Claims (2)
1. the method for separating and analyzing of lipophilicity extract in the agricultural wastes is characterized in that step is as follows:
(1) extracting of lipophilicity extract
Agricultural wastes are cut into small pieces after drying, grind, get part by 4～6mm sieve aperture, place 45～65 ℃ of baking ovens, keep air circulation drying 15～25h, get dried agricultural wastes in cable-styled extractor with organic solvent methyl-tertbutyl ether extracting 12～15h, under 30～40 ℃, remove solvent with rotary evaporator, with residue at N
2Dry and weigh in the stream, calculate lipophilicity extract yield, the amount ratio of described agricultural wastes and organic solvent methyl-tertbutyl ether is 40～60: 1400～2200g/ml;
(2) silanization
Get dried lipophilicity extract, fluoridize acetamide and trimethyl chlorosilane carry out methyl-monosilaneization with two TMSs three, the reactant amount ratio is 2～4: 80～160: 40～80mg/ μ l/ μ l, be reflected in the closed container and carry out, keep 20～30min to finish down at 70～80 ℃ to guarantee reaction, cooling adds 120～240 μ l toluene, shakes up;
(3) gas chromatographic analysis
The sample of silanization is adopted gas chromatographic analysis, gas chromatography adopts the Rtx-1 capillary column, fill kapillary column length 15m, internal diameter 0.53mm with 100% crosslinked dimethyl silicone polymer, coating thickness is 0.10 μ m, and have flame ionization detector, as carrier gas, syringe and detector temperature are set in 340 ℃ with helium, heating furnace is raised to 340 ℃ with the speed of 8 ℃/min from 70 ℃, obtains the composition and the content of lipophilicity extract by analysis.
2. the method for separating and analyzing of lipophilicity extract is characterized in that in the agricultural wastes according to claim 1, and described agricultural wastes are one or more the potpourris in wheat-straw, barley-straw, rye stalk, the straw stalk.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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|---|---|---|---|
| CN 200410015513 CN1260566C (en) | 2004-03-02 | 2004-03-02 | Separation analyzing method for lipophilicity extraction in agricultural waste |
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| CN1260566C CN1260566C (en) | 2006-06-21 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102494935A (en) * | 2011-12-08 | 2012-06-13 | 上海烟草集团有限责任公司 | Method for determining resin and gooey in reconstituted tobacco pulp system of papermaking method |
| CN103018389A (en) * | 2011-09-23 | 2013-04-03 | 北大方正集团有限公司 | High performance liquid chromatography method and application thereof |
| CN104267123A (en) * | 2014-09-30 | 2015-01-07 | 中国农业科学院油料作物研究所 | Analysis method of free sterol components in edible oil sample and swill-cooked dirty oil identification method |
| CN105259089A (en) * | 2015-11-03 | 2016-01-20 | 三峡大学 | Method for identifying quality of wood |
-
2004
- 2004-03-02 CN CN 200410015513 patent/CN1260566C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103018389A (en) * | 2011-09-23 | 2013-04-03 | 北大方正集团有限公司 | High performance liquid chromatography method and application thereof |
| CN103018389B (en) * | 2011-09-23 | 2015-01-07 | 北大方正集团有限公司 | High performance liquid chromatography method and application thereof |
| CN102494935A (en) * | 2011-12-08 | 2012-06-13 | 上海烟草集团有限责任公司 | Method for determining resin and gooey in reconstituted tobacco pulp system of papermaking method |
| CN102494935B (en) * | 2011-12-08 | 2014-01-29 | 上海烟草集团有限责任公司 | Method for determining resin and gooey in reconstituted tobacco pulp system of papermaking method |
| CN104267123A (en) * | 2014-09-30 | 2015-01-07 | 中国农业科学院油料作物研究所 | Analysis method of free sterol components in edible oil sample and swill-cooked dirty oil identification method |
| CN105259089A (en) * | 2015-11-03 | 2016-01-20 | 三峡大学 | Method for identifying quality of wood |
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| CN1260566C (en) | 2006-06-21 |
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