CN108614040A - It is a kind of quickly to measure the remaining method of pesticide in cereal - Google Patents
It is a kind of quickly to measure the remaining method of pesticide in cereal Download PDFInfo
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- CN108614040A CN108614040A CN201711498836.9A CN201711498836A CN108614040A CN 108614040 A CN108614040 A CN 108614040A CN 201711498836 A CN201711498836 A CN 201711498836A CN 108614040 A CN108614040 A CN 108614040A
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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
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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
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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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Abstract
The remaining method of pesticide in cereal is quickly measured this application discloses a kind of, is included the following steps：(1) preparation；(2) sample extraction；(3) quantitative determination of pesticide residue concentration.Step (1) preparation, further comprises：1. opening refrigerator and thermostatted water oil groove in advance.2. cereal to be measured is contained in extraction kettle material barrel, the air being passed through after sealing cover in R134a dischargers is covered.The present invention quickly measures the high performance liquid chromatography pre-treating method of cereals Residual Pesticides in Farm Produce, simplifies operational sequence, and simple in structure, operability is strong, facilitates processing, can METHOD FOR CONTINUOUS DETERMINATION；Wide range of measurement, safety coefficient are high.
Description
Technical field
The present invention relates to chromatography detection technique fields, more particularly to a kind of quickly to measure cereals Residual Pesticides in Farm Produce
High performance liquid chromatography pre-treating method.
Background technology
In recent years, pesticide remains exceeded event in agricultural product and food and happens occasionally, the serious shadow of excessive pesticide residues
The health of people is rung, the health and safety problem of diet also becomes the most important focus of consumer.Rice (Oryza
Sativa L.) it is one of three big staple food grain of China, the Pesticide Residue of rice also becomes focus of people's attention and research is reversed
One of.
Pesticide refers to harming the crops and the pest and disease damage of agricultural and sideline product, weeds and other harmful organisms for preventing
Drug general name.Its to promoting agricultural volume increase to have extremely important effect, be in current agricultural production for it is anti-cure the disease, worm,
The weeds substance indispensable to murrain.However, being continuously increased in pesticide species and quantity, scientifical use pesticide
In the case that educational propaganda dynamics is relatively low, some low toxicity and low residue indiscriminates use of pesticide and pesticide caused by not scientifical use are dirty
Dye problem will be also difficult to avoid that.
Pesticide residue refers to not being decomposed in Pesticide use the latter period and remaining on organism, agricultural and sideline product and soil
The general name of trace pesticide substance, toxic metabolite, degradation product and impurity in the ecological environments such as earth, water body, air.
For analyzing work, sample pre-treatments include mainly：Sample decomposes, sample purification and sample concentration these three
Primary sample is processed into the state that can carry out Instrumental Analysis by link.Traditional Sample Pretreatment Technique is time-consuming and laborious, behaviour
Make complicated and be readily incorporated error, extraction is relatively low with purification efficiency, is consumed while impact analysis result a large amount of toxic
Organic solvent.
Under the greatly developing of the technologies such as substance separation, computer, machine-building and automation, Sample Pretreatment Technique
Tend to easy, quick, low solvent consumption, low stain, micromation and automation development trend.R134a under undercritical conditions
Due to its unique physicochemical property, it is widely used in the numerous areas such as extraction and separation, enzymatic reaction system, there is very big application
Foreground.R134a is gas under normality, and after pressure is raised to its critical pressure (4.07MPa), the organic matter of some low poles shows
Go out higher solubility.This characteristic is applied to the pre-treatment of Residual Pesticides in Farm Produce will substantially reduce pre-treatment required time
And greatly reduce the usage amount of organic solvent.
Invention content
Technical problem to be solved by the present invention lies in provide a kind of quickly measurement cereals Residual Pesticides in Farm Produce
High performance liquid chromatography pre-treating method and its device.Apparatus of the present invention simplify operational sequence, simple in structure, operability
By force, facilitate processing, it can METHOD FOR CONTINUOUS DETERMINATION；Wide range of measurement, safety coefficient are high.
