CN104034824A - ASE-HPLC method for quickly extracting and measuring low-molecular-weight organic acids in soil - Google Patents
ASE-HPLC method for quickly extracting and measuring low-molecular-weight organic acids in soil Download PDFInfo
- Publication number
- CN104034824A CN104034824A CN201410313406.5A CN201410313406A CN104034824A CN 104034824 A CN104034824 A CN 104034824A CN 201410313406 A CN201410313406 A CN 201410313406A CN 104034824 A CN104034824 A CN 104034824A
- Authority
- CN
- China
- Prior art keywords
- acid
- soil
- organic acid
- organic acids
- extraction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 150000007524 organic acids Chemical class 0.000 title claims abstract description 69
- 239000002689 soil Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 35
- 235000005985 organic acids Nutrition 0.000 title claims abstract description 15
- 238000004128 high performance liquid chromatography Methods 0.000 title claims abstract description 11
- 238000000605 extraction Methods 0.000 claims abstract description 46
- 239000012086 standard solution Substances 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 238000010812 external standard method Methods 0.000 claims abstract description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 45
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 34
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 24
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 17
- 238000009335 monocropping Methods 0.000 claims description 15
- 235000006408 oxalic acid Nutrition 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000284 extract Substances 0.000 claims description 11
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 10
- 229940095064 tartrate Drugs 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 9
- 239000002420 orchard Substances 0.000 claims description 9
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 8
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 8
- 239000001630 malic acid Substances 0.000 claims description 8
- 235000011090 malic acid Nutrition 0.000 claims description 8
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 6
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 6
- 239000004310 lactic acid Substances 0.000 claims description 6
- 235000014655 lactic acid Nutrition 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 4
- 239000004576 sand Substances 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 235000011054 acetic acid Nutrition 0.000 claims description 3
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 3
- 235000015165 citric acid Nutrition 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000010926 purge Methods 0.000 claims description 3
- 230000003068 static effect Effects 0.000 claims description 3
- 239000001384 succinic acid Substances 0.000 claims description 3
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 3
- 239000012498 ultrapure water Substances 0.000 claims description 3
- 230000005477 standard model Effects 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 5
- 238000001914 filtration Methods 0.000 abstract description 3
- 239000012071 phase Substances 0.000 description 13
- 239000007791 liquid phase Substances 0.000 description 8
- 238000002137 ultrasound extraction Methods 0.000 description 8
- 239000002253 acid Substances 0.000 description 3
- 239000003627 allelochemical Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000001627 detrimental effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000014666 liquid concentrate Nutrition 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- XEEVLJKYYUVTRC-UHFFFAOYSA-N oxomalonic acid Chemical compound OC(=O)C(=O)C(O)=O XEEVLJKYYUVTRC-UHFFFAOYSA-N 0.000 description 2
- 238000000899 pressurised-fluid extraction Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 150000007965 phenolic acids Chemical class 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Sampling And Sample Adjustment (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to an ASE-HPLC method for quickly extracting and measuring low-molecular-weight organic acids in soil. The method includes the steps that firstly, the extracting solvent and extracting temperature of an ASE are optimized, wherein extraction is conducted on a soil sample to be measured to obtain a spectrogram of all organic acids in the soil sample; secondly, seven kinds of organic acid standard solutions are prepared, and a standard sample spectrogram of all the organic acids is obtained; lastly, the content of the organic acids in the soil to be measured is calculated through an external standard method. The method is used for extracting and measuring the organic acids in the soil; compared with a traditional extraction method, the method has great superiority and has the advantages that operation is easy and quick (free of manual filtration and small in full-automatic operation error), extraction time is short, extraction efficiency is high, and the adding standard recovery rate ranges from 86.33% to 95.41%. Thus, the method is a new method capable of easily, conveniently, quickly and efficiently measuring the content of the organic acids in the soil.
Description
(1) technical field
A kind of ASE-HPLC method that the present invention relates to quickly extracting and determining soil low molecular weight organic acid, belongs to cultivation of fruit tree field.
