CN101210864A - Soil neutral sugar Acetylated Aldononitriles derivation capillary gas chromatography analytical method - Google Patents
Soil neutral sugar Acetylated Aldononitriles derivation capillary gas chromatography analytical method Download PDFInfo
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Abstract
The invention relates to a method for detecting carbohydrates in soil, specifically to a capillary gas chromatographic analysis method for neutral sugars in soil based on acetylated aldononitrile derivatives. The method comprises (1) hydrolysis of a soil sample by weighing a soil sample containing 4-5mg organic carbon, hydrolyzing with 9-12mL 4M trifluoroacetic acid, adding 100Mug pentitol solution, shaking, and filtering to obtain a hydrolysate; (2) purification of the hydrolysate by neutralizing the hydrolysate with potassium hydroxide, adjusting pH to 6.6-6.8, centrifuging, drying by rotary evaporation, dissolving the obtained solid matter in 3-4mL distilled water, adding 100Mug inositol solution, and freeze drying to obtain a dried sample; and (3) derivation of the sample by acetylated aldononitrile method, and detecting by gas chromatography. The invention has the advantages of high sensitivity, good precision and accuracy, and rapid operation; and is suitable for routine analysis and detection.
Description
Technical field
The present invention relates to the mensuration of soil carbon hydrate, specifically a kind of sugared nitrile acetonyl ester derivation capillary gas chromatography analytical method of soil neutral sugar.
Background technology
The soil carbon hydrate accounts for the 5-25% of the soil organism
[1](Murata et al.1999.Seasonalvariations in soil microbial biomass content and soil neutral sugar compositionin grassland in the Japanese Temperate Zone.Applied Soil Ecology 11,253-259.), be the important component part in the variable storehouse of the soil organism, and be the main energy source of microbial process in the soil
[2](Martens and Loeffelmann.2002.Improved accounting ofcarbohydrate carbon from plants and soils.Soil Biology﹠amp; Biochemistry 34,1393-1399).Neutral sugar is a kind of of soil carbon hydrate, and they play an important role to soil aggregation
[3](Puget et al.1999.Nature of carbohydrates associated with water-stableaggregates of two cultivated soils.Soil Biology﹠amp; Biochemistry 31,55-63).Soil neutral sugar can be by the microorganism tachymetabolism, but their degraded is relevant with their existence form and the character of soil mineral.Soil neutral sugar exists with combining with the polysaccharide form of soil agreegate
[4](Rumpel and Dignac 2006.Gas chromatographic analysis of monosaccharidesin forest soil profile:Analysis by gas chromatography after trifluoroacetic acidhydrolysis and reduction-acetylation.Soil Biology﹠amp; Biochemistry 38, and 1478-1481), therefore, the qualitative and quantitative composition of understanding soil neutral sugar is extremely important.
Capillary gas chromatography is a kind of common methods of analyzing soil neutral sugar.Because neutral sugar is a nonvolatile element, therefore before carrying out gas Chromatographic Determination, they must be derived is volatile components.Sugar alcohol acetonyl ester derivatization method is a kind of method of common mensuration soil neutral sugar
[5](Cheshire et al.1990.Labelled and native sugars in particle-size fractions from soils incubatedwith
14C straw for 6-18 years.Journal of Soil Science 41,29-39).But this method needs a large amount of preparation process, especially removes the used excessive borate of reduction step, complex operation, and elapsed time is unfavorable for routine analysis and detection.Recently, Rumpel and Dignac (2006)
[4]Said method is improved, promptly need not remove too much borate, still, the recovery of ribose very low (having only 35%), and some sugared coefficient of variation is very high.
The trimethylsilyl ethers derivatization method also can be used for measuring soil neutral sugar
[6](Larr é-Larrouy and Feller1997.Determination of carbohydrates in two ferrallitic soils:Analysis bycapillary gas chromatography after derivatization by silylation.Soil Biology﹠amp; Biochemistry 29,1585-1589).Yet the shortcoming of this method is every kind of sugar forms two chromatographic peaks, and the chromatogram complexity is unfavorable for quantitative test.Amelung et al (1996)
[7](Amelung et al.1996.Determination of neutral and acidic sugars in soil by capillary gas-liquidchromatography after trifluoroacetic acid hydrolysis.Soil Biology﹠amp; Biochemistry 28,1631-1639) adopt O-methyl-oxime-trimethyl silane method to overcome the shortcoming that forms multiplet, but can only partly overcome the formation of multiplet, and the reaction product instability is unfavorable for preserving in addition
[6], still limited the reliability of quantitative test.
