CN105548382A - Method for detecting benzopyrene in soil - Google Patents
Method for detecting benzopyrene in soil Download PDFInfo
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- CN105548382A CN105548382A CN201510905615.3A CN201510905615A CN105548382A CN 105548382 A CN105548382 A CN 105548382A CN 201510905615 A CN201510905615 A CN 201510905615A CN 105548382 A CN105548382 A CN 105548382A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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Abstract
The invention discloses a method for detecting benzopyrene in soil. The method is characterized by comprising the following steps: accurately weighing a proper amount of an air-dried soil sample and putting the sample into a conical flask provided with a plug; adding an organic solvent A 8-10 times as much as the soil sample, plugging the conical flask, and performing shaking; performing ultrasonic extraction for at least 30 min; collecting a supernatant after centrifugation; in the residual soil sample, adding the organic solvent A 8-10 times as much as the residual soil sample; performing ultrasonic extraction for at least 30 min; performing centrifugation; combining the supernatants; adding the organic solvent A into a solid-phase extraction column for activation; after activation, transferring the combined supernatants into the activated solid-phase extraction column; and performing elution with the organic solvent A. The method is simple in operation and steps; the possibility that a tester inhales benzopyrene or the skin of the tester contacts benzopyrene because of misoperation is reduced, thereby greatly improving the operation safety of the tester.
Description
Technical field
The present invention relates to the detection method of benzopyrene in a kind of soil, belong to method of environmental monitoring technical field.
Background technology
Benzopyrene, also known as benzo (α) pyrene, is a kind of common high activity indirect-acting carcinogen.It enters after in body through breathing or diet, is easy to combine with the DNA of people, has upset the synthesis program of human body protein.It plays the role of " trigger " in the activity of DNA: as long as the benzopyrene of very trace-nanogram rank, just can change the structure of DNA, direction and function; Combine the DNA of benzopyrene, the cell of synthesis is no longer normal cell, but tumour, also just result in cancer.It is at water body, all easily remains in soil and crop.Many countries all carried out benzopyrene investigation of content in soil, and residual concentration depends on the former character of pollution and distance, and in the soil of highway both sides, near refinery in soil and by coal tar, in pitch contaminated soil, the content of benzopyrene is not low.
Benzopyrene harm humans is healthy, and along with the deterioration increasingly of environmental problem, the detection of benzopyrene is more and more subject to people's attention.The method of conventional detection benzopyrene has thin layer chromatography, fluorescence spectrophotometry, vapor-phase chromatography, gas chromatography-mass spectrography, HPLC UV method, stationary phases for HPLC.Wherein fluorescence method has highly sensitive, high repeatability and other advantages, is the method comparatively commonly used.Different according to detected object, be separated, extract, enrichment mode is also different, at present, there has been air in China, national standard assay method in ArsenazoⅢ, but also there is no the detection method of benzopyrene in soil, set up the method for benzopyrene in a kind of accurate, quick, easy detection soil, ecologic environment, health are had great significance.
In addition, in current benzopyrene detection method, the pre-treating method of sample is complicated, complex steps, and be easy to because careless manipulation suction or skin contact are to benzopyrene in pre-treatment sample, this brings great threat to the safety of experimenter.
Summary of the invention
Technical matters to be solved by this invention is, provide a kind of simple and easy to operate, in sample, benzopyrene extracts completely, the detection method of benzopyrene in the soil that testing result is true and reliable.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
In soil, a detection method for benzopyrene, is characterized in that, comprises the following steps:
S01, the preparation of need testing solution: accurately take air-dry after pedotheque in right amount in tool plug conical flask, add the organic solvent A being equivalent to pedotheque 8 ~ 10 times amount, jolting after jumping a queue, ultrasonic extraction at least 30min again, collected after centrifugation supernatant, the organic solvent A being equivalent to pedotheque 8 ~ 10 times amount is added again in residual pedotheque, ultrasonic extraction at least 30min, centrifugal, merge supernatant, get organic solvent A to add solid-phase extraction column and activate, after having activated, the supernatant of merging is transferred in the solid-phase extraction column after activation, use organic solvent A wash-out, collect eluent to measuring bottle, constant volume, cross 0.45um miillpore filter to sample injection bottle, for subsequent use,
S02, the preparation of standard solution: compound concentration is the benzopyrene standard serial solution of 0.05,0.1,0.2,0.3,0.4 μ g/L, and constant volume solution is organic solvent A, shakes up rear 0.45um miillpore filter of crossing to sample injection bottle, for subsequent use;
S03, detects: successively benzopyrene standard serial solution and need testing solution being injected HPLC, HPLC testing conditions is: ODS post; Column temperature: 30 DEG C; Mobile phase: acetonitrile: water=77:23; Fluorescence detector: excitation wavelength 290nm, emission wavelength 430nm.