(2) background technology
The reason that causes apple continuous cropping (continuous cropping) obstacle is complicated, wherein more obvious with the effect of harmful microorganism and allelochemical, allelochemical mainly comprises phenolic acid, organic acid, alkaloid etc., and they can directly poison root system or as soil harmful microbe carbon source and the generation of indirect induction continuous cropping obstacle of apple.Therefore, in research continuous cropping soil, content and the character of certain class allelochemical has important operation instruction meaning to prevention and control continuous cropping obstacle of apple.Existing result of study shows, organic acid substance in soil has impact to continuous cropping obstacle of apple, so, the organic acid content in abundant extraction Accurate Determining soil, and then take measures targetedly, the object that alleviates continuous cropping obstacle of apple for finally reaching provides safeguard.But as ultrasonic extraction, succusion etc., there is the shortcomings such as extraction efficiency is low, solvent-oil ratio is large, extracting cycle is long, poor repeatability, complicated operation in the method for existing extraction and determination Organic Acids In Soil.To sum up, set up a kind of easy, new method of measuring fast and efficiently continuous cropping apple orchard soil organic acid content, to advancing the research of apple orchard continuous cropping obstacle significant.
(3) summary of the invention
In order to address the above problem, the invention provides a kind of ASE-HPLC method of quickly extracting and determining soil low molecular weight organic acid; A kind of accelerated solvent extraction (accelerated solvent extraction that utilizes specifically, ASE) and high performance liquid chromatograph (high performance liquid chromatography, HPLC) be continuous cropping apple orchard soil organic acid extraction and determination method-ASE-HPLC method of core technology.First the method is optimized the extraction solvent of ASE, extraction temperature, and the mobile phase of HPLC and mobile phase pH value are adjusted, and has finally set up a kind of easy, quick, new method-ASE-HPLC method of efficiently measuring Organic Acids In Soil content.
The present invention realizes by following steps:
(1) accurately took the fresh soil sample 1-20g in continuous cropping orchard of 12 mesh sieve, with 20-30g silica sand, mix, the sample mixing is packed in abstraction pool, by following condition, extract: the phosphoric acid solution that the concentration of take is 0.2% is extraction solvent, pressure 10.3Mpa, temperature 60 C, static extracting time 6min, flush volume 60%, purge time 200s, quiet cycle 2 times.After having extracted, extract is used to Rotary Evaporators evaporate to dryness under 40 ℃ of conditions, the phosphoric acid solution that is 0.2% by 2ml concentration is centrifugal after the extract after evaporate to dryness is dissolved; On centrifugal rear supernatant, high performance liquid chromatograph is measured and is obtained every kind of organic acid spectrogram in pedotheque.
(2) preparation of organic acid standard specimen: use ultrapure water to prepare respectively oxalic acid, tartrate, malic acid, lactic acid, citric acid, acetic acid and 7 kinds of organic acid standard solutions of succinic acid, the concentration of organic acid standard solution is respectively: oxalic acid: 51.8mg/ml, tartrate: 301.5mg/ml, malic acid: 104.9mg/ml, lactic acid: 108.5mg/ml, citric acid: 309.7mg/ml, acetic acid: 173.4mg/ml and succinic acid: 108.6mg/ml, obtains respectively every kind of organic acid standard model spectrogram by high performance liquid chromatograph on organic acid standard items.
(3) step 1) and step 2) in chromatographic condition be: chromatographic column: Symmetry C
18(5 μ m, 250mm * 4.6mm), 30 ℃ of column temperatures, the ammonium dihydrogen phosphate (ADP) of mobile phase A: 10mmol/l, Mobile phase B: methyl alcohol (mobile phase A: B=98:2, the two mixed liquor regulates pH to 2.4-2.5 by strong phosphoric acid), flow velocity: 0.9mlmin
-1; Input mode and sampling volume: auto injection, 10 μ l; Detect wavelength: 210nm.
(4) adopt external standard method to calculate the content of Organic Acids In Soil to be checked: C
sample=(A
sample/ A
standard specimen) * (V
soil sample/ m
soil sample) * C
standard specimen* 1/50
Wherein, (1) C
standard specimenthe concentration of=organic acid standard solution
(2) A
standard specimenthe liquid phase peak area of=organic acid standard items
(3) A
sampleorganic acid liquid phase peak area in=pedotheque
(4) m
soil samplethe quality 20g of=soil
(5) V
soil sample=the soil liquid concentrates volume 2ml
(6) extension rate of organic acid standard items is 50
(7) C
samplerefer to the content of Organic Acids In Soil to be checked
Result of study shows that the inventive method can realize the extraction of pedotheque organic acid, and extraction effect is better, and can realize the high efficiency liquid phase of each component of organic acid is detected, and does not occur chromatographic peak disturbed condition.
