CN109100450A - The rapid detection method of diquat dibromide and paraquat residual quantity in a kind of food - Google Patents
The rapid detection method of diquat dibromide and paraquat residual quantity in a kind of food Download PDFInfo
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- CN109100450A CN109100450A CN201811395991.2A CN201811395991A CN109100450A CN 109100450 A CN109100450 A CN 109100450A CN 201811395991 A CN201811395991 A CN 201811395991A CN 109100450 A CN109100450 A CN 109100450A
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
- G01N30/7233—Mass spectrometers interfaced to liquid or supercritical fluid chromatograph
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- G01N30/726—Nebulising, aerosol formation or ionisation by electrical or glow discharge
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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 invention discloses the rapid detection methods of diquat dibromide and paraquat residual quantity in a kind of food, more particularly to a kind of triple level four bars mass spectrums of ultra performance liquid chromatography-series connection based on hydrophilic Interaction Chromatography HILIC mode, detect the detection method of diquat dibromide and paraquat residual quantity in food, step includes extracting, purification, crossing film filtering, triple level four bars Mass Spectrometer Methods of connecting.Method of the invention is easy to operate, favorable reproducibility, effectively remove the impurity in sample extracting solution, qualitative and quantitative analysis quickly can be carried out simultaneously to diquat dibromide in food and paraquat pesticide, China and European Union, the U.S., Japan are fully met to the technical requirements of safety detection, strong technical support will be provided to ensure that our people's food safety and export abroad trade develop in a healthy way.
Description
Technical field
The invention belongs to the fast of diquat dibromide in technical field of food detection more particularly to a kind of food and paraquat residual quantity
Fast detection method.
Background technique
Paraquat, chemical name are 1,1 '-dimethyl -4, and 4 ' bipyridine cation salt are a kind of quick total weed controls
Agent has action of contace poison and certain systemic action.It can be absorbed by plant green tissues rapidly, keep its withered.To non-green tissue
Do not act on.It is passivated in conjunction with soil rapidly in the soil, it is invalid to plant root and perennial subterranean stem and perennial root.Hundred grass
It is withered very big to people's toxicity, and without special efficacy antidote, the oral ingestion death rate is prohibited by more than 20 countries at present up to 90% or more
It limits only or strictly and uses.From on July 1st, 2014, the registration of revocation paraquat aqua and production permit stopped life in China
It produces;But retains the outlet of Mu Yao manufacturing enterprise aqua overseas using registering, allowing to specialize in outlet production, stop aqua and sell at home
With use.Stopping on July 1st, 2016 aqua is sold and is used at home.
Diquat dibromide is generally used for conductibility and tags steriland herbicide, can be rapidly by green plants tissue resorption, with soil
It loses activity quickly after contact.For the weedings such as before crop field, orchard, bare place, harvesting, it is also used as potato and pachyrhizus
Cauline leaf is urged withered.It is more preferable that with paraquat effect is used together in the serious place of gramineae weed.
At present in blood plasma, surface water and environment paraquat and the research of diquat dibromide method for detecting residue it is more, and to food
Method for detecting residue in product is less.To vegetable food detection method, mainly according to professional standard, " SN/T 0293-2014 goes out
Measurement liquid chromatography-mass spectrography/mass spectrography of paraquat and diquat dibromide residual quantity in the plant-derived food of mouth ", this method does not relate to
And in animal food paraquat and diquat dibromide detection method, this method uses hydrochloric acid, and it is stronger to belong to easily system poison and corrosivity
Reagent, it is not friendly enough to human and environment, and method and step have aqueous solution concentration, accurately adjust extracting liquid pH value, ion hand over
The tedious steps such as Solid Phase Extraction are changed, consumption cost is taken time and effort very much.
Therefore, quick, effective, sensitive, reliable and practical residue analysis method is established, is had for food safety important
Realistic meaning.
Summary of the invention
The present invention in view of the above-mentioned deficiencies in the prior art, using liquid-liquid extraction techniques and solid phase extraction techniques to sample
Product are pre-processed, and in conjunction with hydrophilic interaction HILIC chromatographic separation technology, high performance liquid chromatography tandem mass spectrum technology, provide one kind
Fast and efficiently in food the detection of diquat dibromide and paraquat residual quantity method.