Described organic solvent A comprises any one in chloroform, acetone, benzene,toluene,xylene, ether, normal hexane, sherwood oil and cyclohexane.
Need seal with the bottleneck of sealed membrane by tool plug conical flask during ultrasonic extraction.
The order number of described pedotheque is 120 ~ 200 orders.
Described pedotheque also comprises pre-treatment step, adopts grid to arrange method sampling, at least gets 16 points, the section of each point samples respectively to veneer of soil, underearth.
Described centrifugal be 10000r/min, the time is at least 3min.
The activity of described solid-phase extraction column completes standard and is: get organic solvent A and add solid-phase extraction column and activate, be no less than 12 ~ 15ml to naturally lower of organic solvent A, activation completes.
The detection method of benzopyrene in a kind of soil provided by the invention, ultrasonic extraction twice rear method with the benzopyrene in solid-phase extraction column enriching and purifying pedotheque, this method is easy and simple to handle, step is simple, decrease people for maloperation cause sucking or skin contact to the probability of benzopyrene, substantially increase the security of experimenter's work, and this method benzopyrene extracts completely, and obtain certain purification effect, make to enter inclusion-free peak interference when high performance liquid chromatography detects, testing result is accurate, true and reliable.
Embodiment
Below the present invention is further described.
Embodiment 1:
Instrument: Agilent high performance liquid chromatograph, 1200 types; Chromatographic column is ODS post (5 μm, 4.6mm*150mm); Mobile phase: acetonitrile-water; Sample size: 10 μ L; Detecting device is fluorescence detector, excitation wavelength 290nm, emission wavelength 430nm.
Reagent: experiment agents useful for same is to be analyzed pure or top grade is pure, and water used is Millipore ultrapure water.
Benzopyrene standard items: purchased from Chinese medicine standard reference material research centre.
Reference material of soil: GSBZ50012-88(ESS-2) purchased from China Environmental Monitoring General Station and GBW07453(GSS-24), purchased from State Standard Matter Research Centre (Beijing).
1# sample and 2# sample: to pick up near refinery soil respectively and by coal tar, pitch contaminated soil.
In soil, a detection method for benzopyrene, is characterized in that, comprises the following steps:
S01, the preparation of need testing solution: accurately take air-dry after pedotheque 2g in 30ml tool plug conical flask, add 16ml chloroform, jolting after jumping a queue, ultrasonic extraction 30min again, collected after centrifugation supernatant, 16ml chloroform is added again in residual pedotheque, ultrasonic extraction 30min, centrifugal, merge supernatant, get chloroform to add solid-phase extraction column and activate, after having activated, the supernatant of merging is transferred in the solid-phase extraction column after activation, use chloroform wash-out, collect eluent to 50ml measuring bottle, chloroform is settled to scale, shake up, cross 0.45um miillpore filter to sample injection bottle, for subsequent use,
S02, the preparation of standard solution: compound concentration is the benzopyrene standard serial solution of 0.05,0.1,0.2,0.3,0.4 μ g/L, and constant volume solution is chloroform, shakes up rear 0.45um miillpore filter of crossing to sample injection bottle, for subsequent use;
S03, detects: successively benzopyrene standard serial solution and need testing solution being injected HPLC, HPLC testing conditions is: ODS post; Column temperature: 30 DEG C; Mobile phase: acetonitrile: water=77:23; Fluorescence detector: excitation wavelength 290nm, emission wavelength 430nm.
Need seal with the bottleneck of sealed membrane by tool plug conical flask during ultrasonic extraction.
The order number of described pedotheque is 120 orders.
Described pedotheque also comprises pre-treatment step, adopts grid to arrange method sampling, at least gets 16 points, the section of each point samples respectively to veneer of soil, underearth.
Described centrifugal be 10000r/min, the time is 3min.