Sugar nitrile acetonyl ester derivatization method once was used to measure neutral sugar and the amino sugar in the biological sample
[8](Guerrant and Moss 1984.Determination of monosaccharides as aldononitrile, O-methyloxime, alditol, and cyclitol acetates derivatives by gas chromatography.Analytical Chemistry 56,633-638).This method is more simple to operate than sugar alcohol acetonyl ester method, and every kind of sugared chromatographic peak is single, therefore also is better than the trimethylsilyl ethers derivatization method.Zhang and Amelung (1996)
[9](Zhang and Amelung.1996.Gas chromatographic determination ofmuramic acid, glucosamine, mannosamine, and galactosamine in soils.SoilBiology﹠amp; Biochemistry 28,1201-1206) set up the method for measuring the soil amino sugar with sugared nitrile acetonyl ester method, yet this method also are not applied to the mensuration of soil neutral sugar.
Usually soil neutral sugar adopts sulfuric acid and trifluoroacetic acid (TFA) hydrolysis and corresponding purifying procedure to carry out purifying
[7]Yet when adopting sugared nitrile acetonyl ester to derive, which kind of hydrolysis and purifying procedure are more suitable still unclear.
Summary of the invention
In order to solve the deficiencies in the prior art part, the object of the present invention is to provide a kind of sugared nitrile acetonyl ester derivation capillary gas chromatography analytical method of soil neutral sugar, and find out and be suitable for sugared nitrile acetonyl ester and derive and measure the hydrolysis and the purification process of soil neutral sugar.
For achieving the above object, the technical solution used in the present invention is:
A kind of sugared nitrile acetonyl ester derivation capillary gas chromatography analytical method of soil neutral sugar, concrete steps are as follows,
(1) hydrolysis of pedotheque: take by weighing the pedotheque that contains the 4-5mg organic carbon, be hydrolyzed with 9-12ml 4M trifluoroacetic acid, after the hydrolysis, add filter after 100 μ g pentitol solution vibrations shakes up hydrolyzate;
(2) purifying of hydrolyzate: with potassium hydroxide neutralizing hydrolysis liquid, accent pH is 6.6-6.8, and process is centrifugal, rotary evaporation is dry, solid matter 3-4ml dissolved in distilled water, and add 100 μ g inositol solutions, freeze drying obtains dry sample;
(3) deriving of sample: adopt sugared nitrile acetonyl ester method that sample is derived; Carry out gas Chromatographic Determination then.
Described hydrolysis temperature can be 103-108 ℃, time 4-4.5h; At room temperature to 45 ℃ evaporate to dryness, residue is dissolved in the 15-20ml distilled water filtrate with Rotary Evaporators, and to transfer pH with 0.3-0.5mol/LKOH be 6.6-6.8, is deposited in the centrifugal 10-15min of 2800-3000 commentaries on classics/min;
Neutral sugar is in pyridine-methanol solution, be with oxammonium hydrochloride and acetic anhydride sugared nitrile acetonyl ester reaction to take place under the condition of catalyzer with the 4-dimethylamino naphthyridine, the gained derivant can utilize gas Chromatographic Determination, can be with the sample of step (3) with 1: 1 ethyl acetate of volume ratio: behind the n-hexane dissolution, can carry out gas chromatographic analysis.