Useful result: the organic acid in the inventive method extraction and determination soil, with respect to traditional extraction process tool, have an enormous advantage, there is simple and quick (without artificial filtering, full-automatic operation error little), extraction time is short, extraction efficiency is high, and recovery of standard addition is between 86.33%-95.41%.Therefore, the inventive method is a kind of easy, quick, new method of efficiently measuring the content of Organic Acids In Soil.
(4) accompanying drawing explanation
Fig. 1 is the soil organic acid extracted amount under different extraction temperature
Fig. 1 shows, when temperature reaches while more than 65 ℃ (comprising 65 ℃), the extracted amount of oxalic acid is 0, with reference to all the other organic acid extracted amount variation with temperature rules, show that 60 ℃ is to extract organic acid optimum temperature.
Fig. 2 is the impact on organic acid extracted amount of the concentration of phosphoric acid solution
Fig. 2 shows, along with the increase of phosphoric acid solution concentration, various organic acid extracted amounts increase.But, because acid has certain detrimental effect to abstraction instrument utensil, thereby can protect instrument, again can be by under the maximized prerequisite of organic acid extraction efficiency, finally choose 0.2% phosphoric acid solution and extract.
Fig. 3 is that 7 kinds of organic acid standard items are measured spectrogram
Fig. 3 shows, by change mobile phase composition and mobile phase pH, detecting wavelength, is under 210nm condition, to make the peak of each organic acid standard specimen reach good baseline separation.
Fig. 4 is the impact of Different Extraction Method on organic acid extracted amount
Fig. 4 shows, extract in 3 kinds of methods of organic acid, the extraction efficiency of the inventive method is significantly higher than ultrasonic extraction and mechanical shaking extraction method, wherein the tartrate content of the inventive method extraction and determination is respectively ultrasonic extraction and mechanical shaking extraction method 6.57 times and 3.17 times, oxalic acid content is respectively ultrasonic extraction and mechanical shaking extraction method 2.67 times and 6.71 times, organic acid in the inventive method extraction and determination soil is described, with respect to traditional extraction process tool, have an enormous advantage, the inventive method is a kind of easy, fast, the efficient new method of measuring the content of Organic Acids In Soil.
(5) embodiment
Embodiment 1
First the extraction solvent of ASE, extraction temperature parameter are optimized, adopt different extraction temperature (30,40,50,60,65,70 and 80 ℃) to extract test.Result shows, when temperature reaches while more than 65 ℃ (comprising 65 ℃), the extracted amount of oxalic acid is 0, with reference to all the other organic acid extracted amount variation with temperature rules, show that 60 ℃ is to extract organic acid optimum temperature (Fig. 1).By preliminary experiment result, show that phosphoric acid solution is better than deionized water to the extraction effect of soil organic acid, thus we chosen 0.10%, 0.15% and the phosphoric acid solution of 0.20%3 kind of concentration the organic acid in soil is extracted.Result shows the increase along with phosphoric acid solution concentration, and various organic acid extracted amounts increase (Fig. 2).But, because acid has certain detrimental effect to abstraction instrument utensil, thereby can protect instrument, again can be by under the maximized prerequisite of organic acid extraction efficiency, finally choose 0.2% phosphoric acid solution and extract.
Embodiment 2
Accurately took the fresh soil sample 20g in continuous cropping orchard of 12 mesh sieve, silica sand 25g (addition of silica sand is fully disperseing soil sample to be advisable) mixes in mortar.1 sheet glass cellulose filter membrane on the pad of 100ml abstraction pool bottom, packs the sample mixing in abstraction pool into.By the extraction of following condition: 0.2% the phosphoric acid solution of take is extractant, pressure 10.3Mpa, temperature 60 C, static extracting time 6min, flush volume 60% (washing fluid consumption be abstraction pool volume 60%), purge time 200s, quiet cycle 2 times.After having extracted, extract is transferred in round-bottomed flask, under 40 ℃ of conditions, with Rotary Evaporators evaporate to dryness (steam to water droplet all disappear and be advisable).Phosphoric acid solution 2ml with 0.2% dissolves, and is transferred in 2ml centrifuge tube.Rotating speed with 10500r/min is centrifugal, crosses 0.22 μ m filter membrane, and on filtrate, liquid phase is measured.
