CN105758946A - Method for determining residual quantity of 15 kinds of triazole type pesticides in fruit - Google Patents
Method for determining residual quantity of 15 kinds of triazole type pesticides in fruit Download PDFInfo
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- 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
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention relates to a method for determining the residual quantity of 15 kinds of triazole type pesticides in fruit. The method comprises the following steps of (1) sample pretreatment: homogenated fruit samples are subjected to vibration shaking and high-speed centrifugation by using an acetonitrile solution, NaCl and anhydrous MgSO4 to obtain an extracting solution; then, PSA, C18 and anhydrous magnesium sulfate are selected as adsorbents to perform dispersive solid-phase extraction on the extracting solution; still standing, microporous filtering membrane passing and nitrogen gas drying through blowing are performed; next, redissolving is performed by an acetone and cyclohexane mixed solvent; uniform mixing and determination preparation are performed; (2) substrate standard solution preparation; (3) on-line gel color spectrum series gas chromatography-mass spectrum determination. The method has the characteristics of low background interference, high enrichment efficiency, high sensitivity, simplicity, convenience, high speed and accuracy, and can meet the residue monitoring requirements of the triazole type pesticides in the fruit.
Description
Technical field
The present invention relates to the assay method of a kind of pesticide residues in fruits amount, be specifically related to 15 kinds of triazole type in a kind of fruit
The assay method of persticide residue.
Background technology
Triazole pesticide belongs to organic heterocyclic compounds, of a great variety, has bactericide, insecticide, has again plant growth
Conditioning agent, have efficiently, wide spectrum, suction long-acting, interior, the good characteristic such as low toxicity, it has also become applied range, using method flexibly,
Prevention effect is good, most develop a class efficient germicide of application potential.But along with triazole pesticide in fruit use by
Gradually strengthen, its residual the food-safety problem caused the most increasingly gets more and more people's extensive concerning.In order to ensure that consumer pacifies
Entirely, triazole pesticide residual in different fruit has been formulated strict MRL and has been reached 0.010mg/kg standard also by various countries the most
Implement residual monitoring.
At present, the detection method of triazole pesticide residual is more, such as gas chromatography (GC), gas chromatography-mass spectrography
(GC-MS), the detection such as gas chromatography tandem mass spectrometry method (GC-MS/MS), Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) hand
Section, wherein hydrolysis and condensation sensitivity and accuracy are high, apply wider；But the detection of individual method limit can not expire completely
Foot MRL (MRL) requirement, the detection technique of some method is relative with Sample Pretreatment Technique backward simultaneously, and sample
Pre-treatment is that component to be measured is extracted, purifies, is enriched with, be pesticide residue analysis process the most key and and time-consuming link,
Be largely fixed the whether accurate of analysis result, and efficient pretreatment technology can also greatly reduce analysis cost and
Time.
Online gel permeation chromatography-gas chromatography-mass spectrum (GPC-GC/MS) technology be by GPC processing means before purification with
GC/MS couples composition online, uses the separating power of miniature GPC chromatographic column and GC/MS Large volume injection newly developed, it is achieved
Residues of pesticides many components are the most quickly analyzed, and have been applied to the detection of the Pesticide Residues such as veterinary antibiotics, cereal.But GPC
Purification method separating effect for the mixture that molecular dimension is identical is poor, further, since little molecule chaff interference may
It is entrained being eluted in agricultural chemicals, and the agricultural chemicals of bigger molecule first may flow out along with chaff interferences such as greases, cause and cannot separate completely
Entirely, the enrichment clean-up effect of complex sample is poor, affects the rate of recovery.
QuEChERS method development in recent years is very fast, and QuEChERS method is the earliest by Anastassiades and Lehotay etc.