The technical scheme to solve the above technical problems is that in food diquat dibromide and paraquat residual quantity detection side
Method, comprising the following steps:
(1) it extracts: weighing sample into plastic centrifuge tube, formic acid is added, (mixed volume ratio is the mixed solution of first alcohol and water
1:40:60), sufficient vortex mixes, and is centrifuged, obtains extracting solution；
(2) it purifies: the extracting solution obtained after step (1) centrifugation being crossed into hydrophilelipophile copolymer Solid Phase Extraction column purification, is obtained net
Change liquid；
(3) it crosses film filtering: the scavenging solution that step (2) obtains being crossed into 0.22 μm of polytetrafluoroethylene film, to upper machine testing；
(4) triple level four bars mass spectrums (UPLC/MS/MS) of connecting are detected:
Instrument condition:
Mobile phase: A: the aqueous solution of the 150 mM ammonium formate containing 0.2 % formic acid, B: acetonitrile
Ionization mode: ESI+ mode
Chromatographic column: ACQUITY UPLCTMBEH HILIC Column(internal diameter 2.1mm × 100 mm of length, 1.7 μm of partial size)
Sample volume: 1 μ L
Chromatographic separation condition is as follows:
Mass Spectrometry Conditions: multiple-reaction monitoring (MRM) scan pattern, diquat dibromide and paraquat multiple-reaction monitoring (MRM) sweep parameter are such as
Following table:
Wherein band * is quota ion.
Further, step (1) is to weigh 5.0 g of sample of uniform sample preparation in 50 mL centrifuge tubes, and 10.0 mL first are added
The mixed solution (mixed volume ratio is 1:40:60) of acid, first alcohol and water, sufficient vortex mixes, 4000 r/min centrifugation 5
Min, supernatant are transferred in a 25 mL plastics colorimetric cylinders, and residue uses the mixed solution of 10.0 mL formic acid, first alcohol and water again
(mixed volume ratio is 1:40:60), sufficient vortex mixes, and 4000 r/min are centrifuged 5 min, merges extracting solution twice, is used in combination
Formic acid, first alcohol and water mixed solution be settled to 25.0 mL, it is to be clean after mixing.Step (2) is to obtain step (1)
To 5.0 mL of extracting solution cross hydrophilelipophile copolymer solid-phase extraction column, purify, directly collection, the solid-phase extraction column in advance according to
The secondary extracting solution with 3 mL methanol, 3 mL water, 3 mL steps (1) activates.The scavenging solution mistake that step (3) obtains step (2)
0.22 μm of teflon membrane filter (PTFE filter membrane) is filtered in plastics (PP material) sample injection bottle.It is by step (3) in step (4)
Resulting filtrate, according to instrument condition described in step (4), upper machine testing.
The beneficial effects of the present invention are: the method pair that the present invention is combined using liquid-liquid extraction techniques and solid phase extraction techniques
Sample is pre-processed.Liquid-liquid extraction techniques basic operation is to utilize compound in the solvent of two kinds immiscible (or slightly soluble)
The difference of solubility or distribution coefficient is transferred to compound in another solvent from a kind of solvent；Solid phase extraction techniques
Basic operation is exactly that the target compound or impurity absorption in fluid sample are made the matrix of sample and done using solid absorbent
It disturbs compound to separate with target compound, achievees the purpose that separation and enrichment target compound.The present invention utilizes hydrophilic interaction
HILIC chromatographic separation technology carries out chromatographic isolation to sample.Hydrophilic interaction HILIC chromatographic isolation is to be different from normal-phase chromatography, anti-
A kind of anti-reversed phase chromatography separation technology of phase chromatography and ion chromatography, it can retain and separate highly polar diquat dibromide and paraquat.
The method of the present invention detects diquat dibromide and paraquat in food, can rapidly carry out qualitative, quantitative, and detection limit is fully able to meet
Detection demand, detection efficiency greatly promote.
The present invention uses formic acid, the mixed solution of first alcohol and water (then pass through for 1:40:60) extraction by mixed volume ratio
Hydrophilelipophile copolymer Solid Phase Extraction column purification can effectively remove the interference impurity such as fatty acid, sugar, fat in component, keep away
Exempt from very friendly to human and environment using easily system poison, mordant hazardous agents, the present invention such as hydrochloric acid in conventional method.