The preparation of organic acid standard specimen: use ultrapure water to prepare respectively oxalic acid, tartrate, malic acid, lactic acid, citric acid, acetic acid and 7 kinds of organic acid standard solutions of succinic acid, the concentration of organic acid standard solution is respectively oxalic acid: 51.8mg/ml, tartrate: 301.5mg/ml, malic acid: 104.9mg/ml, lactic acid: 108.5mg/ml, citric acid: 309.7mg/ml, acetic acid: 173.4mg/ml and succinic acid: 108.6mg/ml, with the membrane filtration of aperture 0.22 μ m, liquid phase is measured the spectrogram (Fig. 3) that gets standard samples.
Use Waters high performance liquid chromatograph to measure.Liquid phase chromatogram condition is suitably adjusted, by change mobile phase composition and mobile phase pH, made the peak of each organic acid standard specimen reach baseline separation (Fig. 3).Chromatographic column: Symmetry C
18(5 μ m, 250mm * 4.6mm), 30 ℃ of column temperatures (U.S. Waters company), the ammonium dihydrogen phosphate (ADP) of mobile phase A: 10mmol/l, Mobile phase B: methyl alcohol (mobile phase A: Mobile phase B volume ratio=98:2, the strong phosphoric acid that the two mixed liquor is 85% by concentration regulates pH to 2.4-2.5), flow velocity: 0.9mlmin
-1; Input mode and sampling volume: auto injection, 10 μ l; Detect wavelength: 210nm.
Testing result of the present invention is to adopt external standard method to calculate organic acid content, and the phosphoric acid that the concentration of usining is 0.2% is as extraction solvent, take that to record the computation process that soil sample mesoxalic acid content to be checked (being concentration of oxalic acid) is 6.125ug/g be example:
Computing formula is: C
oxalic acid sample=(A
sample/ A
standard specimen) * (V
soil sample/ m
soil sample) * C
standard specimen* 1/50
Wherein, (1) C
standard specimenthe concentration of=oxalic acid standard items is 5.18mg/ml
(2) A
standard specimenthe liquid phase peak area of=oxalic acid standard items is 20955038
(3) A
samplethe liquid phase peak area of=pedotheque mesoxalic acid is 12388958
(4) m
soil samplethe quality 20g of=soil
(5) V
soil sample=the soil liquid concentrates volume 2ml
(6) extension rate of oxalic acid standard items is 50
Embodiment 3
To utilizing respectively ultrasonic extraction, mechanical shaking extraction method and the inventive method to carry out organic acid extraction and determination with the fresh soil sample in a continuous cropping orchard.As seen from Figure 4, in extracting the above-mentioned 3 kinds of methods of organic acid, the extraction efficiency of the inventive method is significantly higher than ultrasonic extraction and mechanical shaking extraction method, wherein the tartrate content of the inventive method extraction and determination is respectively ultrasonic extraction and mechanical shaking extraction method 6.57 times and 3.17 times, oxalic acid content is respectively ultrasonic extraction and mechanical shaking extraction method 2.67 times and 6.71 times, organic acid in the inventive method extraction and determination soil is described, with respect to traditional extraction process tool, have an enormous advantage, have simple and quick (without artificial filtration, full-automatic operation error is little), extraction time is short, extraction efficiency is high, recovery of standard addition is (in Table 1) between 86.33%-95.41%.Therefore, the inventive method is a kind of easy, quick, new method of efficiently measuring the content of Organic Acids In Soil.
Table 1ASE extracts the recovery of standard addition of tartrate, citric acid and malic acid in soil
Table 1: in order to investigate the accuracy of the inventive method, get 3 parts of pedotheques, add respectively tartrate (concentration is 301.5mg/ml), malic acid (concentration is 104.9mg/ml), three kinds of organic acid standard solution of citric acid (concentration is 309.7mg/ml), every kind of standard solution arranges three mark-on gradients (mark-on concentration is 5,10,20 μ g/g), show that the recovery of standard addition of each component, between 86.33%-95.41%, meets analyzing and testing requirement.Continuous cropping apple orchard, ground, the old orchard soils such as great Mo village village, Ci Yao town, Ningyang County, Tai’an, Yi Dui of the present invention Shandong Province, Xuan Zhuan village, Tran town, Daiyue District are measured, respond well.
