CN105628843A - Solid-phase membrane extraction-gas chromatography electron capture detection method for eight pyrethroid pesticides in water body - Google Patents
Solid-phase membrane extraction-gas chromatography electron capture detection method for eight pyrethroid pesticides in water body Download PDFInfo
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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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/12—Preparation by evaporation
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/12—Preparation by evaporation
- G01N2030/126—Preparation by evaporation evaporating sample
Abstract
The invention belongs to the technical field of the safety detection of water quality, and particularly relates to a solid-phase membrane extraction-gas chromatography electron capture detection method for eight pyrethroid pesticides in water body. The method comprises the following steps: the cleaning and activation of a C18 solid-phase extraction membrane, the extraction of a water sample, the elution of pyrethroidcompounds, the condensation of eluent and the detection of a gas chromatography-electron capture detector. Specifically, the C18 solid-phase extraction membrane is firstly immersed in an ethyl acetate/cyclohexane mixture at the volume ratio of 1:1 for 3 minutes in advance, and is then activated by methanol and water in turn; the water sample to be detected is eluted by ethyl acetate and cyclohexane after being extracted by the C18 solid-phase extraction membrane; the eluent is evaporated to dry in a water bath with the temperature of 40-45 degrees centigrade in a rotating manner after being dehydrated by an anhydrous sodium sulfate passing column, and is diluted by n-hexane to constant volume of 1.0mL for gas chromatography-electron capture detection and analysis as well as quantification based on an external standard method.
Description
Technical field
The invention belongs to Water quality safety detection technology field, in particular to the immobilon-p extraction-gas-chromatography electron capture detection method of 8 kinds of pyrethroid pesticides in a kind of water body.
Background technology
Pyrethroid pesticide is the novel pesticide of a kind of cyclopropanates containing phenoxy group, has the features such as wide spectrum, poison efficient, low and low residue. being widely used in farmland fruit vegetables in recent years kills in worm and fishery cultivating, it is by farmland drainage, rainfall drip washing enters water body, also can (be mainly used in cleaning up the pond because of a large amount of uses in fishery cultivating, poisoning trash fish and harmful organism etc.) and remain in water body, enter the pyrethrin in water body (PYRs) not only can be polluted by surface water, also can enrichment in hydrobiont body, enter in fish and human body eventually through food chain, and cause potential hazard, research shows, Mammals is had nerve by PYRs, immunity system, the toxic action such as cardiovascular and hereditary, and be 1000 times of Mammals and birds to the toxicity of fish. at present, the residual problem of PYRs in fishery products causes the attention of a lot of country. in European Union's regulation fishery products, the most high residue amount of Cypermethrin is 50 �� g/kg, and Deltamethrin is 10 �� g/kg, Japan's " Positive List System " defines Cypermethrin in shape order (Oncorhynchi, rainbow trout etc.), the most high residue amount of Deltamethrin be 30 �� g/kg, other fishes and hydrocoles are 10 �� g/kg. the Ministry of Agriculture of China announces the most high residue amount 30 �� g/kg of Deltamethrin in No. 235 regulation fish tissue. in recent years, many scholars have carried out the investigation to pyrethrin pesticide pollution situation in natural water, it has been found that all have the pollution of the horizontal above-mentioned substance of ng/L in water body such as most river and lakes etc. in the investigation result display network of waterways, the Pearl River Delta surface water of researchist, pyrethrin massfraction is between 0.01-0.73 �� g/kg.