In order to solve the above technical problems, the present invention provides a kind of remaining methods of pesticide in quickly measurement cereal, including
Following steps：
(1) preparation；
(2) sample extraction；
(3) quantitative determination of pesticide residue concentration.
Step (1) preparation, further comprises：1. opening refrigerator and thermostatted water oil groove in advance.
Step (1) preparation, further comprises：2. cereal to be measured is contained in extraction kettle material barrel, cover close
The air being passed through after capping in R134a dischargers.
Step (1) preparation, further comprises：3. opening plunger pump, preset pressure is boosted to, verifying attachment
Air-tightness closes reset valve after being verified, and collecting duct is inserted into collector.
Step (2) sample extraction, further comprises：1. weighing cereal to be measured in extraction kettle material barrel, and will be molten
Agent dries up under a nitrogen atmosphere, then changes extraction kettle sealing cover after material barrel is put into extraction kettle.
Step (2) sample extraction, further comprises：2. closing reset valve, plunger pump is opened, it again will be in material barrel
Air drain, R134a fluids are supplemented into extraction kettle by surge tank, until extraction system pressure reach preset pressure value after
Close pump, static extracting 2h.
Step (2) sample extraction, further comprises：3. opening reset valve, fluid in extraction kettle is made to pass through collector
Internal solvent is inhaled, and is then exhausted from after solvent absorption, and flow velocity is small as possible complete to ensure to absorb, and opens simultaneously plunger pump, passes through
Adjusting flow control valve makes the amount of supplement R134a in extraction kettle be equal to reset valve discharge rate, maintains extraction kettle pressure relatively steady
Dynamic extraction 40min under fixed condition.
Step (2) sample extraction, further comprises：4. after dynamic extraction, before closing plunger pump and extraction kettle
Valve, fluid rinses reset valve and follow-up all after solvent absorption using same solvent in collector in kettle to be extracted
Gas-guide tube 3 times, and flushing liquor is collected into collector.
Step (2) sample extraction, further comprises：5. by solution constant volume in collector, 2ml solution is drawn after constant volume
After filtering with microporous membrane, be placed in brown vial refrigerate it is to be checked.
The quantitative determination of step (3) the pesticide residue concentration, further comprises：
1. being detected to sample with high performance liquid chromatography, the standard curve of pesticide concentration is established using external standard method；
2. by the response of each pesticide under liquid chromatogram difference retention time, combined standard curve calculates addition recycling
Rate.
Advantageous effect of the present invention includes：
(1) device of the present invention keeps operational sequence simple compared with traditional extraction device, has operability strong, side
Just process, can METHOD FOR CONTINUOUS DETERMINATION the advantages of；
(2) equipment safety coefficient is high, and extraction kettle and pipeline selection are stainless steel, and the danger such as explosion will not occur, will not
Experimenter is damaged；
(3) this described assay method can survey the pesticide residue situation of various cereal agricultural product, extraction experiments condition adjustable,
Substantially increase the efficiency and the rate of recovery of extraction.
Description of the drawings
Fig. 1 is that the overall structure of measurement cereals Residual Pesticides in Farm Produce pretreating device described in the embodiment of the present invention is shown
It is intended to.Wherein：1 fluid reservoir, 2 refrigeration coils, 3 plunger pumps, 4 surge tanks, 5 thermostatted water oil grooves, 6 extraction kettles, 7 reset valves, 8 receive
Storage.
Fig. 2 is one testing result figure of HPLC chromatogram analysis method described in the embodiment of the present invention；
Fig. 3 is two testing result figure of HPLC chromatogram analysis method described in the embodiment of the present invention.
Specific implementation mode
The present invention is described in detail with reference to embodiment.To keep the objectives, technical solutions, and advantages of the present invention clearer, bright
Really, developing simultaneously referring to the drawings, the present invention is described in more detail for embodiment, but the invention is not limited in these embodiments.