Proposed in 2003, be to utilize solid phase dispersion material to be fully contacted with sample or sample extracting solution, adsorb impurity therein and obtain
To the purpose purified, or utilize solid-phase adsorbent adsorbed target analyte, then resolve and purify.QuEChERS method exists
Fruit and vegetable farming residual analysis has the advantages such as quick, simple, cheap, effective, reliable and safe, the most national in the world
It is verified with area and promotes.Have no the employing QuEChERS sample of 15 kinds of triazole pesticide residual quantities in fruit up to now
Pre-treating method combines the report of GPC-GC/MS detection method, therefore, sets up QuEChERS sample-pretreating method and combines GPC-
In GC/MS quantitative analysis fruit, the detection method of 15 kinds of triazole pesticide residual quantities is significant.
Summary of the invention
The technical problem to be solved is to provide that a kind of ambient interferences is low, bioaccumulation efficiency is high, highly sensitive, simple
Just, the assay method of 15 kinds of triazole pesticide residual quantities in fruit fast and accurately.
The present invention solves its technical problem and employed technical scheme comprise that, 15 kinds of triazole pesticide residual quantities in a kind of fruit
Assay method, comprises the following steps: the assay method of 15 kinds of triazole pesticide residual quantities in a kind of fruit, comprises the following steps:
(1) sample pre-treatments: the fruit sample after homogenate is first used acetonitrile solution, NaCl, anhydrous MgSO4, shaking is also
High speed centrifugation, obtains extract；Then PSA, C are selected18, anhydrous magnesium sulfate as adsorbent, extract is carried out dispersed solid phase extraction
Taking, stand, cross miillpore filter, nitrogen dries up, and then redissolves with acetone, hexamethylene mixed solvent, and mixing is to be checked；
(2) preparation of extraction standard solution: by Flusilazole, propiconazole in 15 kinds of triazole pesticide standard items respectively with acetone
Being configured to the standard liquid of variable concentrations, the standard that uniconazole P, hexaconazole, nitrile bacterium azoles are configured to variable concentrations with methyl alcohol respectively is molten
Liquid, residue triazole pesticide standard items are respectively adopted acetone that volume ratio is 3/7 and hexamethylene mixed solvent is made into variable concentrations
Hybrid standard working solution, be used for making standard working curve；
(3) online gel chromatography series connection Gas Chromatography-Mass Spectrometry: the matrix of each concentration gradient in step (2) is mixed
The injection of standardization solution is furnished with online gel chromatography series connection gas chromatograph-mass spectrometer and is measured, with the chromatogram of standard working solution
Peak area carries out regression analysis to its respective concentration, obtains extraction standard working curve；The most under the same conditions by step (1)
The sample liquid of middle pre-treatment is injected online gel chromatography series connection gas chromatograph-mass spectrometer and is measured, and uses external standard method to calculate 15
Plant the measured value of triazole pesticide residual quantity.
Further, in step (1), accurately weigh the fruit sample after homogenate 10.00～10.05g in 50mL plastic centrifuge
Guan Zhong, adds 10.0mL acetonitrile solution, the anhydrous MgSO of 1.0gNaCl, 4.0g4, shake 1min, with 8000r/min high speed centrifugation
5min, draws 2.0mL upper strata supernatant and proceeds to equipped with 50mgPSA, 50mgC18, 300mg anhydrous magnesium sulfate 10mL centrifuge tube in,
Vortex mixing 1min, stands, after 0.22 μm filter membrane crossed by supernatant, takes 1.0mL nitrogen and dry up, add the acetone that 1mL volume ratio is 3/7
Redissolve with hexamethylene, mixing.