Described sugared nitrile acetonyl ester method is carried out derivatization process with sample and is: add 290-350 μ l derivative reagent in the bottle of deriving of dry sample, seal, heat 25-30min down at 75-80 ℃, vibrate 2-5 time therebetween; After being cooled to room temperature, add the 0.9-1.1ml acetic anhydride, 20-22min is heated in sealing once more, vibrates 2-5 time therebetween; The cooling back adds the methylene chloride of 1.4-1.6ml;
Excessive derivative reagent removed by following two steps:
At first, add 0.9-1.1ml 1mol/L HCl, behind the fierce jolting 25-35s, remove supernatant liquid;
Secondly, identical with top step, wash 3-4 time with the distillation of 1-1.2ml, remove water the last time in the washing process as far as possible, remaining organic phase is used N under 40-45 ℃
2After drying up, with 200-300 μ l v/v=1: be transferred in the sample introduction bottle after 1 ethyl acetate-normal hexane mixed solvent dissolving, can carry out gas Chromatographic Determination;
Derivative reagent is: pyridine-methanol solution of 4: 1, contain 32mgmL
-1Oxammonium hydrochloride and 40mgmL
-14-dimethylaminopyridine.
The present invention has following advantage:
1. favorable reproducibility.Because the pedotheque composition is complicated, need more processing procedure, the present invention adopts internal standard method (in be designated as pentitol) to measure soil neutral sugar, and the gained data are accurate, favorable reproducibility.
2. highly sensitive, the range of linearity is wide, and its range of linearity is 10-640 μ g ml
-1
3. recovery height is operated fast.Average recovery rate reaches 100.1%, and chromatographic peak of the present invention is single, and the gained data accurately and reliably.Purifying procedure that the present invention adopts and sugared nitrile acetonyl ester derivatization method operation steps be simple, fast, so the present invention is better than sugar alcohol acetonyl ester derivatization method and trimethylsilyl ethers derivatization method, can satisfy the demand of routine analysis.
Description of drawings
Fig. 1: the gas chromatogram of neutral sugar, wherein: a: standard specimen, b: pedotheque 1. ribose, 2. rhamnose, 3. arabinose, 4. wood sugar, 5. fucose, 6. pentitol, 7. mannose, 8. glucose, 9. galactose, 10. inositol.
Embodiment
Enumerate an embodiment below, the present invention is further specified.
Embodiment 1:
Measure the content of soil neutral sugar as follows.
1.1 instrument and reagent
Agilent HP 6890 gas chromatographs are joined flame ionization detector (FID), DM-1 type quartz capillary gas chromatographic column (30m * 0.25mm * 0.25 μ m), Rotary Evaporators, freeze drier, accurate well heater, hydro-extractor, baking oven, pH meter etc.
8 kinds of neutral sugar standards, as ribose, rhamnose, arabinose, wood sugar, glucose, galactose, mannose, fucose, mark pentitol and inositol are all bought from Sigma-Aldrich company and Fluka company in reaching; Oxammonium hydrochloride is bought from Sigma-Aldrich company, and the 4-dimethylamino naphthyridine is bought from Fluka company; Methylene chloride, ethyl acetate, normal hexane and absolute methanol are bought from Dima company; It is pure that pyridine, trifluoroacetic acid (TFA), hydrochloric acid and acetic anhydride are analysis.
1.2 the preparation of solution
Standard solution and the preparation of interior target: 8 kinds of neutral sugars, the concentration of pentitol and inositol is 1mg/mL.
The preparation of derivative reagent: pyridine-methanol solution of 4: 1, contain 32mgmL
-1Oxammonium hydrochloride and 40mgmL
-14-dimethylaminopyridine.
1.3 for examination soil
Adopt 4 kinds of soil of different nature.Red soil picks up from red soil development test station, Jiangxi, and two kinds of black earth pick up from Gongzhuling, Jilin Province (G) and the Helen of Heilongjiang Province (H) respectively, and brown earth picks up from the ShenYang, Liaoning Province, and 4 kinds of soil are topsoil (0-20cm), and 250 μ m sieve is crossed in air-dry back, and fundamental property sees Table 1.
