CN105784910A - Method for detecting PAHs (polycyclic aromatic hydrocarbons) in soil and plants through connecting HPLC (high performance liquid chromatography)/ultraviolet-fluorescence detectors in series - Google Patents
Method for detecting PAHs (polycyclic aromatic hydrocarbons) in soil and plants through connecting HPLC (high performance liquid chromatography)/ultraviolet-fluorescence detectors in series Download PDFInfo
- Publication number
- CN105784910A CN105784910A CN201610305140.9A CN201610305140A CN105784910A CN 105784910 A CN105784910 A CN 105784910A CN 201610305140 A CN201610305140 A CN 201610305140A CN 105784910 A CN105784910 A CN 105784910A
- Authority
- CN
- China
- Prior art keywords
- pahs
- soil
- hplc
- sample
- plant
- 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.)
- Pending
Links
Classifications
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
Abstract
The invention discloses a method for detecting PAHs (polycyclic aromatic hydrocarbons) in soil and plants through connecting HPLC (high performance liquid chromatography)/ultraviolet-fluorescence detectors in series, and belongs to the field of analysis and detection. The method comprises the following steps that an ultraviolet extraction method is used for extraction; HPLC/UV-FLD is combined for separating and analyzing the PAHs the soil and plant samples. The method has the advantages that the operation is simple; the time is saved; the recovery rate is higher; the repeatability is better. The method recovery rate of 16 kinds of PAHs in the soil sample is 65.59 percent to 104.4 percent. The relative standard deviation is lower than 15.8 percent; the plant sample method recovery rate is 55.68 percent to 100.8 percent; the relative standard deviation is lower than 16.3 percent; the built analysis method can be used for the detection analysis of polluted soil and plant samples.
Description
Technical field
The invention belongs to analyze field tests, be specifically related to a kind of HPLC/ UV-fluorescence detector and connect for detecting soil
PAHs method in earth and plant.
Background technology
Polycyclic aromatic hydrocarbon (PAHs) is the class excessive risk organic pollution being widely present in environment, and existing known PAHs is up to
Hundreds of kind, wherein owing to there is significant teratogenesis, carcinogenic, mutagenic action in 16 kinds of PAHs, is classified as preferential control by U.S. Environmental Protection Agency (EPA)
Pollutant processed.Along with Chinese national economy high speed development and the enhancing of people's environmental consciousness, the relevant surrounding medium such as soil, plant
In 16 kinds of specific PAHs content, be distributed and the research originated become the focus in international environment field in recent decades it
One.
PAHs detection method is to study the important guarantee of environmental behaviour in its medium reliably.In high performance liquid chromatography
(HPLC) mensuration aspect, the single UV-detector (UV) of many employings or fluorescence detector (FLD), fluorescence detector has Gao Ling
Sensitivity, high-resolution, low detection limit and have the features such as high selection to Cucumber, be widely used in trace in sample in the last few years
The detection analysis of amount PAHs, its detection limit three orders of magnitude low than UV-detector.But, the sample that multiple PAHs is coexisted
Product, single detector suffers from the shadow that detection limit, the standard curve range of linearity, PAHs optical characteristics and concentration difference are big etc.
Ringing, a sample generally requires repeatedly sample introduction, even needs dilution process just can complete the detection of multiple PAHs in sample, operation
Loaded down with trivial details, time-consuming, cost is high.
Summary of the invention
The present invention be directed to the defect that prior art exists, use ultrasonic extraction method to extract in soil and plant sample
PAHs, utilizes HPLC/ UV-fluorescence series connection (UV-FLD) detection technique to analyze sample, it is intended to set up easy, practical, feasible
The PAHs of soil and plant sample analyzes method.For picking up from soil sample and the plant sample of contaminated area, extracted post analysis sample
During middle PAHs, with fluorescence detector for Main Analysis means, when fluoroscopic examination is inapplicable or adopts during PAHs excessive concentration in sample
Use UV-detector assistant analysis.
The purpose of the present invention can be achieved through the following technical solutions:
The series connection of a kind of HPLC/ UV-fluorescence detector is for detecting the PAHs method in soil and plant, and the method includes
Following steps:
1) extraction of sample and purification: sample uses ultrasonic extraction after pretreatment, uses chromatographic column to purify after extraction,
Component to be measured is obtained after purification；
2) component after step (1) being purified uses high performance liquid chromatography to detect component to be measured, high-efficient liquid phase color
Spectral condition is as follows:
Chromatographic column: Ф 4.6 × 250mm special reversed phase chromatographic column of Inertsil ODS-PPAHs；
Flowing phase composition: methanol-water；
Flow rate of mobile phase: 0.5～1.5ml/min；
Column compartment temperature: 35～45 DEG C；
Sample size: 15～25 μ l.