Further, in step (3), GPC-GC/MS analysis condition is: decontaminating column: Shodex EV-200 gel chromatographic columns,
Column length 150mm, internal diameter 2.1mm；Detection wavelength: 210nm；Flowing phase: it is 3/7 that acetone and hexamethylene burn volume ratio, flow velocity: 0.1mL/
min；Column temperature: 40 DEG C；Sample size: 10 μ L；Chromatographic column: inertia capillary column, column length 5m, internal diameter 0.53mm, pre-column Rtx-5ms,
Column length 5m, internal diameter 0.25mm, thickness 0.25 μm, analytical column Rtx-5ms, column length 25m, internal diameter 0.25mm, thickness 0.25 μm, 3
Pillar leads to by two and threeway is used in series；PTV injection port: do not shunt constant voltage mode, temperature programming: 120 DEG C keep 5min, so
After with 80 DEG C/min temperature programming to 250 DEG C keep 36min；Column oven temperature programming: 82 DEG C keep 5min, then with 9 DEG C/
Min temperature programming, to 280 DEG C, keeps 10min；Carrier gas: helium, overall flow rate: 30.0mL/min；Column flow rate: 1.75mL/min；From
Source temperature: 200 DEG C；GC/MS interface temperature: 250 DEG C；Solvent delay time: 9.5min；Detection voltage: 0.79KV；Mass spectrum is examined
Survey pattern: Salbutamol Selected Ion Monitoring SIM, every kind of compound selects 1 quota ion, 2 qualitative ions respectively.
The present invention uses QuEChERS pre-treating method to combine GPC-GC/MS detection method, it is achieved that in-line purification with point
The automation of analysis detection, shortens analysis time, effectively reduces ambient interferences.Matrix matching mark liquid is used to carry out quantitative analysis fall
Low matrix interference, takes the temperature-programmed mode of GPC large volume sample injection and gas chromatographic sample introduction mouth to improve detection spirit simultaneously
Sensitivity.The present invention has that ambient interferences is low, bioaccumulation efficiency is high, highly sensitive, easy, feature fast and accurately, can meet fruit
Middle triazole pesticide residual monitoring requirement.
Accompanying drawing explanation
Fig. 1 is the total ion current figure of 15 kinds of agricultural chemicals (1mg/L).
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the invention will be further described.
1, instrument and reagent
GPC-GC/MS 2010Ultra online gel chromatography series connection gas chromatograph-mass spectrometer (GC-MS) (Shimadzu Corporation of Japan)；
Vertical type high-capacity supercentrifuge (Hitachi company of Japan)；N-EVAT24 Nitrogen evaporator (U.S. Organomation
Associatews)。
Acetonitrile, acetone, hexamethylene (HPLC level, Fisher company)；Acetic acid (HPLC level, J.T.Baker company of the U.S.)；
PSA、C18Adsorbent (particle size range 40～60 μm, Tianjin Beaune Ai Jieer company)；Anhydrous magnesium sulfate, sodium chloride, anhydrous acetic acid
Sodium, sodium citrate (analyzing pure, Tianjin Kermel Chemical Reagent Co., Ltd.), DisodiumHydrogen Citrate (Alfa Aesar)；Micro-
Hole filter membrane (0.22 μm, Tian Jinjin rises company).
In 15 kinds of agricultural chemicals (being shown in Table 1) standard items, (purity (purity >=97%, DR company of Germany) is respectively for Flusilazole, propiconazole
Being configured to the concentration standard liquid as 1000mg/L with acetone, uniconazole P, hexaconazole, nitrile bacterium azoles grind purchased from Ministry of Agriculture's environmental protection
Studying carefully institute, specification 100 μ g/mL, remaining agricultural chemicals standard specimen is all purchased from environmental quality supervision and inspection center of the Ministry of Agriculture (Tianjin), specification
1000mg/L.15 kinds of agricultural chemicals are made into suitable hybrid standard working solution, in-20 DEG C with acetone/hexamethylene (3/7) as required
Refrigerator preserves.Extraction standard solution: be made into the matrix mixed standard solution of variable concentrations with blank sample matrix solution, be used for
Make standard working curve, now with the current.
The retention time of table 1-15 kind agricultural chemicals, selection ion, linear equation, coefficient correlation and detection limit
Embodiment 1: the mensuration of 15 kinds of triazole pesticide residual quantities in fruit
1, sample-pretreating method
Accurately weigh the fruit sample 10g (being accurate to 0.01g) after homogenate in 50mL plastic centrifuge tube, add 10.0mL
Acetonitrile solution, the anhydrous MgSO of 1.0gNaCl, 4.0g4, shake 1min, with 8000r/min high speed centrifugation 5min, draw on 2.0mL
Layer supernatant proceeds to equipped with 50mgPSA, 50mgC18, 300mg anhydrous magnesium sulfate 10mL centrifuge tube in, vortex mixing 1min, quiet
Put, after 0.22 μm filter membrane crossed by supernatant, take 1.0mL nitrogen and dry up, add 1mL acetone/hexamethylene (3/7) and redissolve, mixing.