Table 1 is for examination soil basic physical and chemical (0-20cm)
1.4 the processing of pedotheque
1.4.1 hydrolysis and purifying
Take by weighing the above-mentioned pedotheque (organic carbon content adopts elemental analyser to measure) that contains the 4mg organic carbon respectively and put into the hydrolysis bottle, add 10ml 4M TFA at 105 ℃ of hydrolysis 4h
[7]After the hydrolysis, 1mg/mL pentitol solution (interior mark) vibration that adds 100 μ L shakes up the back and filters.At 45 ℃ of evaporates to dryness, residue is dissolved in the 20ml distilled water filtrate with Rotary Evaporators, and is 6.6-6.8 with 0.4mol/L KOH accent pH, is deposited in the centrifugal 10min of 3000 commentaries on classics/min.Supernatant is the rotary evaporation drying once more, and solid matter 4ml dissolved in distilled water is transferred to the 1mg/mL inositol solution that 5ml derives in the bottle and adds 100 μ L then, carries out freeze drying (more than 8 hours).
1.4.2 derive
(pyridine-methanol solution of 4: 1 contains 32mgmL to add 300 μ l derivative reagents respectively in the above-mentioned bottle of deriving that contains dry sample
-1Oxammonium hydrochloride and 40mgmL
-14-dimethylaminopyridine), seal, at 75-80 ℃ of following heating 30min, vibrate 2-3 time therebetween.After being cooled to room temperature, add the 1ml acetic anhydride, 20min is heated in sealing once more, vibrates 2-3 time therebetween.The cooling back adds the methylene chloride of 1.5ml.Excessive derivative reagent removed by following two steps:
At first, add 1ml 1mol/L HCl, behind the fierce jolting 30s, remove supernatant liquid.
Secondly, identical with top step, wash 3 times with the distillation of 1ml, remove water the last time in the washing process as far as possible.Remaining organic phase is used N under 45 ℃
2After drying up, be to be transferred in the sample introduction bottle after 1: 1 the ethyl acetate-normal hexane mixed solvent dissolving with 200 μ l volume ratios, can carry out gas Chromatographic Determination.
1.5 stratographic analysis
The gradient increased temperature program is: 175 ℃ of column temperatures, keep 4min, and be warming up to 225 ℃ with the speed of 4 ℃/min, keep 2min, the speed with 50 ℃/min is warming up to 300 ℃ again, keeps 2min.Carrier gas is N
2, flow velocity 1.2ml/min.Sample size is 1 μ l, and split ratio is 30: 1.Injector temperature is 250 ℃, and detector temperature is 300 ℃, with the peak area inner mark method ration.
Used chromatographic column is nonpolar capillary chromatographic column among the present invention; What this experiment was adopted is the DM-1 post, HP-1 in fact, OV-1 also can because they all are non-polar columns.DM-1 wherein, HP-1, OV-1 refer to the pillar that different manufacturers is produced.
1.6 typical curve, reappearance and the recovery
The standard solution of drawing 8 kinds of neutral sugars is diluted to a series of 10,20,40,80,160,320 and 640 μ g ml that contain
-1Solution, and after the 1mg/mL pentitol solution that adds 50 μ L derives according to the method described above, carry out gas Chromatographic Determination.Each sample is established 3 reappearances that repeat evaluation method, and the recovery adopts the recovery of standard addition method to estimate.Wherein, pentitol adds after hydrolysis as interior mark one, and inositol added before deriving as interior mark two.
2. result and discussion
2.1 purifying, derive and gas chromatographic technique
(1) purifying
Adopt among the KOH and the TFA hydrolyzate, make organic and the inorganic impurity precipitation, then by centrifugal removal precipitation.Zhang and Amelung (1996)
[9]Dissolve amino sugar with absolute methanol, and the KCl (hydrochloric acid and KOH reaction generates KCl) that is insoluble to methyl alcohol removes by centrifuge method.Yet in the process of the test of the present invention, when adding methyl alcohol, precipitation produces, and may be the result that TFA evaporates fully, therefore adds this step of methyl alcohol can omit.After purification step of the present invention, obtained chromatographic peak preferably.Illustrate that this purifying procedure is fit to the TFA hydrolysis and sugared nitrile acetonyl ester is derived.And purifying procedure of the present invention is than Zhang andA melung (1996)
[9]With Amelung et al (1996)
[7]Purifying procedure fast and simple.Amelung et al (1996) for example
[7]Adopt XAD-7 polymeric adsorbent and Dowex50W X8 Zeo-karb to remove organic and inorganic impurity.