Sample pre-treatments step of the invention is simple and quick, can be completed within single sample -20 minutes 15 minutes, upper machine examination
It surveys using highly sensitive UPLC-MS/MS detection, chromatographic isolation can be completed within 3.5 minutes, entire detection process is in half an hour
It is interior, can be accurate qualitative, quantitative, method detection is limited to 0.01 mg/kg.It is compared with the traditional method compared with the present invention does not need to rotate
The cumbersome enrichment procedures such as evaporation, the dry, concentration of nitrogen, time saving, laborsaving, cost-saving of the invention, and efficiently, quickly, accurate, essence
Degree is high.
Detailed description of the invention
Fig. 1 diquat dibromide liquid chromatography-mass spectrography/mass spectrum multiple-reaction monitoring chromatogram, Fig. 2 paraquat liquid chromatography-mass spectrography/
Mass spectrum multiple-reaction monitoring chromatogram.
Specific embodiment
The principle and features of the present invention will be described below with reference to the accompanying drawings, and the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the invention.
Prepare diquat dibromide and paraquat standard solution, take negative spinach, apple, pork, homogeneous crushes uniformly, respectively to
Spinach, apple, the mixed mark that 3 kinds of various concentrations are added in pork, addition concentration are 10 μ g/kg, 20 μ g/kg, 100 μ g/kg, in
Freezer storage is spare in -18 DEG C of refrigerators, pitch-based sphere be equal to or less than China limit standard, each contents level repeats
10 times.
Embodiment 1: taking above-mentioned spinach samples, detects its diquat dibromide and residual content of paraquat, steps are as follows:
(1) extract: weigh 5.0 g of spinach samples of uniform sample preparation in 50 mL centrifuge tubes, be added 10.0 mL formic acid, methanol and
The mixed solution (mixed volume ratio is 1:40:60) of water, sufficient vortex mixes, and 4000 r/min are centrifuged 5 min, supernatant
It is transferred in a 25 mL plastics colorimetric cylinders, residue uses the mixed solution (mixed volume of 10.0 mL formic acid, first alcohol and water again
Ratio is 1:40:60), sufficient vortex mixes, and 4000 r/min are centrifuged 5 min, merges extracting solution twice, and with formic acid, methanol
25.0 mL are settled to the mixed solution of water, it is to be clean after mixing.
(2) it purifies: 5.0 mL of extracting solution that step (1) obtains is crossed into hydrophilelipophile copolymer solid-phase extraction column, purify,
It directly collects, which is successively activated with the extracting solution of 3 mL methanol, 3 mL water, 3 mL steps (1) in advance.
(3) it crosses film filtering: the scavenging solution that step (2) obtains is crossed into 0.22 μm of teflon membrane filter (PTFE filter membrane),
It filters in plastics (PP material) sample injection bottle.
(4) UPLC/MS/MS is detected:
Instrument condition:
Mobile phase: A: the 150 mM formic acid aqueous ammonium containing 0.2 % formic acid, B: acetonitrile
Ionization mode: ESI+ mode
Chromatographic column: ACQUITY UPLCTMBEH HILIC Column(internal diameter 2.1mm × 100 mm of length, 1.7 μm of partial size)
Sample volume: 1 μ L
Chromatographic separation condition is as follows:
Mass Spectrometry Conditions: multiple-reaction monitoring (MRM) scan pattern.
Diquat dibromide and paraquat multiple-reaction monitoring (MRM) sweep parameter are as follows:
Band * is quota ion in table.
The average recovery rate and relative standard deviation RSD of diquat dibromide and residual content of paraquat in obtained spinach are shown in
Table 1.
Embodiment 2: above-mentioned apple sample is taken, detects its diquat dibromide and residual content of paraquat, steps are as follows:
(1) extract: weigh 5.0 g of apple sample of uniform sample preparation in 50 mL centrifuge tubes, be added 10.0 mL formic acid, methanol and
The mixed solution (mixed volume ratio is 1:40:60) of water, sufficient vortex mixes, and 4000 r/min are centrifuged 5 min, supernatant
It is transferred in a 25 mL plastics colorimetric cylinders, residue uses the mixed solution (mixed volume of 10.0 mL formic acid, first alcohol and water again
Ratio is 1:40:60), sufficient vortex mixes, and 4000 r/min are centrifuged 5 min, merges extracting solution twice, and with formic acid, methanol
25.0 mL are settled to the mixed solution of water, it is to be clean after mixing.