2, the preparation of extraction standard solution: by Flusilazole, propiconazole in 15 kinds of triazole pesticide standard items respectively with acetone
Being configured to the standard liquid of variable concentrations, the standard that uniconazole P, hexaconazole, nitrile bacterium azoles are configured to variable concentrations with methyl alcohol respectively is molten
Liquid, residue triazole pesticide standard items are respectively adopted acetone that volume ratio is 3/7 and hexamethylene mixed solvent is made into variable concentrations
Hybrid standard working solution, be used for making standard working curve；
(3) online gel chromatography series connection Gas Chromatography-Mass Spectrometry: the matrix mixed standard solution of each concentration gradient is noted
Enter to be furnished with online gel chromatography series connection gas chromatograph-mass spectrometer to be measured, with the chromatographic peak area of standard working solution to its phase
Answer concentration to carry out regression analysis, obtain extraction standard working curve；The most under the same conditions the sample liquid of pre-treatment is injected
Online gel chromatography series connection gas chromatograph-mass spectrometer is measured, and records the chromatographic peak area of triazole pesticide, generation in sample liquid
Enter extraction standard working curve, obtain triazole pesticide content in sample liquid, then according to the quality of sample representated by sample liquid
It is calculated triazole pesticide residual quantity in sample.
Wherein, GPC-GC/MS analysis condition is:
Decontaminating column: Shodex EV-200 gel chromatographic columns (150mm × 2.1mm)；Detection wavelength: 210nm；Flowing phase: third
Ketone/hexamethylene burns (3/7, V/V), flow velocity: 0.1mL/min；Column temperature: 40 DEG C；Sample size: 10 μ L.
Chromatographic column: inertia capillary column (5m × 0.53mm), pre-column Rtx-5ms (5m × 0.25mm × 0.25 μm), analyzes
Post Rtx-5ms (25m × 0.25mm × 0.25 μm), 3 pillars are logical and threeway is used in series by two；PTV injection port: do not shunt
Constant voltage mode, temperature programming: 120 DEG C keep 5min, then keep 36min with 80 DEG C/min temperature programming to 250 DEG C；Column oven
Temperature programming: 82 DEG C keep 5min, then with 9 DEG C/min temperature programming to 280 DEG C, keeps 10min；Carrier gas: helium, always flows
Speed: 30.0mL/min；Column flow rate: 1.75mL/min.
Ion source temperature: 200 DEG C；GC/MS interface temperature: 250 DEG C；Solvent delay time: 9.5min；Detection voltage:
0.79KV；Mass Spectrometer Method pattern: Salbutamol Selected Ion Monitoring SIM.Every kind of compound selects 1 quota ion respectively, 2 qualitative from
Son, concrete SIM ion parameters and total ion current figure are shown in Table 1 and Fig. 1.
3, experimental result
Under the chromatographic condition optimized, having investigated the range of linearity and the coefficient correlation of 15 kinds of triazole pesticides, result shows,
In the range of 10～400 μ g/L, matrix matching concentration of standard solution in 6 kinds of matrix of 15 kinds of compounds and corresponding peak area
In good linear relation, coefficient correlation is 0.9958～0.9999.
4, the checking of the accuracy of method
The detection limit of method is determined with 3 times of signal to noise ratios (S/N) of the chromatographic signal of 20 μ g/kg mark-on sample amounts ion pairs
It is 0.9～9.5 μ g/kg, is shown in Table 2.