Owing in environmental water sample, pyrethrin concentration is extremely low, it usually needs could measure through enrichment. In traditional enrichment water, the method for pyrethrin is liquid-liquid extraction method, operate loaded down with trivial details time-consuming, need to consume a large amount of organic solvent, and solid phase extraction because of have simple to operate, consumption solvent is few and enrichment times height is widely used in the analysis of agricultural chemicals. Finding one simpler, in the water body of environmental protection, the pre-treating process of chlorobenzene compound becomes research focus. Immobilon-p extracts the one as Solid-Phase Extraction, the solid-phase extraction membrane that it uses, it is possible to process the water sample of comparatively large vol faster, and enrichment times height. In addition, immobilon-p extraction can directly process water sample at scene, convenient and swift stable. The instrument detection technique of pyrethrin has gas-chromatography, gas chromatography-mass spectrography, liquid chromatograph mass spectrography etc. Pyrethrin detection, as the detecting instrument of selectively highly sensitive, is had higher sensitivity and accuracy by gas-chromatography-electron capture detection. In the last few years, researchist is had to carry out the research to area, some river mouths pyrethrin residual and distribution, but research about water body kind pyrethrin residual is few.
Summary of the invention
The object of the present invention is exactly the deficiency overcoming existing analytical procedure, there is provided the immobilon-p extraction-gas-chromatography electron capture detection method of 8 kinds of pyrethroid pesticides in a kind of water body fast and accurately, to realize the quantitative and qualitative test of pyrethrin in water body.
The technical solution adopted for the present invention to solve the technical problems is:
An immobilon-p extraction-gas-chromatography electron capture detection method for 8 kinds of pyrethroid pesticides in water body, the method comprises C18Concentrated and the gas chromatography-electron capture detector of the extraction of the cleaning of solid-phase extraction membrane and activation, water sample, the wash-out of pyrethroid coumpound, elutriant detects several steps, is specially: C18Solid-phase extraction membrane is in advance with the ethyl acetate of 1:1 volume ratio/hexanaphthene mixed liquid dipping 3min, then activates C with methyl alcohol, water respectively18Solid-phase extraction membrane, water sample to be measured is through C18After Solid-Phase Extraction membrane extraction, successively with ethyl acetate and hexanaphthene wash-out, elutriant through anhydrous sodium sulphate cross post except after water in 40-45 DEG C of water-bath rotary evaporated to dryness, be settled to 1.0mL with normal hexane, carry out gas-chromatography electron capture detection analysis, quantified by external standard method. Bifenthrin in water body, Fenvalerate, cyhalothrin, Cypermethrin, permethrin, taufluvalinate, fenvalerate and Deltamethrin 8 kinds of chrysanthemum ester compounds are specifically carried out gas-chromatography electron capture detection by the present invention. The method adopts immobilon-p to extract pre-treatment and the enrichment of water sample, and vapor-phase chromatography completes Component seperation and detection in conjunction with electron capture detector. The method is simple, quick, highly sensitive, favorable reproducibility, the assay that can be used for chlorobenzene compound in water body.
As preferably, 8 kinds of described pyrethroid pesticides refer to that main component is the agricultural chemicals of one or more in bifenthrin, Fenvalerate, cyhalothrin, Cypermethrin, permethrin, taufluvalinate, fenvalerate and Deltamethrin.
As preferably, the method concrete steps are as follows:
a.C18The cleaning of solid-phase extraction membrane and activation: C18Solid-phase extraction membrane, in advance with the mixed liquid dipping 3min of 5mL ethyl acetate/hexanaphthene 1:1 volume ratio, activates C with 10mL methyl alcohol, 10mL water successively18Solid-phase extraction membrane, allows solvent all flow through solid-phase extraction membrane, in the process, can not make solid-phase extraction membrane contact air;
B. the extraction of water sample: in advance with 0.45 ��m of filtering with microporous membrane water sample, pretreated 500mL water sample is added to and C is housed18In the polytetrafluoroethylene filter of solid-phase extraction membrane, drive vacuum pump, after water sample passes through with the flow velocity of 10mL/min, continue the residual moisture vacuumizing to remove in solid-phase extraction membrane;
C. the wash-out of pyrethroid coumpound and concentrated: successively with 10mL ethyl acetate and 10mL hexanaphthene wash-out C18Solid-phase extraction membrane, elutriant through anhydrous sodium sulphate cross post except after water in 40 DEG C of water-bath rotary evaporated to dryness, be settled to 1.0mL with normal hexane, to be analyzed;
D. gas chromatography-electron capture detector detection: gas chromatography-electron capture detector detects: adopt gas chromatograph, configuration electron capture detector detection, use DB-35, the capillary gas chromatographic column of 30m �� 0.25mm �� 0.25 ��m realizes Component seperation, setting gas-chromatography heating schedule detects, qualitative with retention time, quantified by external standard method carries out separation and the detection of 8 kinds of chrysanthemum ester compounds.