The present invention quickly measures the high performance liquid chromatography pretreating device of cereals Residual Pesticides in Farm Produce, is somebody's turn to do with utilizing
Device measures the remaining method of pesticide in brown rice under the conditions of subcritical R134a (HFA 134a).
Technical scheme of the present invention is illustrated below.
A kind of device, including R134a storage tanks, refrigeration coil, plunger pump, surge tank, thermostatted water oil groove, extraction kettle, fine tuning
Valve, collector and highly effective liquid phase chromatographic device.
Further, the splicing sequence of device is R134a storage tanks, refrigeration coil, plunger pump, surge tank, thermostatted water oil groove, extraction
It takes kettle, reset valve, reset valve, collector and connects highly effective liquid phase chromatographic device offline.
Further, the surge tank, extraction kettle are by water oil loop temperature-control in chuck；Reset valve and pipeline are logical
It crosses to be immersed in water oil groove and realizes temperature control.
In order to solve the above technical problems, the present invention provides a kind of remaining methods of pesticide in quickly measurement cereal, including
Following steps：
(1) preparation；
(2) sample extraction；
(3) quantitative determination of pesticide residue concentration.
Step (1) preparation, further comprises：1. opening refrigerator and thermostatted water oil groove in advance.
Step (1) preparation, further comprises：2. cereal to be measured is contained in extraction kettle material barrel, cover close
The air being passed through after capping in R134a dischargers.
Step (1) preparation, further comprises：3. opening plunger pump, preset pressure is boosted to, verifying attachment
Air-tightness closes reset valve after being verified, and collecting duct is inserted into collector.
Step (2) sample extraction, further comprises：1. weighing cereal to be measured in extraction kettle material barrel, and will be molten
Agent dries up under a nitrogen atmosphere, then changes extraction kettle sealing cover after material barrel is put into extraction kettle.
Step (2) sample extraction, further comprises：2. closing reset valve, plunger pump is opened, it again will be in material barrel
Air drain, R134a fluids are supplemented into extraction kettle by surge tank, until extraction system pressure reach preset pressure value after
Close pump, static extracting 2h.
Step (2) sample extraction, further comprises：3. opening reset valve, fluid in extraction kettle is made to pass through collector
Internal solvent is inhaled, and is then exhausted from after solvent absorption, and flow velocity is small as possible complete to ensure to absorb, and opens simultaneously plunger pump, passes through
Adjusting flow control valve makes the amount of supplement R134a in extraction kettle be equal to reset valve discharge rate, maintains extraction kettle pressure relatively steady
Dynamic extraction 40min under fixed condition.
Step (2) sample extraction, further comprises：4. after dynamic extraction, before closing plunger pump and extraction kettle
Valve, fluid rinses reset valve and follow-up all after solvent absorption using same solvent in collector in kettle to be extracted
Gas-guide tube 3 times, and flushing liquor is collected into collector.
Step (2) sample extraction, further comprises：5. by solution constant volume in collector, 2ml solution is drawn after constant volume
After filtering with microporous membrane, be placed in brown vial refrigerate it is to be checked.
The quantitative determination of step (3) the pesticide residue concentration, further comprises：
1. being detected to sample with high performance liquid chromatography, the standard curve of pesticide concentration is established using external standard method；
2. by the response of each pesticide under liquid chromatogram difference retention time, combined standard curve calculates addition recycling
Rate.
The present invention provides a kind of to measure pesticide in brown rice (Yuan's rice) using the device under the conditions of subcritical R134a
Remaining method, includes the following steps：
(1) air-discharging：
The amount of taking fully brown rice to be measured is in high-pressure balancing kettle material barrel, after covering tightly high-pressure balancing kettle, all valves in device for opening
Door, and R134a storage tank valves are opened simultaneously, the air displacement in device is drained with R134a gases.