Claims (1)
1. an ASE-HPLC method for quickly extracting and determining soil low molecular weight organic acid, is characterized in that comprising the following steps:
1) accurately took the fresh soil sample 1-20g in continuous cropping orchard of 12 mesh sieve, with 20-30g silica sand, mix, the sample mixing is packed in abstraction pool, by following condition, extract: the phosphoric acid solution that the concentration of take is 0.2% is extraction solvent, pressure 10.3Mpa, temperature 60 C, static extracting time 6min, flush volume 60%, purge time 200s, quiet cycle 2 times; After having extracted, extract is used to Rotary Evaporators evaporate to dryness under 40 ℃ of conditions, the phosphoric acid solution that is 0.2% by 2ml concentration is centrifugal after the extract after evaporate to dryness is dissolved; On centrifugal rear supernatant, high performance liquid chromatograph is measured and is obtained every kind of organic acid spectrogram in pedotheque;
2) preparation of organic acid standard specimen: use ultrapure water to prepare respectively oxalic acid, tartrate, malic acid, lactic acid, citric acid, acetic acid and 7 kinds of organic acid standard solutions of succinic acid, the concentration of organic acid standard solution is respectively: oxalic acid: 51.8mg/ml, tartrate: 301.5mg/ml, malic acid: 104.9mg/ml, lactic acid: 108.5mg/ml, citric acid: 309.7mg/ml, acetic acid: 173.4mg/ml and succinic acid: 108.6mg/ml, obtains respectively every kind of organic acid standard model spectrogram by high performance liquid chromatograph on organic acid standard items;
3) step 1) and step 2) in chromatographic condition be: chromatographic column: Symmetry C
18(5 μ m, 250mm * 4.6mm), 30 ℃ of column temperatures, the ammonium dihydrogen phosphate (ADP) of mobile phase A: 10mmol/l; Mobile phase B: methyl alcohol; Mobile phase A: Mobile phase B volume ratio=98:2, the two mixed liquor regulates pH value to 2.4-2.5 by strong phosphoric acid, flow velocity: 0.9mlmin
-1; Auto injection, sample size 10 μ l; Detect wavelength: 210nm;
4) adopt external standard method to calculate the content of Organic Acids In Soil to be checked.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410313406.5A CN104034824B (en) | 2014-07-02 | 2014-07-02 | A kind of ASE-HPLC method of quickly extracting and determining soil low molecular weight organic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410313406.5A CN104034824B (en) | 2014-07-02 | 2014-07-02 | A kind of ASE-HPLC method of quickly extracting and determining soil low molecular weight organic acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104034824A true CN104034824A (en) | 2014-09-10 |
| CN104034824B CN104034824B (en) | 2015-09-16 |
Family
ID=51465673
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410313406.5A Expired - Fee Related CN104034824B (en) | 2014-07-02 | 2014-07-02 | A kind of ASE-HPLC method of quickly extracting and determining soil low molecular weight organic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104034824B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105092739A (en) * | 2015-09-18 | 2015-11-25 | 江南大学 | Method for measuring seven kinds of organic acid in rice wine by adopting solid-phase extraction-liquid-phase chromatogram method |
| CN110672766A (en) * | 2019-10-17 | 2020-01-10 | 中国科学院山西煤炭化学研究所 | C in Fischer-Tropsch synthetic oil1-C4Method for detecting content of organic acid |
| CN110687234A (en) * | 2019-09-27 | 2020-01-14 | 同济大学 | Method for separating and quantifying water-soluble, fat-soluble and indissolvable organic acids in hydrocarbon source rock |
| CN113984466A (en) * | 2021-10-14 | 2022-01-28 | 安徽科技学院 | Batch determination method for detecting soil phenolic acid |
-
2014
- 2014-07-02 CN CN201410313406.5A patent/CN104034824B/en not_active Expired - Fee Related
Non-Patent Citations (5)
| Title |
|---|
| P.A.W. VAN HEES 等: "Low molecular weight organic acids and their Al-complexes in soil solution—composition, distribution and seasonal variation in three podzolized soils", 《GEODERMA》, vol. 94, 31 December 2000 (2000-12-31), pages 173 - 200 * |
| PATRICK A.W. VAN HEES 等: "Determination of low molecular weight organic acids in soil solution by HPLC", 《TALANTA》, vol. 48, 31 December 1999 (1999-12-31), pages 173 - 179 * |
| 孙晓等: "集约经营下雷竹林土壤中低分子量有机酸的初步研究", 《第五届中国竹业学术大会论文集》, 1 October 2009 (2009-10-01), pages 323 - 327 * |