As preferably, gas-chromatography heating schedule is: 120 DEG C keep 1min, and 15 DEG C/min is warming up to 260 DEG C, and 5 DEG C/min is warming up to 320 DEG C, keep 8min.
The present invention is with C18Solid-phase extraction membrane realizes the enrichment of pyrethrin in water body, adopts gas-chromatography-electron capture detection method detection. 8 kinds of pyrethroid pesticide detections are limited to 0.001��0.01 �� g/L, and the rate of recovery is 86��114%. The method is simple to operate, it may also be useful to organic solvent amount is few, favorable reproducibility, linearity range width, favorable reproducibility, rate of recovery height, can measure pyrethroid pesticide concentration in water body fast.
Accompanying drawing explanation
Fig. 1 is the gas chromatogram of 100 �� g/mL8 kind chrysanthemum ester compound standardized solution; 1. bifenthrin, 2. Fenvalerate, 3. cyhalothrin, 4. Cypermethrin, 5. permethrin, 6. taufluvalinate, 7. fenvalerate, 8. Deltamethrin.
Fig. 2 is the gas chromatogram adding chrysanthemum ester compound in mark seawater; 1. bifenthrin, 2. Fenvalerate, 3. cyhalothrin, 4. Cypermethrin, 5. permethrin, 6. taufluvalinate, 7. fenvalerate, 8. Deltamethrin.
Embodiment
Below by specific embodiment, the technical scheme of the present invention is described in further detail. It is to be understood that the enforcement of the present invention is not limited to the following examples, any formal accommodation that the present invention is made and/or change and all will fall into protection domain of the present invention.
In the present invention, if not refering in particular to, all part, per-cent are weight unit, and the equipment adopted and raw material etc. all can be buied from market or this area is conventional. Method in following embodiment, if no special instructions, is the ordinary method of this area.
The mensuration of 8 kinds of polyester compounds in the tap water of embodiment 1 laboratory
(1)C18The cleaning of solid-phase extraction membrane and activation: C18Solid-phase extraction membrane soaks 3min with 5mL ethyl acetate/hexanaphthene (volume ratio 1:1) in advance, successively with 10mL methyl alcohol, 10mL water activation C18Solid-phase extraction membrane, allows solvent all flow through solid-phase extraction membrane, in the process, can not make solid-phase extraction membrane contact air;
(2) extraction of water sample: in advance with 0.45 ��m of filtering with microporous membrane laboratory water sample from the beginning, pretreated 500mL laboratory from the beginning water sample be added to C be housed18In the polytetrafluoroethylene filter of solid-phase extraction membrane, drive vacuum pump, after water sample passes through with the flow velocity of 10mL/min, continue the residual moisture vacuumizing to remove in solid-phase extraction membrane;
(3) wash-out of pyrethroid coumpound and concentrated: successively with 10mL ethyl acetate and 10mL hexanaphthene wash-out C18Solid-phase extraction membrane, elutriant through anhydrous sodium sulphate cross post except after water in 40 DEG C of water-bath rotary evaporated to dryness, be settled to 1.0mL with normal hexane, to be analyzed;
(4) gas chromatography-electron capture detector detection: adopt VARIAN Oncology Systems's CP3380 gas chromatograph, configuration electron capture detector detection, it may also be useful to DB-35 capillary gas chromatographic column (30m �� 0.25mm �� 0.25 ��m) realizes Component seperation. Injector temperature: 260 DEG C; Electron capture actuator temperature: 300 DEG C; Sample size 1.0mL, Splitless injecting samples, flow velocity is 2mL/min; Gas-chromatography heating schedule is: 120 DEG C keep 1min, and 15 DEG C/min is warming up to 260 DEG C, and 5 DEG C/min is warming up to 320 DEG C, keep 8min. Detecting according to the gas chromatography-electron capture detector condition set, qualitative with retention time, quantified by external standard method, can realize effective separation of 8 kinds of chrysanthemum ester compounds, as shown in Figure 1.
