CN106468691B - A method of rapidly and efficiently detecting soil, 11 kinds of antibiotic contents in sludge simultaneously - Google Patents
A method of rapidly and efficiently detecting soil, 11 kinds of antibiotic contents in sludge simultaneously Download PDFInfo
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The present invention provides a kind of methods for detecting 11 kinds of antibiotic in soil simultaneously, detect antibiotic using UPLC-MS/MS method, the rate of recovery of detection method is determined with mark-on method.This method mainly uses SAX and the concatenated form of HLB pillar to carry out abstraction purification to the antibiotic of extraction, is detected using UPLC/MS/MS.The method of the invention is that a kind of rate of recovery is high, it is reproducible, can rapid batch detect the novel method of antibiotic in soil simultaneously, step is easy, quickly, detected antibiotic is totally separated out in 10 minutes, and detection limit is low, and the antibiotic suitable for low content detects, for antibiotic pollution in detection environment, antibiotic content is monitored, Degradation of Antibiotics transformation mechanism is studied, provides convenient condition.
Description
Technical field
The invention belongs to the detection technique fields of environmental contaminants, and in particular to a kind of rapidly and efficiently to detect soil, sludge
Middle chloramphenicol, Florfenicol, furazolidone, Enrofloxacin, Ofloxacin, terramycin, erythromycin, sulphadiazine, sulfalene are disliked
The method of 11 type antibiotic of azoles, ampicillin and tetracycline.
Background technique
Since antibiotic has good antibacterial action, it is widely used in the disease treatment of humans and animals, is especially being raiseeed
The usage amount of animal husbandry and culture fishery is very big, this to detect difference in environmental matrices and food at home and abroad
The antibiotic of concentration.Antibiotic content not only serious disturbance edaphon gene pool, influences ecology erroneous zone in environment,
It can also be enriched with and be entered in superior being body by the transmitting of food chain, endanger the health of humans and animals.
Establishing and measuring Multiple Classes of Antibiotics in the solid-phase matrix such as soil and sludge quickly, accurately, simultaneously is that research and control are anti-
The basis of raw element ecological risk.Up to now, the detection method of antibiotic mainly includes microbiological method, immunoassay,
Physico-chemical tests method three categories.Wherein, Physico-chemical tests method detection limit is minimum, is current most widely used antibiotic detection method.
However, antibiotic and metabolite is many kinds of and concentration is low in soil and sludge, and soil and sludge itself is various organic
Or inorganic impurity can all interfere the detection of antibiotic.Therefore, how effectively to clean, fast qualitative quantitatively becomes detection antibiotic
Emphasis.
UPLC/MS/MS detection technique is by surveying mass-to-charge ratio abundance to obtain ion stream chromatogram, and specificity is stronger, institute
It is less to interfere, it is qualitative accurate.LC-MS high sensitivity, detection limit low and analysis time is short, is adapted to detect for traces of antibiotic,
Multiple Classes of Antibiotics rapidly and efficiently can be detected simultaneously, before antibiotic context of detection has a wide range of applications in soil and sludge
Scape.
Summary of the invention
The object of the invention is that a kind of method that can simultaneously detect Multiple Classes of Antibiotics in soil is provided, it can be quickly high
Multiple types antibiotic in the detection soil of effect, detection limit it is low, high sensitivity and detection speed it is fast.
Technical solution
(1) soil, the acquisition of mud sample, preservation and pre-processing
Acquisition 0~20cm topsoil is kept in dark place under the conditions of -20 DEG C.For bed mud, acquisition pays attention to driving out of when saving
Air, ground 40 mesh sieve cold dry using freeze drier, -20 DEG C of refrigerations.
(2) soil, sludge antibiotic extracting solution are prepared
It weighs containing there are two the sodium dihydrogen phosphate 3.12g of the crystallization water, 200 μ L concentrated phosphoric acids of addition are settled to ultrapure water
100ml obtains the phosphate buffer solution of pH=3.Chromatographic grade acetonitrile is mixed with phosphate buffer solution according to volume ratio 7:3, is obtained
To soil extract.
(3) soil, antibiotic in sludge are extracted
Soil or mud sample 1g (being accurate to 0.0001g) are weighed in 50ml centrifuge tube, sequentially adds 0.2g
Na2EDTA and 10mL soil, sludge antibiotic extracting solution (see (1)).It is vortexed 1 minute, ultrasound 10 minutes is centrifuged (8000 turns) 15
Minute, collect supernatant.This process is repeated 3 times altogether.After obtained supernatant is merged, 400ml is diluted to ultrapure water.It uses
0.45 μm of organic phase miillpore filter filters.
(4) solid phase extraction concentration and antibiotic is concentrated
Solid Phase Extraction is carried out using SAX and HLB pillar: SAX column and HLB column are connected by SPE connecting column smallclothes
It is placed in Vacuum Manifold for Solid Phase Extraction.Successively pillar is activated and rinsed using 6ml hplc grade methanol and 6mL ultrapure water.
Then, antibiotic extracting solution (see (2)) is connect using bulk sampling pipe with solid-phase extraction column, opens vacuum pump and carries out solid phase
Extraction.After, solid phase extraction column is cleaned with ultrapure water, is dried in vacuo 30 minutes.Discard SAX pillar.Use 2 × 5mL color
Spectrum level methanol elutes antibiotic in 15mL test tube from HLB pillar, and high pure nitrogen is blown to close dry under 50 DEG C of water bath conditions.Add
It after adding 1mL hplc grade methanol to dissolve antibiotic again, is transferred in 2mL sample introduction bottle using 0.22 μm of pin type filter membrane, upper machine is surveyed
It is fixed.
(5) UPLC/MS/MS is detected
Extracting solution to be measured is subjected to analysis detection, measurement by UPLC/MS/MS (water generation science and technology (Shanghai) Co., Ltd.)
Chromatographic condition are as follows: use BEH-C18Chromatographic column, 2.1 × 100mm, binary gradient pump (scientific and technological (Shanghai) limited public affairs of water generation
Department)；MS/MS detector (water generation science and technology (Shanghai) Co., Ltd.)；The formic acid that mobile phase A is 0.5%, Mobile phase B is acetonitrile；
10 μ L of sampling volume；Flow velocity 0.4mL/min；50 DEG C of column temperature；Gradient elution sequence: 0~1.5min, 90%~84%A；1.5~
2min, 84%~82%A；2~2.5min, 82%~80%A；2.5~3min, 80%~78%A；3~4min, 78%~
65%A；4~4.5min, 65%~40%A；4.5~5min, 40%A；5~6.5min, 40%~5%A；6.5~7min,
5%~90%A；7~10min, 90%A.
Mass Spectrometry Conditions are as follows: chloramphenicol uses negative ion mode, orifice potential 34V, collision voltage 16V, qualitatively judge it is female from
Sub- mass-to-charge ratio is 321.00, and daughter ion mass-to-charge ratio is 151.97；Florfenicol uses negative ion mode, orifice potential 16V, collision
Voltage 18/8V, qualitatively judging mother ion mass-to-charge ratio is 356.03, and daughter ion mass-to-charge ratio is 185.05/336.00；Furazolidone is adopted
With positive ion mode, orifice potential 46V, collision voltage 20/22V, qualitatively judging mother ion mass-to-charge ratio is 226.07, daughter ion matter
Lotus ratio is 67.08/122.06；Enrofloxacin uses positive ion mode, and orifice potential 10V, collision voltage 24V are qualitatively judged female
Ion mass-to-charge ratio is 360.2603, and daughter ion mass-to-charge ratio is 342.2815；Ofloxacin uses positive ion mode, and orifice potential is
12V, collision voltage 30V, qualitatively judging mother ion mass-to-charge ratio is 362.2395, qualitatively judges daughter ion mass-to-charge ratio and is
261.2175/318.2567；Terramycin uses positive ion mode, and orifice potential 10V, collision voltage 26V are qualitatively judged female
Ion mass-to-charge ratio is 461.2439, and qualitatively judging daughter ion mass-to-charge ratio is 426.2635；Erythromycin uses positive ion mode, taper hole
Voltage is 6V, collision voltage 34/34V, and qualitatively judging mother ion mass-to-charge ratio is 734.4931, qualitatively judges daughter ion mass-to-charge ratio
For 158.1931/576.5374；Sulphadiazine uses positive ion mode, and orifice potential 6V, collision voltage 24V are qualitative to sentence
Determining mother ion mass-to-charge ratio is 251.1482, and qualitatively judging daughter ion mass-to-charge ratio is 156.0689；Sulfamethoxazole uses cation
Mode, orifice potential 4V, collision voltage 24V, qualitatively judging mother ion mass-to-charge ratio is 254.148, qualitatively judges daughter ion
Mass-to-charge ratio is 156.0694；Ampicillin uses positive ion mode, and orifice potential 32V, collision voltage 16/16V are qualitative
Determine that mother ion mass-to-charge ratio is 350.08, qualitative judgement daughter ion mass-to-charge ratio is 106.1/174.06；Tetracycline uses cation
Mode, orifice potential 4V, collision voltage 24/22V, qualitatively judge mother ion mass-to-charge ratio be 445.249, qualitatively judge son from
Sub- mass-to-charge ratio is 154.1075/410.1938.
(6) the corresponding peak area of antibiotic isolated is calculated, quantitative calculating is carried out according to standard curve, obtains antibiotic
Content.
(7) the method rate of recovery, detection limit and quantitative limit
Using the rate of recovery of standard samples recovery detection method: blank soil treatment at containing 50 μ g/L standard antibiotics
Soil detects the content of antibiotic, to calculate the rate of recovery of this method in aforementioned manners.Detection limit is determined with 3 times of signal-to-noise ratio,
Quantitative limit is determined with 10 times of signal-to-noise ratio, and the results are shown in Table 1.
Table 1 is a kind of rapidly and efficiently detect simultaneously soil, in sludge the method for 11 kinds of antibiotic contents the rate of recovery, detection limit
And quantitative limit
The advantages of the present invention
(1) technology is a variety of extracting solutions for comparing documents and materials report for the selection of extracting solution, optimizes extracting solution kind
Class and ratio make to reach best to the antibiotic extraction effect of multiple types, and prepare simply, Na2EDTA is directly added into soil
In earth, Na is eliminated2The difficult problem of EDTA dissolution, operating procedure are simple.
(2) technology is used using UPLC/MS/MS detection technique, high s/n ratio, highly sensitive, is adapted to detect for sample
The antibiotic of middle low content.
(3) UPLC/MS/MS detection technique operating pressure compared with HPLC/MS/MS is high, and disengaging time is short, is examined within 10 minutes
Antibiotic whole appearance is surveyed, rapidly and efficiently.In comparison with other other technologies, detection limits low, high sensitivity, can examine simultaneously
Multiple Classes of Antibiotics is surveyed, to probe into antibiotic adsorption-desorption rule in the soil, Transport And Transformation and degradation rule are provided very
Convenient way.
Specific embodiment
The present invention is described in further detail by following embodiment, but the technology contents that are described of the present embodiment be it is illustrative,
Without being restrictive, protection scope of the present invention should not be limited to according to this.
Embodiment 1
(1) Yuqiao Reservoir front damming bed mud soil sample is acquired, when preservation drives air out of, is put into that ice bag is stored refrigerated, and use is cold
Lyophilizer is cold dry, ground 40 mesh sieve, -20 DEG C of refrigerations.
(2) soil, sludge antibiotic extracting solution are prepared
It weighs containing there are two the sodium dihydrogen phosphate 3.12g of the crystallization water, 200 μ L concentrated phosphoric acids of addition are settled to ultrapure water
100ml obtains the phosphate buffer solution of pH=3.Chromatographic grade acetonitrile is mixed with phosphate buffer solution according to volume ratio 7:3, is obtained
To soil extract.
(3) soil, antibiotic in sludge are extracted
Mud sample 1g (being accurate to 0.0001g) is weighed in 50ml centrifuge tube, sequentially adds 0.2g Na2EDTA and
10ml soil, sludge antibiotic extracting solution (see (1)).It is vortexed 1 minute, ultrasound 10 minutes, centrifugation (8000 turns) 15 minutes is collected
Supernatant.This process is repeated 3 times altogether.After obtained supernatant is merged, 400ml is diluted to ultrapure water.Had using 0.45 μm
Machine phase miillpore filter filters.
(4) solid phase extraction concentration and antibiotic is concentrated
Solid phase microextraction is carried out using SAX with HLB pillar: SAX column has been connected with HLB column by SPE connecting column smallclothes
To be placed in Vacuum Manifold for Solid Phase Extraction.Successively pillar is activated and rushed using 6ml hplc grade methanol and 6mL ultrapure water
It washes.Then, antibiotic extracting solution (see (2)) is connect using bulk sampling pipe with solid-phase extraction column, opens vacuum pump and carries out
Solid Phase Extraction.After, solid phase extraction column is cleaned with ultrapure water, is dried in vacuo 30 minutes.Discard SAX pillar.Using 2 ×
From in HLB pillar, elution is in 15mL test tube by antibiotic for 5mL hplc grade methanol, and high pure nitrogen is blown to closely under 50 DEG C of water bath conditions
It is dry.After addition 1mL hplc grade methanol dissolves antibiotic again, it is transferred in 2mL sample introduction bottle using 0.22 μm of pin type filter membrane, on
Machine measurement.
(5) UPLC/MS/MS is detected
Extracting solution to be measured is subjected to analysis detection, measurement by UPLC/MS/MS (water generation science and technology (Shanghai) Co., Ltd.)
Chromatographic condition are as follows: use BEH-C18Chromatographic column, 2.1 × 100mm, binary gradient pump (scientific and technological (Shanghai) limited public affairs of water generation
Department)；MS/MS detector (water generation science and technology (Shanghai) Co., Ltd.)；The formic acid that mobile phase A is 0.5%, Mobile phase B is acetonitrile；
10 μ L of sampling volume；Flow velocity 0.4mL/min；50 DEG C of column temperature；Gradient elution sequence: 0~1.5min, 90%~84%A；1.5~
2min, 84%~82%A；2~2.5min, 82%~80%A；2.5~3min, 80%~78%A；3~4min, 78%~
65%A；4~4.5min, 65%~40%A；4.5~5min, 40%A；5~6.5min, 40%~5%A；6.5~7min,
5%~90%A；7~10min, 90%A.
Mass Spectrometry Conditions are as follows: chloramphenicol uses negative ion mode, orifice potential 34V, collision voltage 16V, qualitatively judge it is female from
Sub- mass-to-charge ratio is 321.00, and daughter ion mass-to-charge ratio is 151.97；Florfenicol uses negative ion mode, orifice potential 16V, collision
Voltage 18/8V, qualitatively judging mother ion mass-to-charge ratio is 356.03, and daughter ion mass-to-charge ratio is 185.05/336.00；Furazolidone is adopted
With positive ion mode, orifice potential 46V, collision voltage 20/22V, qualitatively judging mother ion mass-to-charge ratio is 226.07, daughter ion matter
Lotus ratio is 67.08/122.06；Enrofloxacin uses positive ion mode, and orifice potential 10V, collision voltage 24V are qualitatively judged female
Ion mass-to-charge ratio is 360.2603, and daughter ion mass-to-charge ratio is 342.2815；Ofloxacin uses positive ion mode, and orifice potential is
12V, collision voltage 30V, qualitatively judging mother ion mass-to-charge ratio is 362.2395, qualitatively judges daughter ion mass-to-charge ratio and is
261.2175/318.2567；Terramycin uses positive ion mode, and orifice potential 10V, collision voltage 26V are qualitatively judged female
Ion mass-to-charge ratio is 461.2439, and qualitatively judging daughter ion mass-to-charge ratio is 426.2635；Erythromycin uses positive ion mode, taper hole
Voltage is 6V, collision voltage 34/34V, and qualitatively judging mother ion mass-to-charge ratio is 734.4931, qualitatively judges daughter ion mass-to-charge ratio
For 158.1931/576.5374；Sulphadiazine uses positive ion mode, and orifice potential 6V, collision voltage 24V are qualitative to sentence
Determining mother ion mass-to-charge ratio is 251.1482, and qualitatively judging daughter ion mass-to-charge ratio is 156.0689；Sulfamethoxazole uses cation
Mode, orifice potential 4V, collision voltage 24V, qualitatively judging mother ion mass-to-charge ratio is 254.148, qualitatively judges daughter ion
Mass-to-charge ratio is 156.0694；Ampicillin uses positive ion mode, and orifice potential 32V, collision voltage 16/16V are qualitative
Determine that mother ion mass-to-charge ratio is 350.08, qualitative judgement daughter ion mass-to-charge ratio is 106.1/174.06；Tetracycline uses cation
Mode, orifice potential 4V, collision voltage 24/22V, qualitatively judge mother ion mass-to-charge ratio be 445.249, qualitatively judge son from
Sub- mass-to-charge ratio is 154.1075/410.1938.
(6) the corresponding peak area of antibiotic isolated is calculated, quantitative calculating is carried out according to standard curve, obtains antibiotic
Content.
Table 2 is actually detected result
Table 2
Detailed description of the invention
Fig. 1 is furazolidone standard sample peak spectrogram
Fig. 2 is Florfenicol standard sample appearance spectrogram
Fig. 3 is sulphadiazine standard sample appearance spectrogram
Fig. 4 is chloramphenicol standard sample appearance spectrogram
Fig. 5 is that erythromycin standard sample goes out peak figure
Fig. 6 is terramycin standard sample appearance spectrogram
Fig. 7 is Ofloxacin standard sample appearance spectrogram
Fig. 8 is Enrofloxacin standard sample appearance spectrogram
Fig. 9 is tetracycline standard sample appearance spectrogram
Figure 10 is sulfamethoxazole standard sample appearance spectrogram
Figure 11 is ampicillin standard sample appearance spectrogram
Figure 12 is that standard sample always goes out peak figure
Figure 13 is that practical test sample always goes out peak figure
Claims (1)
1. it is a kind of rapidly and efficiently detect simultaneously soil, in sludge 11 kinds of antibiotic contents method, which is characterized in that comprising following
Step:
(1) soil, the acquisition of mud sample, preservation and pre-processing
Acquisition 0 ~ 20cm topsoil is kept in dark place under the conditions of -20 DEG C, and for bed mud, acquisition pays attention to driving air out of when saving,
Cold dry, ground 40 mesh sieve using freeze drier, -20 DEG C of refrigerations；
(2) soil, sludge antibiotic extracting solution are prepared
It weighing containing there are two the sodium dihydrogen phosphate 3.12g of the crystallization water, 200 μ L concentrated phosphoric acids of addition are settled to 100ml with ultrapure water,
Obtain the phosphate buffer solution of pH=3；Chromatographic grade acetonitrile is mixed with phosphate buffer solution according to volume ratio 7:3, obtain soil,
Sludge extracting solution;
(3) soil, antibiotic in sludge are extracted
Soil or mud sample 1g are weighed, 0.0001g is accurate to, in 50ml centrifuge tube, sequentially adds 0.2gNa2EDTA and
10mL soil, sludge antibiotic extracting solution are vortexed 1 minute, ultrasound 10 minutes, centrifugation, 8000 turns, 15 minutes, collect supernatant,
This process is repeated 3 times altogether, after obtained supernatant is merged, is diluted to 400ml with ultrapure water, is used 0.45 μm of organic phase micropore
Filter membrane filters,
(4) solid phase extraction concentration and antibiotic is concentrated
Solid Phase Extraction is carried out using SAX and HLB pillar: SAX column and HLB column being connected by SPE connecting column smallclothes and are placed in
In Vacuum Manifold for Solid Phase Extraction, successively pillar is activated and rinsed using 6ml hplc grade methanol and 6mL ultrapure water, then,
Antibiotic extracting solution is connect with solid-phase extraction column using bulk sampling pipe, vacuum pump is opened and carries out Solid Phase Extraction, after,
Solid phase extraction column is cleaned with ultrapure water, is dried in vacuo 30 minutes, is discarded SAX pillar, will be resisted using 2 × 5mL hplc grade methanol
Raw element is from elution in HLB pillar in 15mL test tube, and high pure nitrogen is blown to close dry under 50 DEG C of water bath conditions, adds 1mL chromatographic grade
It after methanol dissolves antibiotic again, is transferred in 2mL sample introduction bottle using 0.22 μm of pin type filter membrane, upper machine measurement,
(5) UPLC/MS/MS is detected
Extracting solution to be measured is subjected to analysis detection, the chromatographic condition of measurement by UPLC/MS/MS are as follows: use BEH-C18Chromatographic column,
2.1 × 100mm, binary gradient pump；MS/MS detector；The formic acid that mobile phase A is 0.5%, Mobile phase B is acetonitrile；Sampling volume