(2) it purifies: 5.0 mL of extracting solution that step (1) obtains is crossed into hydrophilelipophile copolymer solid-phase extraction column, purify,
It directly collects, which is successively activated with the extracting solution of 3 mL methanol, 3 mL water, 3 mL steps (1) in advance.
(3) it crosses film filtering: the scavenging solution that step (2) obtains is crossed into 0.22 μm of teflon membrane filter (PTFE filter membrane),
It filters in plastics (PP material) sample injection bottle.
(4) UPLC/MS/MS is detected:
Instrument condition:
Mobile phase: A: the 150 mM formic acid aqueous ammonium containing 0.2 % formic acid, B: acetonitrile
Ionization mode: ESI+ mode
Chromatographic column: ACQUITY UPLCTMBEH HILIC Column(internal diameter 2.1mm × 100 mm of length, 1.7 μm of partial size)
Sample volume: 1 μ L
Chromatographic separation condition is as follows:
Mass Spectrometry Conditions: multiple-reaction monitoring (MRM) scan pattern.
Diquat dibromide and paraquat multiple-reaction monitoring (MRM) sweep parameter are as follows:
Band * is quota ion in table.
The average recovery rate and relative standard deviation RSD of diquat dibromide and residual content of paraquat in obtained apple are shown in
The following table 1.
Embodiment 3: above-mentioned pork sample is taken, detects its diquat dibromide and residual content of paraquat, steps are as follows:
(1) extract: weigh 5.0 g of pork sample of uniform sample preparation in 50 mL centrifuge tubes, be added 10.0 mL formic acid, methanol and
The mixed solution (mixed volume ratio is 1:40:60) of water, sufficient vortex mixes, and 4000 r/min are centrifuged 5 min, supernatant
It is transferred in a 25 mL plastics colorimetric cylinders, residue uses the mixed solution (mixed volume of 10.0 mL formic acid, first alcohol and water again
Ratio is 1:40:60), sufficient vortex mixes, and 4000 r/min are centrifuged 5 min, merges extracting solution twice, and with formic acid, methanol
25.0 mL are settled to the mixed solution of water, it is to be clean after mixing.
(2) it purifies: 5.0 mL of extracting solution that step (1) obtains is crossed into hydrophilelipophile copolymer solid-phase extraction column, purify,
It directly collects, which is successively activated with the extracting solution of 3 mL methanol, 3 mL water, 3 mL steps (1) in advance.
(3) it crosses film filtering: the scavenging solution that step (2) obtains is crossed into 0.22 μm of teflon membrane filter (PTFE filter membrane),
It filters in plastics (PP material) sample injection bottle.
(4) UPLC/MS/MS is detected:
Instrument condition:
Mobile phase: A: the 150 mM formic acid aqueous ammonium containing 0.2 % formic acid, B: acetonitrile
Ionization mode: ESI+ mode
Chromatographic column: ACQUITY UPLCTMBEH HILIC Column(internal diameter 2.1mm × 100 mm of length, 1.7 μm of partial size)
Sample volume: 1 μ L
Chromatographic separation condition is as follows:
Mass Spectrometry Conditions: multiple-reaction monitoring (MRM) scan pattern.
Diquat dibromide and paraquat multiple-reaction monitoring (MRM) sweep parameter are as follows:
Band * is quota ion in table.
The average recovery rate and relative standard deviation RSD of diquat dibromide and residual content of paraquat in obtained pork are shown in
The following table 1.