(5) typical curve draws (external standard method): gets appropriate chrysanthemum ester compound standard reserving solution respectively, is the chrysanthemum ester compound mixed standard solution of 0.5 �� g/L, 1.0 �� g/L, 5.0 �� g/L, 10 �� g/L, 20 �� g/L, 50 �� g/L with normal hexane configuration concentration. Operate according to the requirement of above-mentioned (1), (2), (3), (4) step, according to the corresponding relation Criterion curve of the chrysanthemum ester compound concentration added and peak area. The gas chromatogram of 8 kinds of chrysanthemum ester compound standardized solution is shown in Fig. 1. The linearity range of the inventive method and detection limit are in table 1, the recovery testu that difference adds scalar in different water body (laboratory tap water and marine site, Zhoushan seawater) the results are shown in Table 2, and the gas chromatogram wherein adding chrysanthemum ester compound in mark seawater is shown in Fig. 2.
The linearity range of table 1 the inventive method and detection limit
The rate of recovery of table 2 different substrates water body and precision experimental result.
According to result it will be seen that adopt this external standard method, recording 8 kinds of pyrethrin content in the tap water of laboratory and be non-detection, the rate of recovery adding the mark laboratory each chrysanthemum ester compound of tap water is 86%-112%, meets analytical procedure to the requirement of the rate of recovery.
The mensuration of 8 kinds of polyester compounds in the seawater of marine site, embodiment 2 Zhoushan
(1)C18The cleaning of solid-phase extraction membrane and activation: C18Solid-phase extraction membrane soaks 3min with 5mL ethyl acetate/hexanaphthene (volume ratio 1:1) in advance, successively with 10mL methyl alcohol, 10mL water activation C18Solid-phase extraction membrane, allows solvent all flow through solid-phase extraction membrane, in the process, can not make solid-phase extraction membrane contact air;
(2) extraction of water sample: in advance with marine site, 0.45 ��m of filtering with microporous membrane Zhoushan water sample, marine site, pretreated 500mL Zhoushan water sample is added to and C is housed18In the polytetrafluoroethylene filter of solid-phase extraction membrane, drive vacuum pump, after water sample passes through with the flow velocity of 10mL/min, continue the residual moisture vacuumizing to remove in solid-phase extraction membrane;
(3) wash-out of pyrethroid coumpound and concentrated: successively with 10mL ethyl acetate and 10mL hexanaphthene wash-out C18Solid-phase extraction membrane, elutriant through anhydrous sodium sulphate cross post except after water in 40 DEG C of water-bath rotary evaporated to dryness, be settled to 1.0mL with normal hexane, to be analyzed;
(4) gas chromatography-electron capture detector detection: adopt VARIAN Oncology Systems's CP3380 gas chromatograph, configuration electron capture detector detection, it may also be useful to DB-35 capillary gas chromatographic column (30m �� 0.25mm �� 0.25 ��m) realizes Component seperation. Injector temperature: 260 DEG C; Electron capture actuator temperature: 300 DEG C; Sample size 1.0mL, Splitless injecting samples, flow velocity is 2mL/min; Gas-chromatography heating schedule is: 120 DEG C keep 1min, and 15 DEG C/min is warming up to 260 DEG C, and 5 DEG C/min is warming up to 320 DEG C, keep 8min.