(2) air-leakage test：
After draining air, plunger pump is closed and opened to the reset valve of device least significant end, band pressure rises to default pressure
The valve between pressure gauge in device is closed in termination of pumping after power, and whether each unit pressure is stablized in checking device, it is ensured that without gas leakage
Situation.
(3) extraction of pesticide residue substance：
Heated for controlling temperature is carried out to device by thermostatted water oil groove, plunger is opened after temperature is increased to preset temperature and stablizes
Pump, maintains static extracting after being pressurized to preset pressure value, reset valve is opened after a period of time, plunger pump is opened in sampling process
Pressure is supplemented, so that high-pressure balancing kettle pressure is maintained near preset pressure value, i.e. dynamic extraction, dynamic extraction closes afterwards for a period of time
Reset valve is closed, the gas being during which discharged is collected by collector, the solute in collector in the suitable solvent dissolved gas of selection,
Until after extraction gas reactor all empties, the channel interior after reset valve is rinsed 5 times using solvent, and flushing liquor is collected
It is quantitative by offline high performance liquid chromatography detection after volumetric flask constant volume step by concentrating into collector.
Referring to Fig.1, it is a kind of cereals Residual Pesticides in Farm Produce pretreating device of the present invention, by fluid reservoir, refrigeration
Coil pipe, plunger pump, surge tank, thermostatted water oil groove, extraction kettle, reset valve and collector composition.The surge tank 4 and extraction
For kettle 6 by the circulating pump and autoclave body external jacket temperature control of thermostatted water oil groove 9, reset valve 7 is immersed in thermostatted water oil groove 5.
For fluid R134a, need that fluid is pre-chilled in advance before plunger pump is suppressed, before making fluid enter high-pressure pump
State be liquid.In the inlet and outlet of extraction kettle, cotton and fine screen mesh are added, prevents the grain of rice to be blown into reset valve and causes to block up
Plug.
The assay method operates as follows：
(1) preparation
1. opening refrigerator and thermostatted water oil groove in advance；
2. enough brown rice is contained in extraction kettle material barrel, the air being passed through after sealing cover in R134a dischargers is covered；
3. opening plunger pump, preset pressure is boosted to, the air-tightness of verifying attachment closes reset valve 7 after being verified, will
Collecting duct is inserted into collector.
(2) sample extraction
1. weighing brown rice sample 30g in extraction kettle material barrel, the mixed liquor 5ml of 9 kinds of pesticides is added, and by solvent in nitrogen
It dries up under the conditions of gas, then changes extraction kettle sealing cover after material barrel is put into extraction kettle.
2. closing reset valve 7, plunger pump is opened, again drains the air in material barrel, by surge tank to extraction kettle
Interior supplement R134a fluids close pump, static extracting 2h after extraction system pressure reaches preset pressure value.
3. opening reset valve 7, so that fluid in extraction kettle is inhaled by collector internal solvent, is then exhausted from after solvent absorption,
Flow velocity is small as possible complete to ensure to absorb, and opens simultaneously plunger pump, makes to supplement in extraction kettle by adjusting flow control valve
The amount of R134a is equal to reset valve discharge rate, maintains extraction kettle pressure with respect to dynamic extraction 40min under stable condition.Dynamic extracts
Reset valve 7 needs additional electric heating sheets during taking, and is heated to reset valve, reset valve is prevented to be subcooled in exhaust process,
Maintain the steady operation of reset valve.
4. after dynamic extraction, closing plunger pump and extraction kettle early gate, fluid is all by solvent in kettle to be extracted
After absorption, reset valve and follow-up gas-guide tube 3 times are rinsed using same solvent in collector, and flushing liquor is collected into collector
In.
5. drawing 2ml solution by solution constant volume in collector, after constant volume after miillpore filter (0.45m) filtering, it is placed on palm fibre
It is refrigerated in color bottle to be checked.