(2) derive
The program of deriving of the present invention is faster than sugar alcohol acetonyl ester derivatization method
[8]Although Rumpel and Dignac (2006)
[4]Improved sugar alcohol acetonyl ester derivatization method, but some sugared recovery is lower, and the coefficient of variation is higher.And chromatographic peak of the present invention is single, therefore also is better than the trimethylsilyl ethers derivatization method.
(3) gas chromatographic technique
The present invention adopts non-polar column DM-1 to separate the derivant of 8 kinds of neutral sugars, and nonpolar comparing with polar column has column life advantage long and that clean easily.The target chromatogram is seen Fig. 1 in 8 kinds of neutral sugars and two kinds, has all reached baseline separation.Retention time sees Table 2.
The retention time (RT) of table 28 kind of neutral sugar and interior mark derivant and relative correction factor (Rf)
2.2 the range of linearity and the recovery
(1) range of linearity
The range of linearity of 8 kinds of neutral sugars of the present invention is 10-640 μ g ml
-1(R
2＞0.999).The range of linearity of known method mensuration soil neutral sugar yet there are no report at present
[7]The average coefficient of variation of 8 kinds of neutral sugar standards is less than 4.2% (n=3), and the average coefficient of variation of instrument is less than 2% (n=3).
(2) recovery
Neutral sugar sees Table 3 with respect to the recovery of pentitol.During with the TFA hydrolysis, the average recovery rate of 8 kinds of neutral sugars is 100.1%, illustrates in the whole sample set-up procedure, and interior mark is consistent with the extent of damage of 8 kinds of neutral sugars.The variation range of the recovery coefficient of variation is 1.6-10.6%, and this coefficient of variation is than Amelung et al (1996)
[7]The numerical value of report is low.In addition, pentitol is 85% with respect to the recovery of inositol, illustrates that to select pentitol for use proper as interior mark.
In addition, the groping in the process of experimental technique, the present invention has studied the effect of sulphuric acid hydrolysis neutral sugar, finds that pentitol only is 51% with respect to the recovery of inositol, may be because itself and BaSO
4The reason of co-precipitation (adopting the baryta hydrate neutralization during sulphuric acid hydrolysis).The coefficient of variation of other 8 kinds of neutral sugars is 13-205%, and the coefficient of variation is bigger.Therefore, when adopting sugared nitrile acetonyl ester derivatization method to measure soil neutral sugar, sulfuric acid is not suitable for the hydrolysis neutral sugar.
The process of its sulphuric acid hydrolysis neutral sugar and said method difference are: pedotheque is at the 12M of 1ml H
2SO
4Hydrolysis 16h under the room temperature uses 1M H again
2SO
4100 ℃ of hydrolysis 6h (Hu et al.1995.Soil carbohydrates in aggrading and degrading agroecosystems:influences of fungi and aggregates.Agriculture, Ecosystems and Environment54,77-88)
[10]After the hydrolysis, add the vibration of 100 μ g pentitols (interior mark) and shake up the back filtration.Filtrate is used Ba (OH)
2Transfer pH to neutral (pH 6.6-6.8), remove precipitation with the centrifugal 10-15min of 2800-3000 commentaries on classics/min then.At room temperature to 45 ℃ evaporate to dryness, transfer in the bottle of deriving of 5ml then and add the 1mg/mL inositol solution of 100 μ L, carries out freeze drying (more than the 8h) by residual solid matter 4mL dissolved in distilled water with Rotary Evaporators for supernatant.
The neutral sugar of table 3TFA hydrolysis with respect to the recovery of standard addition of interior mark pentitol (means ± SD, n=5)
2.3 the application of method
Adopt 4 kinds of soil of different nature the present invention to be verified the coefficient of variation that records 4 kinds of soil is 4.6%-7.6% (table 4), in these 4 kinds of soil, the total content scope of neutral sugar is 1622.4-5269.9mg kg
-1, account for 10% of the soil organism, with Amelung et al (1996)
[7]With Murata et al (1999)
[1]Report unanimity Deng the people.Arabinose, wood sugar, mannose, glucose and galactose account for major part in 8 kinds of neutral sugars, account for 90% of 8 kinds of neutral sugar total amounts, with Angers etal. (1988)
[11](Angers et al.1988.Determination of carbohydrate composition ofsoil hydrolysates by high-performance liquid chromatography.Journal ofChromatography 454,444-449) people's such as grade report unanimity.