In technical solution of the present invention: use gradient elution and ultraviolet, the method separation detection 16 kinds of fluorescence detector series connection
PAHs, ultraviolet and fluorescence all use wavelength to switch, and detection program is as follows:
Detection program is as follows:
Table 2 HPLC/UV-FLD detection method program
In technical solution of the present invention: pedotheque is to pick up from top layer, nonirrigated farmland, cross 20 mesh sieves after soil sample is freeze-dried standby.
In technical solution of the present invention: after plant sample gathers, the root, stem and leaf of plant is separated and fully rinses with distilled water,
Dipping in dry surface moisture with filter paper, freeze-dried rear pulverizing is standby.
Beneficial effects of the present invention:
Extract with ultrasonic extraction, and combine HPLC/UV-FLD and divide the PAHs of analysis of variance soil and plant sample, have
Simple to operate, save time, the response rate is higher, repeated preferable advantage.In pedotheque, the method response rate of 16 kinds of PAHs is
65.59%～104.4%, relative standard deviation is respectively less than 15.8%, the plant sample method response rate be 55.68%～
100.8%, relative standard deviation is then less than 16.3%, and the analysis method set up can be used for the inspection of contaminated soil and plant sample
Cls analysis.
Accompanying drawing explanation
Fig. 1 is that UV detects PAHs liquid chromatogram.
Fig. 2 FLD detects PAHs liquid chromatogram
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described, but protection scope of the present invention is not limited to this:
Reagent and instrument:
Dichloromethane, normal hexane, anhydrous sodium sulfate, silica gel for chromatography (200-300 mesh) are analytical pure；Methanol is chromatograph
Alcohol.KQ-300DE medical digital controlled ultrasonic cleaner, RE-201D Rotary Evaporators, CHRIST freezer dryer, diameter 0.7cm
× 25cm chromatographic column.
Shimadzu high performance liquid chromatograph, is furnished with SPD-2A UV-detector, RF-10AXL fluorescence detector, CTO-20A post
Incubator, LC-20AT low pressure quaternary gradient pump, Ф 4.6 × 250mm Inertsil special reversed phase chromatographic column of ODS-P polycyclic aromatic hydrocarbon.
Sample collecting and pretreatment:
Soil is yellowish soil, picks up from top layer, nonirrigated farmland (0～20cm), crosses 20 mesh sieves standby after soil sample is freeze-dried.
After plant sample gathers, the root, stem and leaf of plant separated and fully rinses with distilled water, dipping in dry surface water with filter paper
Point, freeze-dried rear pulverizing is standby.Ready sample is all stored in the refrigerator of-20 DEG C.
The extraction of sample and purification:
Take the above-mentioned pedotheque prepared of 2g in 30mL glass centrifuge tube, add 30mL organic extractant (the two of 1:1
Chloromethanes and hexane solution) divide 3 times, each 10mL ultrasonic extraction 60min in ultrasonic water bath；Extract was collected layer
Analysis post (upper strata 2g anhydrous sodium sulfate, lower floor's 2g silica gel) purifies and with the dichloromethane of 11mL1:1 and hexane solution eluting；Wash
De-liquid is collected to rotary evaporation bottle, is concentrated to dryness under 40 DEG C of constant temperature, after methanol constant volume to 2mL, excessively 0.22 μm aperture filter membrane,
HPLC/UV-FLD analyzes.
Take a certain amount of above-mentioned plant sample prepared in 30mL glass centrifuge tube, with 30mL organic extractant (1:1's
Dichloromethane and hexane solution) divide 3 times, each 10mL ultrasonic extraction 30min in ultrasonic water bath；Extract was collected
Chromatographic column (upper strata 2g anhydrous sodium sulfate, lower floor's 2g silica gel) purifies and with the dichloromethane of 11mL1:1 and hexane solution eluting；
Eluent is collected to rotary evaporation bottle, is concentrated to dryness by extract under 40 DEG C of constant temperature, by methanol constant volume to 2mL, crosses 0.22 μm
After the filter membrane of aperture, HPLC/UV-FLD analyzes.