(5) typical curve draws (external standard method): gets appropriate chrysanthemum ester compound standard reserving solution respectively, is the chrysanthemum ester compound mixed standard solution of 0.5 �� g/L, 1.0 �� g/L, 5.0 �� g/L, 10 �� g/L, 20 �� g/L, 50 �� g/L, 100 �� g/L with normal hexane configuration concentration. Operate according to the requirement of above-mentioned (1), (2), (3), (4) step, according to the corresponding relation Criterion curve of the chrysanthemum ester compound concentration added and peak area.
In table 2, adopting this external standard method, record 8 kinds of pyrethrin content in the seawater of marine site, Zhoushan and be non-detection, the rate of recovery adding mark marine site, the Zhoushan each chrysanthemum ester compound of seawater is 91%-114%, meets analytical procedure to the requirement of the rate of recovery.
Above-described embodiment is the explanation to the present invention, is not limitation of the invention, any scheme after simple transformation of the present invention is all belonged to protection scope of the present invention.
Claims (4)
1. the immobilon-p extraction-gas-chromatography electron capture detection method of 8 kinds of pyrethroid pesticides in a water body, it is characterised in that: the method comprises C18Concentrated and the gas chromatography-electron capture detector of the extraction of the cleaning of solid-phase extraction membrane and activation, water sample, the wash-out of pyrethroid coumpound, elutriant detects several steps, is specially: C18Solid-phase extraction membrane is in advance with the ethyl acetate of 1:1 volume ratio/hexanaphthene mixed liquid dipping 3min, then activates C with methyl alcohol, water respectively18Solid-phase extraction membrane, water sample to be measured is through C18After Solid-Phase Extraction membrane extraction, successively with ethyl acetate and hexanaphthene wash-out, elutriant through anhydrous sodium sulphate cross post except after water in 40-45 DEG C of water-bath rotary evaporated to dryness, be settled to 1.0mL with normal hexane, carry out gas-chromatography electron capture detection analysis, quantified by external standard method.
2. detection method according to claim 1, it is characterised in that: 8 kinds of described pyrethroid pesticides refer to that main component is the agricultural chemicals of one or more in bifenthrin, Fenvalerate, cyhalothrin, Cypermethrin, permethrin, taufluvalinate, fenvalerate and Deltamethrin.
3. detection method according to claim 1, it is characterised in that the method concrete steps are as follows:
a.C18The cleaning of solid-phase extraction membrane and activation: C18Solid-phase extraction membrane, in advance with the mixed liquid dipping 3min of 5mL ethyl acetate/hexanaphthene 1:1 volume ratio, activates C with 10mL methyl alcohol, 10mL water successively18Solid-phase extraction membrane, allows solvent all flow through solid-phase extraction membrane, in the process, can not make solid-phase extraction membrane contact air;
B. the extraction of water sample: in advance with 0.45 ��m of filtering with microporous membrane water sample, pretreated 500mL water sample is added to and C is housed18In the polytetrafluoroethylene filter of solid-phase extraction membrane, drive vacuum pump, after water sample passes through with the flow velocity of 10mL/min, continue the residual moisture vacuumizing to remove in solid-phase extraction membrane;
C. the wash-out of pyrethroid coumpound and concentrated: successively with 10mL ethyl acetate and 10mL hexanaphthene wash-out C18Solid-phase extraction membrane, elutriant through anhydrous sodium sulphate cross post except after water in 40 DEG C of water-bath rotary evaporated to dryness, be settled to 1.0mL with normal hexane, to be analyzed;
D. gas chromatography-electron capture detector detection: adopt gas chromatograph, configuration electron capture detector detection, use DB-35, the capillary gas chromatographic column of 30m �� 0.25mm �� 0.25 ��m realizes Component seperation, setting gas-chromatography heating schedule detects, qualitative with retention time, quantified by external standard method carries out separation and the detection of 8 kinds of chrysanthemum ester compounds.
4. detection method according to claim 3, it is characterised in that: gas-chromatography heating schedule is: 120 DEG C keep 1min, and 15 DEG C/min is warming up to 260 DEG C, and 5 DEG C/min is warming up to 320 DEG C, keep 8min.
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