| 尹承苗等: "一种分析土壤中酚酸类物质含量的新方法——以连作苹果园土壤为试材", 《中国农业科学》, vol. 46, no. 21, 31 December 2013 (2013-12-31) * |
| 王瑞琪等: "加速溶剂萃取离子色谱法测定烟草中无机阴离子和有机酸", 《浙江大学学报（理学版）》, vol. 39, no. 2, 31 March 2012 (2012-03-31), pages 205 - 209 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105092739A (en) * | 2015-09-18 | 2015-11-25 | 江南大学 | Method for measuring seven kinds of organic acid in rice wine by adopting solid-phase extraction-liquid-phase chromatogram method |
| CN105092739B (en) * | 2015-09-18 | 2017-05-24 | 江南大学 | Method for measuring seven kinds of organic acid in rice wine by adopting solid-phase extraction-liquid-phase chromatogram method |
| CN110687234A (en) * | 2019-09-27 | 2020-01-14 | 同济大学 | Method for separating and quantifying water-soluble, fat-soluble and indissolvable organic acids in hydrocarbon source rock |
| CN110672766A (en) * | 2019-10-17 | 2020-01-10 | 中国科学院山西煤炭化学研究所 | C in Fischer-Tropsch synthetic oil1-C4Method for detecting content of organic acid |
| CN113984466A (en) * | 2021-10-14 | 2022-01-28 | 安徽科技学院 | Batch determination method for detecting soil phenolic acid |
| CN113984466B (en) * | 2021-10-14 | 2024-01-12 | 安徽科技学院 | Batched determination method for detecting soil phenolic acid |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104034824B (en) | 2015-09-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104034824B (en) | A kind of ASE-HPLC method of quickly extracting and determining soil low molecular weight organic acid | |
| CN103257198B (en) | GC-MS/MS (Gas Chromatography-Mass Spectrometer) method for analyzing organo-chlorine pesticide residues in tobacco and tobacco products | |
| CN105136951A (en) | Rapid quantitative method for tea polysaccharide monosaccharide composition | |
| CN107091892A (en) | The method that the content of synthetic coloring matter in food is tested using high performance liquid chromatography | |
| CN102411034A (en) | Method for determining carbonyl compounds in water-based adhesive through direct derivation and high performance liquid chromatography | |
| CN106198832B (en) | A kind of quality of production control method of intensified loquet distillate | |
| CN105548392A (en) | Method for simultaneously detecting various antibiotics in livestock and poultry manure by high performance liquid chromatography | |
| CN104155375B (en) | The method of amino benzenes compounds in synchronous derivative ultrasonic emulsification micro-extraction gas chromatography determination environmental water sample | |
| CN102539565A (en) | Method for quickly measuring methanal content in dried beancurd sticks | |
| CN106770839A (en) | The extraction detection method of flavone compound in a kind of subprostrate sophora | |
| CN104101661B (en) | A kind of method for quick of Detection of Magdala in Food Through | |
| CN104251897A (en) | Method for simultaneously measuring residue contents of five weedicides with different structures in soil | |
| CN102890126B (en) | Method for simultaneously measuring content of multiple active ingredients in eucommia ulmoides | |
| CN102539572A (en) | Method for detecting rutin and quercetol through ionic liquid-accelerating solvent extraction and high performance liquid chromatograph chemiluminescence | |
| CN105021733B (en) | A kind of UPLC-IE method is used to measure the method for main carbonyl compounds in cigarette shreds | |
| CN106483230A (en) | A kind of method for quick of urine Hydroxyl Polycyclic Aromatic | |
| CN106841498B (en) | A kind of method for measuring tobacco and tobacco product abienol | |
| CN106770765B (en) | The detection method and application of a kind of albendazole and its metabolin | |
| CN102520107A (en) | Method for measuring matrine pesticide residual quantity in tobacco | |
| CN105486788A (en) | Kit for determining zeatin nucleoside content and method thereof | |
| CN103837615B (en) | Method applying HPLC and simultaneously determining phytoecdysone substance | |
| CN103983711B (en) | A kind of anoectochilus roxburghii glycosides quantitative analysis detection method | |
| CN104807917A (en) | Method for measuring contents of fructose and glucose in honey | |
| CN104090049B (en) | A kind of extracting method for oligosaccharides in the rice embryo of HPLC detection | |
| CN104535684A (en) | Method for detecting content of blue dyestuff in textile and leather product |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150916 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |