CN107300597A - The detection method of the sulfonic acid of 2 phenylbenzimidazol 5 in a kind of soil - Google Patents
The detection method of the sulfonic acid of 2 phenylbenzimidazol 5 in a kind of soil Download PDFInfo
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- CN107300597A CN107300597A CN201710671617.XA CN201710671617A CN107300597A CN 107300597 A CN107300597 A CN 107300597A CN 201710671617 A CN201710671617 A CN 201710671617A CN 107300597 A CN107300597 A CN 107300597A
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Abstract
The invention belongs to environmental analysis field, the detection method of the sulfonic acid of 2 phenylbenzimidazol 5 in specifically related to a kind of soil, research currently for PBSA is concentrated mainly on contents level in cosmetics and product, and mechanism of degradation is studied in water environment, but PBSA detection method research and contents level research almost blank in soil, therefore, in order to understand the concentration level and environmental behaviour of PBSA in soil environment, need to set up a kind of efficient quick, the high analysis method of sensitivity, qualitative and quantitative detection for the sulfonic acid of 2 phenylbenzimidazol of trace in soil 5, the purpose of invention is to provide a kind of analyzing detecting method of the sulfonic acid of 2 phenylbenzimidazol 5 (PBSA) in soil, in particular it is to use ultrasonic extraction, silica gel column chromatography column purification and the analysis method of high performance liquid chromatography GC-MS detection.
Description
First, technical field
The invention belongs to environmental analysis field, and in particular to 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID in a kind of soil
Detection method.
2nd, background technology
In recent years, because whitening and ultraviolet protection are increasingly valued by people, the use increasingly frequency of sun-screening agent
It is numerous.Sun-screening agent after use, as people's activity can be directly entered in environment, or is introduced into town sewage on people's skin
In processing system, then being discharged into environment with sludge and sewage.Many researchs show that sun-screening agent can be in many water rings
Detected in border, as a kind of emerging pollutant, have been received by the attention of environmental administration and Environmental Scientific Research worker.Some research tables
Bright, Orangic sunscreen has endocrine disrupting and bioaccumulation in the environment, has to environment potentially hazardous.
2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID (2-Phenylbenzimidazole-5-sulfonic acid, abbreviation PBSA)
It is a kind of conventional sun-screening agent, due to its excellent sun-proof performance, is widely used in sun care preparations.
The essential information of the 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID of table 1
Research currently for PBSA is concentrated mainly on contents level in cosmetics and product, and is dropped in water environment
Study mechanism is solved, but PBSA detection method research and contents level in soil study almost blank.Therefore, to know clearly
PBSA concentration level and environmental behaviour is, it is necessary to set up the high analysis side of a kind of efficient quick, sensitivity in solution soil environment
Method, the qualitative and quantitative detection for trace 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID in soil.
3rd, the content of the invention
The purpose of invention is to be directed to problem above and deficiency, is to provide 2-Phenylbenzimidazole -5- sulphurs in a kind of soil
The analyzing detecting method of sour (PBSA), is in particular to use ultrasonic extraction, silica gel column chromatography column purification and high performance liquid chromatography
The analysis method of GC-MS detection.
Technical scheme comprises the following steps：
(1) ultrasonic extraction
After collecting soil sample, dry and remove the larger impurity such as stone cleaning and plant tissue, grinding sieving.Weigh soil
Inner mark solution is added dropwise in centrifuge tube with cover in earth sample, treats that solvent volatilizees；Extractant is added, lid is tightened, is well mixed
Afterwards, ultrasonic extraction, is centrifuged, and draws supernatant liquor in pear-shaped flask；Extraction step is repeated, extract is incorporated in pears
In shape flask, and rotary evaporated to dryness.
(2) silica gel column chromatography column purification
Load a small amount of mineral wool in glass chromatography column bottom, sequentially add after silica gel and anhydrous sodium sulfate, flat surface,
Add solvent cleaning and activated silica gel.Solvent is added into pear-shaped flask to dissolve again, and solution is transferred to silica gel column chromatography
In；The part efflux needed for chromatographic column is received with glass tube, is dried up in nitrogen evaporator.1mL methanol is added into glass tube
Again dissolve, after filtering, to preserve to be measured in 2mL brown sample introduction bottles.
(3) standard working solution is prepared
The standard substance of PBSA and internal standard compound is weighed with assay balance, storing solution is made into respectively, and it is molten to be diluted to work
Liquid, is finally configured to the standard working solution of gradient concentration.
(4) high performance liquid chromatography GC-MS is detected
The standard working solution of gradient concentration is determined in high performance liquid chromatography GC-MS, built using internal standard method
Vertical standard working curve.The sample solution in step (2) is injected in high performance liquid chromatography GC-MS under the same conditions
It is measured, the chromatographic peak area of target compound in sample is substituted into standard working curve, obtains the qualitative of PBSA in sample
Quantitative result.If the PBSA concentration working curve range of linearity that is above standard is reached the standard grade in sample, sample size weight should be accordingly reduced
New extraction and cleaning and detection.
In step (1), it is preferred to use freeze-drying, sample grinding consequence 0.90mm sieves, sealing preserve is in 4 DEG C
Environment in.
In step (1), pedotheque amount is preferably 5~10g.
In step (1), internal standard compound is preferably 2- methyl -4- chlorine amoxy propionic acid (mecoprop).
In step (1), extractant is the mixed solvent of ethyl acetate and formic acid, and both volume ratios are 50:1~100:
1。
In step (1), specific extraction process tightens lid to add 7~10mL of extractant, and vortex mixed 30s surpasses
Sound extracts 15~20min, 2500rpm centrifugation 15min, draws supernatant liquor in pear-shaped flask, repeats extraction 2~3 times,
Combining extraction liquid is in pear-shaped flask, rotary evaporated to dryness.
In step (2), silica gel and anhydrous sodium sulfate are respectively 1.0g and 0.5g.
In step (2), silica gel activating concrete operations are：Sequentially add 10mL methanol, 10 mL ethyl acetate and 10mL just oneself
Alkane, liquid level cannot be below interface on anhydrous sodium sulfate during noting.
In step (2), sample solution is added and the detailed process of elution is：Into pear-shaped flask add 2~3mL just oneself
Alkane is dissolved again, and solution is transferred in silica gel column chromatography, discards efflux, repeats step 2 time；Into pear-shaped flask
Add 2~3mL ethyl acetate to dissolve again, and solution is transferred in silica gel column chromatography, efflux is received with glass tube, then
Repeat step 2 times, merges efflux, is dried up in nitrogen evaporator.
In step (3), internal standard compound preferably is 2- methyl -4- chlorine amoxy propionic acid (mecoprop), standard working curve
Gradient concentration at least five more than.
In step (4), chromatographic condition preferably is as follows：Chromatographic column is Agilent SB-C18 (3.0 × 100mm, 1.8 μ
M), column temperature is 40 DEG C, and mobile phase is water (A) and acetonitrile (B)；Gradient elution program is the Mobile phase Bs of 0~2min 50~90%, 2
The Mobile phase Bs of~5min 90%, flow velocity 0.30mL/min.
In step (4), Mass Spectrometry Conditions preferably are as follows：Electro-spray ionization ion gun (ESI) negative mode；Dry temperature
300 DEG C of degree, flow velocity 3mL/min；The psi of nebulizer pressure 30；250 DEG C of sheath temperature degree, flow velocity 11mL/min；Capillary voltage
3000V, spray nozzle voltage 1000V.On this condition, PBSA and interior target mass spectrometry parameters are as shown in table 2.
Table 2PBSA and the interior mass spectrometry parameters for being marked on high performance liquid chromatography mass spectrometry
A runics are quota ion
The present invention is built using ultrasonic extraction, silica gel column chromatography column purification and high performance liquid chromatography GC-MS detection technique
Found the analyzing detecting method of 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID, effectively to the trace 2-Phenylbenzimidazole in soil-
5- sulfonic acid carries out qualitative and quantitative detection, and the present invention has following innovative point.
(1) polarity of 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID is stronger, and the present invention uses the ethyl acetate conduct that formic acid is acidified
Extraction solvent, can suppress ionization of the 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID in extraction process, increase the rate of recovery, while in
The ethyl acetate solvent of isopolarity can reduce the undue extraction of chaff interference in soil, reduce the matrix interference of method, improve
Sensitivity.
(2) soil matrix is complicated, for the matrix interference of method, and the present invention uses homemade silica gel column chromatography column purification, first
Non polar impurities are eluted using n-hexane, then target compound 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID is eluted with ethyl acetate, are reached
To purification purpose, method sensitivity is further increased.
(3) present invention uses inner mark method ration, after instrument condition optimizes, the internal standard compound 2- methyl -4- chlorine penta of selection
Epoxide propionic acid and the target compound peak type in instrument are good, and retention time is close, and is added to before extraction in sample,
Counteract in the error caused by target compound loses in extraction process, many experiments and all achieve the good rate of recovery.
(4) China is less to the 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID concern in soil environment at present, due to soil environment
Matrix is complicated, and conventional method of analysis serious interference causes analysis difficulty, and its analysis and detection technology is still in technological gap.This hair
The detection technique of the bright 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID from a set of soil is provided in terms of extraction, purification and Instrumental Analysis,
Average recovery rate is 91.8%~92.1%, and detection is limited to 0.19~0.22ng/g, is quantitatively limited to 0.64~0.74ng/g, is fitted
Analysis detection for 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID in soil.
The beneficial effect of the present invention is to set up the high analysis method of a kind of efficient quick, sensitivity, for trace 2- in soil
The qualitative and quantitative detection of phenylbenzimidazol -5- sulfonic acid
Brief description of the drawings
Fig. 1 is 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID (PBSA) and 2- methyl -4- chlorine amoxy propionic acid (mecoprop)
Characteristic ion flow graph.
5th, embodiment
Embodiment 1
(1) ultrasonic extraction
Collecting soil sample 100g, is freeze-dried and removes stone cleaning and the larger impurity such as plant tissue, ground
0.90mm is sieved.5g pedotheques are weighed in centrifuge tube with cover, the 100 μ L 1mg/L oxygen of internal standard compound 2- methyl -4- chlorine penta is added dropwise
Base propionic acid working solution, treats that solvent volatilizees；Add 10mL ethyl acetate and formic acid mixed solvent (volume ratio 50:1) lid, is tightened
Son, vortex mixed 30s, ultrasonic extraction 15min, 2500rpm centrifugation 15min, draws supernatant liquor in pear-shaped flask, then weigh
Extract 2 times again, combining extraction liquid is in pear-shaped flask, 45 DEG C of rotary evaporated to dryness.
(2) silica gel column chromatography column purification
Load a small amount of mineral wool in glass chromatography column bottom, sequentially add 1g silica gel and 0.5g anhydrous sodium sulfates, rap glass
Glass post flat surface, sequentially adds 10mL methanol, 10mL ethyl acetate and 10mL n-hexane activated silica gel posts, during noting
Liquid level cannot be below interface on anhydrous sodium sulfate.2mL n-hexanes are added into pear-shaped flask to dissolve again, and solution is shifted
Into silica gel column chromatography, efflux is discarded, step 2 time is repeated；2mL ethyl acetate is added into pear-shaped flask to dissolve again,
And solution is transferred in silica gel column chromatography, efflux is received with glass tube, step 2 time is repeated, merges efflux, in nitrogen
Blow in instrument and dry up.1mL methanol is added into glass tube to dissolve again, after filtering, is treated with being preserved in 2mL brown sample introduction bottles
Survey.
(3) standard working solution is prepared
The reference material of 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID and 2- methyl -4- chlorine amoxy propionic acid is weighed with assay balance
Matter, 100mg/L stock solutions are configured to methanol and 1 mg/L working solutions are diluted to respectively, be finally configured to concentration for 1,5,
10th, 20,50,100 and 200 μ g/L standard working solution, wherein internal standard compound concentration are 100 μ g/L.
(4) high performance liquid chromatography GC-MS is detected
The standard working solution of gradient concentration is determined in high performance liquid chromatography GC-MS, built using internal standard method
Vertical standard working curve.The sample solution in step (2) is injected in high performance liquid chromatography GC-MS under the same conditions
It is measured, the chromatographic peak area of target compound in sample is substituted into standard working curve, obtains the qualitative of PBSA in sample
Quantitative result.
Qualitative Identification：Under the conditions of same instruments, if the chromatographic peak of 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID retains in sample
Time is consistent with the retention time in standard working solution, and qualitative and quota ion pair abundance ratio and standard liquid
Equally, then it can determine whether there is 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID in sample.
Quantitative analysis：Standard working curve, the μ g/L of the range of linearity 0~200, standard curve phase relation are set up with internal standard method
Number>0.999, the concentration of 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID in sample solution is calculated by software, is finally calculated by sample size
The concentration of 2-Phenylbenzimidazole -5- sulfonic acid in sample.
Recovery of standard addition, repeatability and matrix effect：
The rate of recovery uses 3 parallel mark-ons, and mark-on method is：100 μ L 1mg/L 2- are added in 5.0g pedotheques
Phenylbenzimidazol -5- sulfonic acid standard liquids so that the concentration of 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID is 20ng/g in sample, etc.
30min is treated, after solvent volatilization completely, is extracted and is detected.The mark-on sample concentration of practical measurement is subtracted into blank sample dense
Degree, and be compared with theory addition concentration, the rate of recovery of 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID is obtained, with 3 parallel mark-ons
As a result standard deviation method for expressing repeatability.Matrix effect is tested by the following method：Blank sample is extracted and is concentrated into
After 1mL, 100 μ L sample solution is taken in sample introduction bottle, is dried up on nitrogen evaporator, and it is respectively 100 μ to add 100 μ L concentration
G/L 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID and the mixed standard solution of 2- methyl -4- chlorine amoxy propionic acid, vortex mixing are equal
It is even, upper machine testing.The mark-on sample concentration of practical measurement is subtracted into blank sample concentration, and compared with theory addition concentration
Compared with obtaining the matrix effect result of method.Recovery of standard addition, repeatability and the matrix effect of method the results are shown in Table shown in 3, can
To find out, in the case that spiked levels are 20ng/g in soil, the average recovery rate of 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID is
91.8%, standard deviation is 1.4%, and matrix effect is 92.2%, and the illustration method rate of recovery and reproducible, matrix interference are low,
Detection available for pedotheque.
Detection limit and quantitative limit：
Corresponding concentration is detection limit when signal to noise ratio is 3, and corresponding concentration is quantitative limit when signal to noise ratio is 10, specific behaviour
As：The signal to noise ratio under spiked levels is calculated by data processing software, with the spiked levels divided by signal to noise ratio, the result
3 times be method test limit, 10 times be quantitative limit.The detection limit and quantitative limit result of method are as shown in table 3, it can be seen that soil
In the case that spiked levels are 20ng/g in earth, the detection of 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID is limited to 0.19ng/g, quantitative limit
For 0.64ng/g, illustrate that the sensitivity of this detection method is high, available for trace 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID in pedotheque
Detection.
The method rate of recovery of table 3, matrix effect, detection limit and quantitative limit
aAverage value ± standard deviation (%) (n=3)；bAverage value ± standard deviation (%) (n=3)；c(ng/g)；d(ng/
g)
Embodiment 2
(1) ultrasonic extraction
Collecting soil sample 100g, is freeze-dried and removes stone cleaning and the larger impurity such as plant tissue, ground
0.90mm is sieved.10g pedotheques are weighed in centrifuge tube with cover, 100 μ L 1mg/L internal standard compound 2- methyl -4- chlorine penta is added dropwise
Epoxide propionic acid working solution, treats that solvent volatilizees；Add 10mL ethyl acetate and formic acid mixed solvent (volume ratio 100:1), tighten
Lid, vortex mixed 30s, ultrasonic extraction 15min, 2500rpm centrifugation 15min, draws supernatant liquor in pear-shaped flask, then
Repeat to extract 2 times, combining extraction liquid is in pear-shaped flask, 45 DEG C of rotary evaporated to dryness.
(2) silica gel column chromatography column purification
Load a small amount of mineral wool in glass chromatography column bottom, sequentially add 1g silica gel and 0.5g anhydrous sodium sulfates, rap glass
Glass post flat surface, sequentially adds 10mL methanol, 10mL ethyl acetate and 10mL n-hexane activated silica gel posts, during noting
Liquid level cannot be below interface on anhydrous sodium sulfate.2mL n-hexanes are added into pear-shaped flask to dissolve again, and solution is shifted
Into silica gel column chromatography, efflux is discarded, step 2 time is repeated；2mL ethyl acetate is added into pear-shaped flask to dissolve again,
And solution is transferred in silica gel column chromatography, efflux is received with glass tube, step 2 time is repeated, merges efflux, in nitrogen
Blow in instrument and dry up.1mL methanol is added into glass tube to dissolve again, after filtering, is treated with being preserved in 2mL brown sample introduction bottles
Survey.
(3) standard working solution is prepared
The reference material of 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID and 2- methyl -4- chlorine amoxy propionic acid is weighed with assay balance
Matter, 100mg/L stock solutions are configured to methanol and 1 mg/L working solutions are diluted to respectively, be finally configured to concentration for 1,5,
10th, 20,50,100 and 200 μ g/L standard working solution, wherein internal standard compound concentration are 100 μ g/L.
(4) high performance liquid chromatography GC-MS is detected
The standard working solution of gradient concentration is determined in high performance liquid chromatography GC-MS, built using internal standard method
Vertical standard working curve.The sample solution in step (2) is injected in high performance liquid chromatography GC-MS under the same conditions
It is measured, the chromatographic peak area of target compound in sample is substituted into standard working curve, obtains the qualitative of PBSA in sample
Quantitative result.
Qualitative Identification：Under the conditions of same instruments, if the chromatographic peak of 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID retains in sample
Time is consistent with the retention time in standard working solution, and qualitative and quota ion pair abundance ratio and standard liquid
Equally, then it can determine whether there is 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID in sample.
Quantitative analysis：Standard working curve, the μ g/L of the range of linearity 0~200, standard curve phase relation are set up with internal standard method
Number>0.999, the concentration of 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID in sample solution is calculated by software, is finally calculated by sample size
The concentration of 2-Phenylbenzimidazole -5- sulfonic acid in sample.
Recovery of standard addition, repeatability and matrix effect：
The rate of recovery uses 3 parallel mark-ons, and mark-on method is：100 μ L 1mg/L 2- are added in 10.0g pedotheques
Phenylbenzimidazol -5- sulfonic acid standard liquids so that the concentration of 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID is 10ng/g in sample, etc.
30min is treated, after solvent volatilization completely, is extracted and is detected.The mark-on sample concentration of practical measurement is subtracted into blank sample dense
Degree, and be compared with theory addition concentration, the rate of recovery of 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID is obtained, with 3 parallel mark-ons
As a result standard deviation method for expressing repeatability.Matrix effect is tested by the following method：Blank sample is extracted and is concentrated into
After 1mL, 100 μ L sample solution is taken in sample introduction bottle, is dried up on nitrogen evaporator, and it is respectively 100 μ to add 100 μ L concentration
G/L 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID and the mixed standard solution of 2- methyl -4- chlorine amoxy propionic acid, vortex mixing are equal
It is even, upper machine testing.The mark-on sample concentration of practical measurement is subtracted into blank sample concentration, and compared with theory addition concentration
Compared with obtaining the matrix effect result of method.Recovery of standard addition, repeatability and the matrix effect of method the results are shown in Table shown in 4, can
To find out, in the case that spiked levels are 10ng/g in soil, the average recovery rate of 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID is
90.5%, standard deviation is 1.2%, and matrix effect is 91.1%, and the illustration method rate of recovery and reproducible, matrix interference are low,
Detection available for pedotheque.
Detection limit and quantitative limit：
Corresponding concentration is detection limit when signal to noise ratio is 3, and corresponding concentration is quantitative limit when signal to noise ratio is 10, specific behaviour
As：The signal to noise ratio under spiked levels is calculated by data processing software, with the spiked levels divided by signal to noise ratio, the result
3 times be method test limit, 10 times be quantitative limit.The detection limit and quantitative limit result of method are as shown in table 4, it can be seen that soil
In the case that spiked levels are 10ng/g in earth, the detection of 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID is limited to 0.22ng/g, quantitative limit
For 0.74ng/g, illustrate that the sensitivity of this detection method is high, available for trace 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID in pedotheque
Detection.
The method rate of recovery of table 4, matrix effect, detection limit and quantitative limit
aAverage value ± standard deviation (%) (n=3)；bAverage value ± standard deviation (%) (n=3)；c(ng/g)；d(ng/
g)
Above-described embodiment is preferably embodiment, but embodiments of the present invention are not by above-described embodiment of the invention
Limitation, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, it is simple
Change, should be equivalent substitute mode, be included within protection scope of the present invention.
Claims (4)
1. the detection method of 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID in a kind of soil, it is characterised in that comprise the following steps：
(1) ultrasonic extraction
After collecting soil sample, dry and remove the larger impurity such as stone cleaning and plant tissue, grinding sieving weighs pedotheque
In centrifuge tube with cover, inner mark solution is added dropwise, treats that solvent volatilizees；Extractant is added, lid is tightened, after being well mixed, ultrasound
Extraction, is centrifuged, and draws supernatant liquor in pear-shaped flask；Extract is incorporated in pear-shaped flask, and rotary evaporation is extremely
It is dry；
(2) silica gel column chromatography column purification
Load a small amount of mineral wool in glass chromatography column bottom, sequentially add after silica gel and anhydrous sodium sulfate, flat surface, add molten
Agent cleaning and activated silica gel, into pear-shaped flask, addition solvent is dissolved again, and solution is transferred in silica gel column chromatography；Use glass
Glass pipe receives the part efflux needed for chromatographic column, is dried up in nitrogen evaporator, 1mL methanol is added into glass tube again molten
Solution, after filtering, into glass tube, addition 1mL methanol dissolves again, molten as sample using in 2mL brown sample introduction bottles after filtering
Liquid preserves to be measured；
(3) standard working solution is prepared
The standard substance of PBSA and internal standard compound is weighed with assay balance, storing solution is made into respectively, and is diluted to working solution, is prepared
Into the standard working solution of gradient concentration；
(4) liquid chromatography mass combined instrument is detected
The standard working solution of gradient concentration is determined in liquid chromatography mass combined instrument, setting up standard using internal standard method works
Curve, the sample solution in step (2) is injected and is measured in liquid chromatography mass combined instrument, by target compound in sample
Chromatographic peak area substitute into standard working curve, obtain the qualitative, quantitative result of PBSA in sample.
2. according to claim 1 in a kind of soil 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID detection method, it is characterized in that：Institute
State in step (1), drying means uses freeze-drying, crosses 0.90mm sieves after sample grinding, sealing preserve is in 4 DEG C of environment
In, in the step (1), pedotheque amount is 5~10g, in the step (1), and inner mark solution is preferably 2- methyl -4- chlorine penta
In epoxide propionic acid, the step (1), extractant is the mixed solvent of ethyl acetate and formic acid, and both volume ratios are 50:1~
100:1, in the step (1), 7~10mL of extractant is added, lid is tightened, vortex mixed 30s, ultrasonic extraction 15~
20min, 2500rpm centrifuge 15min, draw supernatant liquor in pear-shaped flask, repeat extraction 2~3 times, combining extraction liquid in
In pear-shaped flask, rotary evaporated to dryness.
3. according to claim 1 in a kind of soil 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID detection method, it is characterized in that：Institute
State in step (2), silica gel and anhydrous sodium sulfate are respectively the specific behaviour of activated silica gel making in 1.0g and 0.5g, the step (2)
As：Sequentially add 10mL methanol, 10mL ethyl acetate and 10mL n-hexanes, during liquid level cannot be below on anhydrous sodium sulfate
Sample solution is added in interface, the step (2) and the detailed process of elution is：2~3mL n-hexanes are added into pear-shaped flask
Again dissolve, and solution is transferred in silica gel column chromatography, discard efflux, repeat step 2 time；Added into pear-shaped flask
2~3mL ethyl acetate is dissolved again, and solution is transferred in silica gel column chromatography, is received efflux with glass tube, is repeated step
Rapid 2 times, merge efflux, dried up in nitrogen evaporator.
4. according to claim 1 in a kind of soil 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID detection method, it is characterized in that, institute
State in step (3), internal standard compound is 2- methyl -4- chlorine amoxy propionic acid, more than gradient concentration at least five of standard working curve,
In the step (4), chromatographic condition is as follows：Chromatographic column is that Agilent SB-C18 column temperatures are 40 DEG C, and mobile phase is water (A) and second
Nitrile (B)；Gradient elution program is the Mobile phase Bs of 0~2min 50~90%, the Mobile phase Bs of 2~5min 90%, flow velocity 0.30mL/
Mass Spectrometry Conditions are as follows in min, the step (4)：Electro-spray ionization ion gun (ESI) negative mode；300 DEG C of temperature degree is dried,
Flow velocity 3mL/min；Nebulizer pressure 30psi；250 DEG C of sheath temperature degree, flow velocity 11mL/min；Capillary voltage 3000V, nozzle electricity
Press 1000V.
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