The neutral sugar content (0-20cm) of table 44 kind of soil (means ± SD, n=5)
3. conclusion
In a word, the present invention relates to a kind of gas chromatography analysis method of measuring simultaneously 8 kinds of neutral sugars of soil, Have highly sensitively, the range of linearity is wide, favorable reproducibility, and rate of recovery height operates the advantages such as quick, can To satisfy the demand of routine analysis.
Claims (5)
1. the sugared nitrile acetonyl ester derivation capillary gas chromatography analytical method of a soil neutral sugar, it is characterized in that: concrete steps are as follows,
(1) hydrolysis of pedotheque: take by weighing the pedotheque that contains the 4-5mg organic carbon, be hydrolyzed with 9-12ml 4M trifluoroacetic acid, after the hydrolysis, add filter after 100 μ g pentitol solution vibrations shakes up hydrolyzate;
(2) purifying of hydrolyzate: with potassium hydroxide neutralizing hydrolysis liquid, accent pH is 6.6-6.8, and process is centrifugal, rotary evaporation is dry, solid matter 3-4ml dissolved in distilled water, and add 100 μ g inositol solutions, freeze drying obtains dry sample;
(3) deriving of sample: adopt sugared nitrile acetonyl ester method that sample is derived; Carry out gas Chromatographic Determination then.
2. analytical approach according to claim 1 is characterized in that: hydrolysis temperature is 103-108 ℃, time 4-4.5h.
3. analytical approach according to claim 1, it is characterized in that: filtrate uses Rotary Evaporators at room temperature to 45 ℃ evaporate to dryness, residue is dissolved in the 15-20ml distilled water, and to transfer pH with 0.3-0.5mol/LKOH be 6.6-6.8, is deposited in the centrifugal 10-15min of 2800-3000 commentaries on classics/min.
4. analytical approach according to claim 1, it is characterized in that: neutral sugar is in pyridine-methanol solution, be with oxammonium hydrochloride and acetic anhydride sugared nitrile acetonyl ester reaction to take place under the condition of catalyzer with the 4-dimethylamino naphthyridine, the gained derivant can utilize gas Chromatographic Determination, can be with the sample of step (3) with 1: 1 ethyl acetate of volume ratio: behind the n-hexane dissolution, can carry out gas chromatographic analysis.
5. analytical approach according to claim 1 is characterized in that:
Described sugared nitrile acetonyl ester method is carried out derivatization process with sample and is, adds 290-350 μ l derivative reagent in the bottle of deriving of dry sample, seals, and heats 25-30min down at 75-80 ℃, vibrates 2-5 time therebetween; After being cooled to room temperature, add the 0.9-1.1ml acetic anhydride, 20-22min is heated in sealing once more, vibrates 2-5 time therebetween; The cooling back adds the methylene chloride of 1.4-1.6ml;
Excessive derivative reagent removed by following two steps:
At first, add 0.9-1.1ml 1mol/L HCl, behind the fierce jolting 25-35s, remove supernatant liquid;
Secondly, identical with top step, wash 3-4 time with the distillation of 1-1.2ml, remove water the last time in the washing process as far as possible, remaining organic phase is used N under 40-45 ℃
2After drying up, be to be transferred in the sample introduction bottle after 1: 1 the ethyl acetate-normal hexane mixed solvent dissolving with 200-300 μ l volume ratio, can carry out gas Chromatographic Determination;
Derivative reagent is: pyridine-methanol solution of 4: 1, contain 32mgmL
-1Oxammonium hydrochloride and 40mgmL
-14-dimethylaminopyridine.
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| CN107462657A (en) * | 2017-09-11 | 2017-12-12 | 夏永刚 | A kind of method for detecting uronic acid and aldose simultaneously using gaschromatographic mass spectrometric analysis method |
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