(3) quantitative determination of pesticide residue concentration
1. with high performance liquid chromatography (Agilent 1260, Zorbax SB-C18250mm × 4.6mm, 5m) at two not
With under testing conditions【HPLC chromatogram analysis method one (Fluoxastrobin, ethiprole, Tebuconazole, pyraclostrobin, poison with poison by Flutriafol
Tick) mobile phase：Methanol/ultra-pure water (70/30)；Sample size：20L；Flow velocity：0.7mL/min；Column temperature：35℃；Ultraviolet detection wave
It is long：230nm.HPLC chromatogram analysis method two (dinotefuran, Diacloden, imidacloprid) mobile phase：Methanol/ultra-pure water (30/70)；Into
Sample amount：20L；Flow velocity：0.7mL/min；Column temperature：35℃；Ultraviolet detection wavelength：250nm.】Sample is detected, external standard is utilized
Method establishes the standard curve of 9 kinds of pesticide concentrations.
2. by the response of each pesticide under liquid chromatogram difference retention time, combined standard curve calculates 9 pesticides
Respective TIANZHU XINGNAO Capsul.
The results are shown in Table 1 for standard curve under liquid phase chromatogram condition for (4) 9 kinds of pesticides：
Standard curve result under 1.9 kinds of pesticide liquid phase chromatogram conditions of table
As seen from table, 9 kinds of pesticides have higher curvilinear correlation under the conditions of liquid chromatographic detection.
(5) liquid chromatography results of pesticide TIANZHU XINGNAO Capsul are as shown in table 1 in device detection brown rice.
TIANZHU XINGNAO Capsul situation of (6) 9 kinds of pesticides in brown rice is as shown in table 2.
TIANZHU XINGNAO Capsul of the 2.9 kinds of pesticides of table under this glass and method
The above is only several embodiments of the present invention, not any type of limitation is done to the present invention, although this hair
It is bright to be disclosed as above with preferred embodiment, however not to limit the present invention, any person skilled in the art is not taking off
In the range of technical solution of the present invention, makes a little variation using the technology contents of the disclosure above or modification is equal to
Case study on implementation is imitated, is belonged in technical solution of the present invention protection domain.
Claims (10)
1. a kind of quickly measuring the remaining method of pesticide in cereal, which is characterized in that include the following steps：
(1) preparation；
(2) sample extraction；
(3) quantitative determination of pesticide residue concentration.
2. quickly measuring the remaining method of pesticide in cereal according to claim 1, which is characterized in that the step (1) is accurate
Standby work, further comprises：1. opening refrigerator and thermostatted water oil groove in advance.
3. quickly measuring the remaining method of pesticide in cereal according to claim 1, which is characterized in that the step (1) is accurate
Standby work, further comprises：2. cereal to be measured is contained in extraction kettle material barrel, R134a discharge dresses are passed through after covering sealing cover
Set interior air.
4. quickly measuring the remaining method of pesticide in cereal according to claim 1, which is characterized in that the step (1) is accurate
Standby work, further comprises：3. opening plunger pump, preset pressure is boosted to, the air-tightness of verifying attachment is closed after being verified
Collecting duct is inserted into collector by reset valve.
5. quickly measuring the remaining method of pesticide in cereal according to claim 1, which is characterized in that step (2) sample
Product extract, and further comprise：1. weighing cereal to be measured in extraction kettle material barrel, and solvent is dried up under a nitrogen atmosphere, so
Extraction kettle sealing cover is changed after material barrel is put into extraction kettle afterwards.
6. quickly measuring the remaining method of pesticide in cereal according to claim 1, which is characterized in that step (2) sample
Product extract, and further comprise：2. closing reset valve, plunger pump is opened, the air in material barrel is drained again, passes through surge tank
R134a fluids are supplemented into extraction kettle, and pump, static extracting 2h are closed after extraction system pressure reaches preset pressure value.