10μL；Flow velocity 0.4mL/min；50 DEG C of column temperature；Gradient elution sequence: 0 ~ 1.5min, 90% ~ 84%A；1.5 ~ 2min, 84% ~ 82%A；
2 ~ 2.5min, 82% ~ 80%A；2.5 ~ 3min, 80% ~ 78%A；3 ~ 4min, 78% ~ 65%A；4 ~ 4.5min, 65% ~ 40%A；4.5~
5min, 40%A；5 ~ 6.5min, 40% ~ 5%A；6.5 ~ 7min, 5% ~ 90%A；7 ~ 10min, 90%A;
Mass Spectrometry Conditions are as follows: chloramphenicol uses negative ion mode, and orifice potential 34V, collision voltage 16V qualitatively judge parent ion matter
Lotus ratio is 321.00, and daughter ion mass-to-charge ratio is 151.97；Florfenicol uses negative ion mode, orifice potential 16V, collision voltage
18/8V, qualitatively judging mother ion mass-to-charge ratio is 356.03, and daughter ion mass-to-charge ratio is 185.05/336.00；Furazolidone is using just
Ion mode, orifice potential 46V, collision voltage 20/22V, qualitatively judging mother ion mass-to-charge ratio is 226.07, daughter ion mass-to-charge ratio
For 67.08/122.06；Enrofloxacin uses positive ion mode, and orifice potential 10V, collision voltage 24V qualitatively judge parent ion
Mass-to-charge ratio is 360.2603, and daughter ion mass-to-charge ratio is 342.2815；Ofloxacin use positive ion mode, orifice potential 12V,
Collision voltage is 30V, and qualitatively judging mother ion mass-to-charge ratio is 362.2395, and qualitatively judging daughter ion mass-to-charge ratio is 261.2175/
318.2567；Terramycin uses positive ion mode, and orifice potential 10V, collision voltage 26V qualitatively judge parent ion matter lotus
Than being 461.2439, qualitatively judging daughter ion mass-to-charge ratio is 426.2635；Erythromycin uses positive ion mode, and orifice potential is
6V, collision voltage 34/34V, qualitatively judging mother ion mass-to-charge ratio is 734.4931, qualitatively judges daughter ion mass-to-charge ratio and is
158.1931/576.5374；Sulphadiazine uses positive ion mode, and orifice potential 6V, collision voltage 24V are qualitatively judged
Mother ion mass-to-charge ratio is 251.1482, and qualitatively judging daughter ion mass-to-charge ratio is 156.0689；Sulfamethoxazole uses cation mould
Formula, orifice potential 4V, collision voltage 24V, qualitatively judging mother ion mass-to-charge ratio is 254.148, qualitatively judges daughter ion matter
Lotus ratio is 156.0694；Ampicillin uses positive ion mode, and orifice potential 32V, collision voltage 16/16V are qualitative to sentence
Determining mother ion mass-to-charge ratio is 350.08, and qualitative judgement daughter ion mass-to-charge ratio is 106.1/174.06；Tetracycline uses cation mould
Formula, orifice potential 4V, collision voltage 24/22V, qualitatively judging mother ion mass-to-charge ratio is 445.249, qualitatively judges daughter ion
Mass-to-charge ratio is 154.1075/410.1938,
(6) the corresponding peak area of antibiotic isolated is calculated, quantitative calculating is carried out according to standard curve, show that antibiotic contains
Amount.
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| CN109270180A (en) * | 2018-11-01 | 2019-01-25 | 苏州立升净水科技有限公司 | The detection method of antibiotic in soil |
| CN114720572B (en) * | 2020-12-22 | 2023-11-24 | 上海市环境科学研究院 | Method for detecting 15 antibiotics content in fish meat |
| CN114720571B (en) * | 2020-12-22 | 2023-11-24 | 上海市环境科学研究院 | Method for detecting 15 antibiotics in fish body |
| CN114965777A (en) * | 2022-05-27 | 2022-08-30 | 浙江省海洋水产研究所 | Ultra-high performance liquid chromatography tandem mass spectrometry detection method for quinolone antibiotics in sediments |
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| CN102401818B (en) * | 2011-08-25 | 2013-05-22 | 四川农业大学 | High performance liquid chromatography determination method of tetracycline antibiotic in soil, dung and biogas slurry |
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