The activity of described solid-phase extraction column completes standard and is: get organic solvent A and add solid-phase extraction column and activate, be no less than 12ml to naturally lower of organic solvent A, activation completes.
Testing result:
Typical curve is Y=3.982X+0.204(R
2=1), illustrate that benzopyrene is good in the scope internal linear relation of 0.05 ~ 0.4 μ g/L, after Precision Experiment, stability test, replica test and average recovery test, find that each experimental result of this detection method is all good, can be used to detect the benzopyrene content in pedotheque, average recovery test findings well illustrates that the benzopyrene in pedotheque of the present invention extracts completely, and testing result is true and reliable.
After testing, soil and by coal tar near refinery, the benzopyrene content in pitch contaminated soil is all greater than the benzopyrene upper content limit 0.01ug/L that national standard specifies Drinking Water water quality standard, illustrates that these two local soil are not suitable for planting farming.
Embodiment 2:
Instrument: Agilent high performance liquid chromatograph, 1200 types; Chromatographic column is ODS post (5 μm, 4.6mm*150mm); Mobile phase: acetonitrile-water; Sample size: 10 μ L; Detecting device is fluorescence detector, excitation wavelength 290nm, emission wavelength 430nm.
Reagent: experiment agents useful for same is to be analyzed pure or top grade is pure, and water used is Millipore ultrapure water.
Benzopyrene standard items: purchased from Chinese medicine standard reference material research centre.
Reference material of soil: GSBZ50012-88(ESS-2) purchased from China Environmental Monitoring General Station and GBW07453(GSS-24), purchased from State Standard Matter Research Centre (Beijing).
1# sample and 2# sample: to pick up near refinery soil respectively and by coal tar, pitch contaminated soil.
In soil, a detection method for benzopyrene, is characterized in that, comprises the following steps:
S01, the preparation of need testing solution: accurately take air-dry after pedotheque 2g in 30ml tool plug conical flask, add 20ml normal hexane, jolting after jumping a queue, ultrasonic extraction 40min again, collected after centrifugation supernatant, 20ml normal hexane is added again in residual pedotheque, ultrasonic extraction 40min, centrifugal, merge supernatant, get normal hexane to add solid-phase extraction column and activate, after having activated, the supernatant of merging is transferred in the solid-phase extraction column after activation, with hexane, collect eluent to 50ml measuring bottle, normal hexane is settled to scale, shake up, cross 0.45um miillpore filter to sample injection bottle, for subsequent use,
S02, the preparation of standard solution: compound concentration is the benzopyrene standard serial solution of 0.05,0.1,0.2,0.3,0.4 μ g/L, and constant volume solution is normal hexane, shakes up rear 0.45um miillpore filter of crossing to sample injection bottle, for subsequent use;
S03, detects: successively benzopyrene standard serial solution and need testing solution being injected HPLC, HPLC testing conditions is: ODS post; Column temperature: 30 DEG C; Mobile phase: acetonitrile: water=77:23; Fluorescence detector: excitation wavelength 290nm, emission wavelength 430nm.
Need seal with the bottleneck of sealed membrane by tool plug conical flask during ultrasonic extraction.
The order number of described pedotheque is 200 orders.
Described pedotheque also comprises pre-treatment step, adopts grid to arrange method sampling, at least gets 16 points, the section of each point samples respectively to veneer of soil, underearth.
Described centrifugal be 10000r/min, the time is 5min.
The activity of described solid-phase extraction column completes standard and is: get organic solvent A and add solid-phase extraction column and activate, be no less than 15ml to naturally lower of organic solvent A, activation completes.
After testing, soil and by coal tar near refinery, the benzopyrene content in pitch contaminated soil is all greater than the benzopyrene upper content limit 0.01ug/L that national standard specifies Drinking Water water quality standard, illustrates that these two local soil are not suitable for planting farming.