Mensuration program:
Flowing is methanol-water mutually, uses gradient elution and ultraviolet, the method separation detection 16 kinds of fluorescence detector series connection
PAHs, ultraviolet and fluorescence all use wavelength to switch, and flow velocity is 1.0mL/min, column temperature 40 DEG C, and sample size is 20 μ L.In this condition
It is complete that lower 16 kinds of PAHs go out peak in 40min.High performance liquid chromatograph detection program is as follows:
Table 3 HPLC/UV-FLD detection method program
Table 4 UV measures PAHs standard curve
Table 5 FLD measures PAHs standard curve
The mensuration of pedotheque
According to pre-treating method and the chromatographiccondition of aforementioned pedotheque, the PAHs of analysis margin comparison pedotheque
Background concentration.It addition, weigh above-mentioned pedotheque 2g, the PAHs hybrid standard liquid of addition methanol dilution, it is placed in dark place,
After methanol volatilizees, analyze P in soil AHs content by preceding method, and calculate the P in soil AHs method response rate.
The recovery of standard addition of PAHs in table 6 yellowish soil sample
Plant sample
Using the pre-treating method of afore-mentioned plants sample and above-mentioned analysis condition, the PAHs background analyzing plant sample is (empty
White comparison) take above-mentioned sample simultaneously, it is separately added into the PAHs hybrid standard liquid of methanol dilution；Dark place stands, and treats that methanol volatilizees
After, test the PAHs method response rate, the results are shown in Table.
The recovery of standard addition of PAHs in table 7 Chinese cabbage leaf sample
The recovery of standard addition of PAHs in table 8 Chinese cabbage stem sample
The recovery of standard addition of PAHs in table 9 Rice Leaf sample
The recovery of standard addition of PAHs in table 10 rice stem sample
The recovery of standard addition of PAHs in table 11 rice root sample
The recovery of standard addition of PAHs in table 12 rice husk sample
The recovery of standard addition of PAHs in table 13 Rice Samples
Extract with ultrasonic extraction, and combine HPLC/UV-FLD and divide the PAHs of analysis of variance soil and plant sample, have
Simple to operate, save time, the response rate is higher, repeated preferable advantage.In pedotheque, the method response rate of 16 kinds of PAHs is
65.59%～104.4%, relative standard deviation is respectively less than 15.8%, the plant sample method response rate be 55.68%～
100.8%, relative standard deviation is then less than 16.3%, and the analysis method set up can be used for the inspection of contaminated soil and plant sample
Cls analysis.
Claims (4)
1. a HPLC/ UV-fluorescence detector series connection is for detecting the PAHs method in soil and plant, it is characterised in that:
The method comprises the following steps:
1) extraction of sample and purification: sample uses ultrasonic extraction after pretreatment, uses chromatographic column to purify, purifies after extraction
After obtain component to be measured；
2) component after step (1) being purified uses high performance liquid chromatography to detect component to be measured, high performance liquid chromatography bar
Part is as follows:
Chromatographic column: Ф 4.6 × 250mm special reversed phase chromatographic column of Inertsil ODS-PPAHs；
Flowing phase composition: methanol-water；
Flow rate of mobile phase: 0.5～1.5ml/min；
Column compartment temperature: 35～45 DEG C；
Sample size: 15～25 μ l.
HPLC/ UV-fluorescence detector the most according to claim 1 series connection is for detecting the PAHs side in soil and plant
Method, it is characterised in that: use gradient elution and ultraviolet, 16 kinds of PAHs of method separation detection of fluorescence detector series connection, ultraviolet and
Fluorescence all uses wavelength to switch, and detection program is as follows:
Table 1 HPLC/UV-FLD detection method program
HPLC/ UV-fluorescence detector the most according to claim 1 series connection is for detecting the PAHs side in soil and plant
Method, it is characterised in that: pedotheque is to pick up from top layer, nonirrigated farmland, crosses 20 mesh sieves standby after soil sample is freeze-dried.
HPLC/ UV-fluorescence detector the most according to claim 1 series connection is for detecting the PAHs side in soil and plant
Method, it is characterised in that: after plant sample gathers, the root, stem and leaf of plant separated and fully rinses with distilled water, dipping in filter paper dry
Surface moisture, freeze-dried rear pulverizing is standby.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610305140.9A CN105784910A (en) | 2016-05-10 | 2016-05-10 | Method for detecting PAHs (polycyclic aromatic hydrocarbons) in soil and plants through connecting HPLC (high performance liquid chromatography)/ultraviolet-fluorescence detectors in series |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610305140.9A CN105784910A (en) | 2016-05-10 | 2016-05-10 | Method for detecting PAHs (polycyclic aromatic hydrocarbons) in soil and plants through connecting HPLC (high performance liquid chromatography)/ultraviolet-fluorescence detectors in series |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105784910A true CN105784910A (en) | 2016-07-20 |
Family
ID=56401187
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610305140.9A Pending CN105784910A (en) | 2016-05-10 | 2016-05-10 | Method for detecting PAHs (polycyclic aromatic hydrocarbons) in soil and plants through connecting HPLC (high performance liquid chromatography)/ultraviolet-fluorescence detectors in series |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105784910A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108535496A (en) * | 2018-06-14 | 2018-09-14 | 广东腾湃医疗股份有限公司 | A kind of novel purification lead chelating type immune complex method |
| CN115932109A (en) * | 2022-12-29 | 2023-04-07 | 南京农业大学 | High performance liquid chromatography detection method for measuring phthalic acid ester in soil |
-
2016
- 2016-05-10 CN CN201610305140.9A patent/CN105784910A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108535496A (en) * | 2018-06-14 | 2018-09-14 | 广东腾湃医疗股份有限公司 | A kind of novel purification lead chelating type immune complex method |
| CN115932109A (en) * | 2022-12-29 | 2023-04-07 | 南京农业大学 | High performance liquid chromatography detection method for measuring phthalic acid ester in soil |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Iinuma et al. | A highly resolved anion-exchange chromatographic method for determination of saccharidic tracers for biomass combustion and primary bio-particles in atmospheric aerosol | |
| CN101706480B (en) | Method for analyzing polycyclic aromatic hydrocarbon content of soil | |
| CN101881758A (en) | Method for measuring phthalic ester in atmospheric particulates | |
| CN101787057B (en) | Method for separating and purifying rhamnolipid | |
| CN102288720A (en) | Method for detecting benzo(a)pyrene of oiltea camellia seed oil | |
| CN109884207A (en) | A method of quick and precisely analyzing polyphenol content in rapeseed oil | |
| CN101865898B (en) | Method for determining phthalate ester in soil | |
| CN101706484B (en) | Method for synchronously purifying and separating organic extract of environmental medium step by step | |
| CN108693262B (en) | Method for determining various preservatives in cosmetics | |
| CN105784881A (en) | Determination method of perfluorinated compound isomer in soil and/or plants | |
| CN107192596A (en) | Method for preparing purified for the THC standard substance of forensic science illicit drugs inspection | |
| CN108802255A (en) | The method for measuring ganoderic acid A and Ganoderma lucidum triterpenes components content in compound preparation | |
| CN105445407B (en) | Detection method for fatty acid and vitamin E in idesia | |
| CN104807688B (en) | A kind of method of micro polycyclic aromatic hydrocarbon in extracting and enriching large volume environmental water sample | |
| CN105784910A (en) | Method for detecting PAHs (polycyclic aromatic hydrocarbons) in soil and plants through connecting HPLC (high performance liquid chromatography)/ultraviolet-fluorescence detectors in series | |
| CN107607648A (en) | The solid phase extraction GC MS detection method of phthalate compound in a kind of deposit | |
| Wu et al. | A novel selective accelerated solvent extraction for effective separation and rapid simultaneous determination of six anthraquinones in tartary buckwheat and its products by UPLC–DAD | |
| CN102507794A (en) | Method for rapidly detecting poisoned substances by adopting urine | |
| CN102507793A (en) | Method for detecting poison quickly by using blood | |
| CN103163271A (en) | Measuring method for residual amount of cnidium lactone in tobacco leaves | |
| CN102590372A (en) | Method for detecting types and contents of phenolic acid in flue-cured tobacco root system secretion | |
| CN101972292B (en) | Method for measuring flavone glycoside compounds in herba epimedii | |
| CN104215614B (en) | A kind of high performance liquid chromatography-diode array/fluorescence detector Series detectors barbaloin A, B and the method for aloe-emodin | |
| CN102520107A (en) | Method for measuring matrine pesticide residual quantity in tobacco | |
| CN106932518B (en) | The detection method of incretion interferent in a kind of complex biological matrix |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160720 |