Table 1: diquat dibromide and the paraquat rate of recovery and relative standard deviation (n=10) in food
As can be seen from the data in the table, the average recovery rate of diquat dibromide and paraquat is 73% ~ 92% in various food, relative standard
Deviation RSD < 10%, the rate of recovery and relative standard deviation meet Detecting Pesticide standard.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (6)
1. the rapid detection method of diquat dibromide and paraquat residual quantity in a kind of food, it is characterised in that the following steps are included:
(1) it extracts: weighing sample into plastic centrifuge tube, the mixed solution of formic acid, first alcohol and water, three in mixed solution is added
The volume ratio of component is 1:40:60, and sufficient vortex mixes, is centrifuged, obtains extracting solution；
(2) it purifies: the extracting solution obtained after step (1) centrifugation being crossed into hydrophilelipophile copolymer Solid Phase Extraction column purification, is obtained net
Change liquid；
(3) cross film filtering: the scavenging solution that step (2) is obtained passes through 0.22 μm of polytetrafluoroethylene film, to upper machine testing；
(4) the triple level four bars Mass Spectrometer Methods of series connection:
Instrument condition:
Mobile phase: A: the 150 mM formic acid aqueous ammonium containing 0.2 % formic acid, B: acetonitrile
Ionization mode: ESI+ mode
Chromatographic column: ACQUITY UPLCTM BEH HILIC Column, internal diameter 2.1mm × 100 mm of length, 1.7 μm of partial size
Sample volume: 1 μ L
Chromatographic separation condition is as follows:
Mass Spectrometry Conditions: diquat dibromide and paraquat multiple-reaction monitoring sweep parameter are as follows:
Wherein band * is quota ion.
2. the rapid detection method of diquat dibromide and paraquat residual quantity in food according to claim 1, it is characterised in that
Extraction as described in step (1) is to weigh 5.0 g of sample of uniform sample preparation in 50 mL centrifuge tubes, 10.0 mL formic acid of addition,
The mixed solution of first alcohol and water, sufficient vortex mix, and 4000 r/min are centrifuged 5 min, and supernatant is transferred to a 25 mL modeling
Expect in colorimetric cylinder, residue uses the mixed solution of 10.0 mL formic acid, first alcohol and water again, and sufficient vortex mixes, 4000 r/min from
5 min of the heart merges extracting solution twice, and is settled to 25.0 mL with the mixed solution of formic acid, first alcohol and water, after mixing
It is to be clean.
3. the rapid detection method of diquat dibromide and paraquat residual quantity in food according to claim 1, it is characterised in that
Purification described in step (2) is that 5.0 mL of extracting solution that step (1) obtains is crossed hydrophilelipophile copolymer solid-phase extraction column,
Purification is directly collected, which is successively activated with the extracting solution of 3 mL methanol, 3 mL water, 3 mL steps (1) in advance.
4. the rapid detection method of diquat dibromide and paraquat residual quantity, feature exist in middle food according to claim 1
It is that the scavenging solution for obtaining step (2) passes through 0.22 μm of teflon membrane filter, filter that film filtering is crossed described in step (3)
Enter in plastics sample injection bottle, to upper machine testing.
5. the rapid detection method of diquat dibromide and paraquat residual quantity in food according to claim 1, it is characterised in that
The triple level four bars Mass Spectrometer Methods of series connection described in step (4) are step (3) resulting filtrate, according to instrument described in step (4)
Device condition, upper machine testing.
6. the rapid detection method of diquat dibromide and paraquat residual quantity in food according to claim 1, it is characterised in that
All vessel used in step (1)-(4), equipment are non-glass material.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109959737A (en) * | 2019-04-10 | 2019-07-02 | 珠海天祥粤澳质量技术服务有限公司 | The detection method of paraquat in traditional Chinese medicinal material raw materials |
| CN112098538A (en) * | 2020-08-26 | 2020-12-18 | 中国农业科学院茶叶研究所 | Method for detecting paraquat in different tea species |
| CN112578058A (en) * | 2020-12-10 | 2021-03-30 | 北京农业质量标准与检测技术研究中心 | Method for extracting paraquat in oil |
| CN113049691A (en) * | 2020-12-15 | 2021-06-29 | 通标标准技术服务（青岛）有限公司 | Pretreatment method and residual quantity detection method of diquat in food |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109959737A (en) * | 2019-04-10 | 2019-07-02 | 珠海天祥粤澳质量技术服务有限公司 | The detection method of paraquat in traditional Chinese medicinal material raw materials |
| CN112098538A (en) * | 2020-08-26 | 2020-12-18 | 中国农业科学院茶叶研究所 | Method for detecting paraquat in different tea species |
| CN112578058A (en) * | 2020-12-10 | 2021-03-30 | 北京农业质量标准与检测技术研究中心 | Method for extracting paraquat in oil |
| CN113049691A (en) * | 2020-12-15 | 2021-06-29 | 通标标准技术服务（青岛）有限公司 | Pretreatment method and residual quantity detection method of diquat in food |
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Application publication date: 20181228 |