The above is only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (7)
1. the detection method of benzopyrene in soil, is characterized in that, comprise the following steps:
S01, the preparation of need testing solution: accurately take air-dry after pedotheque in right amount in tool plug conical flask, add the organic solvent A being equivalent to pedotheque 8 ~ 10 times amount, jolting after jumping a queue, ultrasonic extraction at least 30min again, collected after centrifugation supernatant, the organic solvent A being equivalent to pedotheque 8 ~ 10 times amount is added again in residual pedotheque, ultrasonic extraction at least 30min, centrifugal, merge supernatant, get organic solvent A to add solid-phase extraction column and activate, after having activated, the supernatant of merging is transferred in the solid-phase extraction column after activation, use organic solvent A wash-out, collect eluent to measuring bottle, constant volume, cross 0.45um miillpore filter to sample injection bottle, for subsequent use,
S02, the preparation of standard solution: compound concentration is the benzopyrene standard serial solution of 0.05,0.1,0.2,0.3,0.4 μ g/L, and constant volume solution is organic solvent A, shakes up rear 0.45um miillpore filter of crossing to sample injection bottle, for subsequent use;
S03, detects: successively benzopyrene standard serial solution and need testing solution being injected HPLC, HPLC testing conditions is: ODS post; Column temperature: 30 DEG C; Mobile phase: acetonitrile: water=77:23; Fluorescence detector: excitation wavelength 290nm, emission wavelength 430nm.
2. the detection method of benzopyrene in a kind of soil according to claim 1, is characterized in that: described organic solvent A comprises any one in chloroform, acetone, benzene,toluene,xylene, ether, normal hexane, sherwood oil and cyclohexane.
3. the detection method of benzopyrene in a kind of soil according to claim 1, is characterized in that: need seal with the bottleneck of sealed membrane by tool plug conical flask during ultrasonic extraction.
4. the detection method of benzopyrene in a kind of soil according to claim 1, is characterized in that: the order number of described pedotheque is 120 ~ 200 orders.
5. the detection method of benzopyrene in a kind of soil according to claim 1, it is characterized in that: described pedotheque also comprises pre-treatment step, adopt grid to arrange method sampling, at least get 16 points, the section of each point samples respectively to veneer of soil, underearth.
6. the detection method of benzopyrene in a kind of soil according to claim 1, is characterized in that: described centrifugal be 10000r/min, the time is at least 3min.
7. the detection method of benzopyrene in a kind of soil according to claim 1, it is characterized in that: the activity of described solid-phase extraction column completes standard and is: get organic solvent A and add solid-phase extraction column and activate, be no less than 12 ~ 15ml to naturally lower of organic solvent A, activation completes.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106501411A (en) * | 2016-11-04 | 2017-03-15 | 无锡艾科瑞思产品设计与研究有限公司 | A kind of method for quick of benzopyrene from edible oil |
| CN109444009A (en) * | 2018-12-10 | 2019-03-08 | 红云红河烟草(集团)有限责任公司 | Online direct measurement equipment for benzopyrene in atmospheric environment |
| CN111272903A (en) * | 2020-03-17 | 2020-06-12 | 江苏中气环境科技有限公司 | Detection method for determining content of benzopyrene in fixed pollution source by high performance liquid chromatography |
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| CN103808816A (en) * | 2012-11-13 | 2014-05-21 | 云南健牛生物科技有限公司 | New method for quickly detecting benzopyrene in soil |
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- 2015-12-10 CN CN201510905615.3A patent/CN105548382A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103808816A (en) * | 2012-11-13 | 2014-05-21 | 云南健牛生物科技有限公司 | New method for quickly detecting benzopyrene in soil |
Non-Patent Citations (4)
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| JAMES B.BEACH ET AL.: "Determination of Benzo[a]pyrene and Other Polycyclic Aromatic Hydrocarbons (PAHs) at Trace Levels in Human Tissues", 《JOURNAL OF ANALYTICAL TOXICOLOGY》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106501411A (en) * | 2016-11-04 | 2017-03-15 | 无锡艾科瑞思产品设计与研究有限公司 | A kind of method for quick of benzopyrene from edible oil |
| CN109444009A (en) * | 2018-12-10 | 2019-03-08 | 红云红河烟草(集团)有限责任公司 | Online direct measurement equipment for benzopyrene in atmospheric environment |
| CN109444009B (en) * | 2018-12-10 | 2024-02-20 | 红云红河烟草(集团)有限责任公司 | On-line direct test equipment for benzopyrene in atmospheric environment |
| CN111272903A (en) * | 2020-03-17 | 2020-06-12 | 江苏中气环境科技有限公司 | Detection method for determining content of benzopyrene in fixed pollution source by high performance liquid chromatography |
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Application publication date: 20160504 |