7. quickly measuring the remaining method of pesticide in cereal according to claim 1, which is characterized in that step (2) sample
Product extract, and further comprise：3. opening reset valve, fluid in extraction kettle is set to be inhaled by collector internal solvent, by solvent absorption
After be then exhausted from, flow velocity it is small as possible with ensure absorb it is complete, opens simultaneously plunger pump, by adjust flow control valve make extraction kettle
The amount of interior supplement R134a is equal to reset valve discharge rate, maintains extraction kettle pressure with respect to dynamic extraction 40min under stable condition.
8. quickly measuring the remaining method of pesticide in cereal according to claim 1, which is characterized in that step (2) sample
Product extract, and further comprise：4. after dynamic extraction, closing plunger pump and extraction kettle early gate, fluid is complete in kettle to be extracted
Reset valve and follow-up gas-guide tube 3 times rinse after solvent absorption, using same solvent in collector in portion, and flushing liquor is received
Collect in collector.
9. quickly measuring the remaining method of pesticide in cereal according to claim 1, which is characterized in that step (2) sample
Product extract, and further comprise：5. drawing 2ml solution by solution constant volume in collector, after constant volume after filtering with microporous membrane, it is placed on
It is refrigerated in brown vial to be checked.
10. quickly measuring the remaining method of pesticide in cereal according to claim 1, which is characterized in that step (3) agriculture
The quantitative determination of medicine residual concentration, further comprises：
1. being detected to sample with high performance liquid chromatography, the standard curve of pesticide concentration is established using external standard method；
2. by the response of each pesticide under liquid chromatogram difference retention time, combined standard curve calculates TIANZHU XINGNAO Capsul.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711498836.9A CN108614040A (en) | 2017-12-30 | 2017-12-30 | It is a kind of quickly to measure the remaining method of pesticide in cereal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711498836.9A CN108614040A (en) | 2017-12-30 | 2017-12-30 | It is a kind of quickly to measure the remaining method of pesticide in cereal |
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Family
ID=63658509
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101810658A (en) * | 2010-05-07 | 2010-08-25 | 青岛东仁生物医药技术有限公司 | Method for removing residual pesticide from ginseng |
| CN101905091A (en) * | 2010-07-12 | 2010-12-08 | 新疆大学 | Equipment and method for extracting biologically active ingredients from subcritical fluid |
| CN102445511A (en) * | 2011-09-22 | 2012-05-09 | 中国海洋大学 | Subcritical R134a pretreatment method for aquatic product sex hormone residue analysis sample |
| CN103549236A (en) * | 2013-10-30 | 2014-02-05 | 河南亚临界生物技术有限公司 | Method for removing pesticide residues of natural plants by virtue of subcritical dry-cleaning technique |
| CN104173399A (en) * | 2014-09-15 | 2014-12-03 | 刘智谋 | Preparation method of ginseng stem and leaf total saponins with low pesticide residues |
-
2017
- 2017-12-30 CN CN201711498836.9A patent/CN108614040A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101810658A (en) * | 2010-05-07 | 2010-08-25 | 青岛东仁生物医药技术有限公司 | Method for removing residual pesticide from ginseng |
| CN101905091A (en) * | 2010-07-12 | 2010-12-08 | 新疆大学 | Equipment and method for extracting biologically active ingredients from subcritical fluid |
| CN102445511A (en) * | 2011-09-22 | 2012-05-09 | 中国海洋大学 | Subcritical R134a pretreatment method for aquatic product sex hormone residue analysis sample |
| CN103549236A (en) * | 2013-10-30 | 2014-02-05 | 河南亚临界生物技术有限公司 | Method for removing pesticide residues of natural plants by virtue of subcritical dry-cleaning technique |
| CN104173399A (en) * | 2014-09-15 | 2014-12-03 | 刘智谋 | Preparation method of ginseng stem and leaf total saponins with low pesticide residues |
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| Title |
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Application publication date: 20181002 |