The 15 kinds of triazole pesticide mixed standard solutions adding 20,50,100 μ g/kg in 6 kinds of matrix respectively carry out mark-on
The rate of recovery is tested, and each spiked levels replication 6 times, the rate of recovery of 15 kinds of agricultural chemicals is 82.7%～116.1%, relative standard
Deviation (RSD) is 0.2%～9.9%.Method meets the testing requirement of domestic and international residue limits.
Table 2-15 kind agricultural chemicals is in the recovery of standard addition of 6 kinds of matrix and relative standard deviation (n=6)
Claims (3)
1. the assay method of 15 kinds of triazole pesticide residual quantities in a fruit, it is characterised in that comprise the following steps:
(1) sample pre-treatments: the fruit sample after homogenate is first used acetonitrile solution, NaCl, anhydrous MgSO4, shaking and at a high speed from
The heart, obtains extract；Then PSA, C are selected18, anhydrous magnesium sulfate as adsorbent, extract is carried out dispersive solid-phase extraction, quiet
Putting, cross miillpore filter, nitrogen dries up, and then redissolves with acetone, hexamethylene mixed solvent, and mixing is to be checked；
(2) preparation of extraction standard solution: Flusilazole, propiconazole in 15 kinds of triazole pesticide standard items are prepared with acetone respectively
Becoming the standard liquid of variable concentrations, uniconazole P, hexaconazole, nitrile bacterium azoles are configured to the standard liquid of variable concentrations respectively with methyl alcohol,
Residue triazole pesticide standard items are respectively adopted acetone that volume ratio is 3/7 and hexamethylene mixed solvent is made into the mixed of variable concentrations
Standardization working solution；
(3) online gel chromatography series connection Gas Chromatography-Mass Spectrometry: the matrix of each concentration gradient in step (2) is mixed mark
The injection of quasi-solution is furnished with online gel chromatography series connection gas chromatograph-mass spectrometer and is measured, with the chromatographic peak face of standard working solution
Amass and its respective concentration is carried out regression analysis, obtain extraction standard working curve；The most under the same conditions by before in step (1)
The sample liquid processed is injected online gel chromatography series connection gas chromatograph-mass spectrometer and is measured, and uses external standard method to calculate 15 kind three
The measured value of azoles farm chemicals residual quantity.
The assay method of 15 kinds of triazole pesticide residual quantities in fruit the most according to claim 1, it is characterised in that step
(1) in, accurately weigh the fruit sample after homogenate 10.00～10.05g in 50mL plastic centrifuge tube, add 10.0mL acetonitrile
Solution, the anhydrous MgSO of 1.0gNaCl, 4.0g4, shake 1min, with 8000r/min high speed centrifugation 5min, draw on 2.0mL upper strata
Clear liquid proceeds to equipped with 50mgPSA, 50mgC18, 300mg anhydrous magnesium sulfate 10mL centrifuge tube in, vortex mixing 1min, stand, on
After 0.22 μm filter membrane crossed by clear liquid, take 1.0mL nitrogen and dry up, add acetone and hexamethylene redissolution, mixing that 1mL volume ratio is 3/7.
The assay method of 15 kinds of triazole pesticide residual quantities in fruit the most according to claim 1 and 2, it is characterised in that
In step (3), GPC-GC/MS analysis condition is: decontaminating column: Shodex EV-200 gel chromatographic columns, column length 150mm, internal diameter
2.1mm；Detection wavelength: 210nm；Flowing phase: it is 3/7 that acetone and hexamethylene burn volume ratio, flow velocity: 0.1mL/min；Column temperature: 40 DEG C；
Sample size: 10 μ L；Chromatographic column: inertia capillary column, column length 5m, internal diameter 0.53mm, pre-column Rtx-5ms, column length 5m, internal diameter
0.25mm, thickness 0.25 μm, analytical column Rtx-5ms, column length 25m, internal diameter 0.25mm, thickness 0.25 μm, 3 pillars lead to by two
It is used in series with threeway；PTV injection port: do not shunt constant voltage mode, temperature programming: 120 DEG C keep 5min, then with 80 DEG C/min
Temperature programming keeps 36min to 250 DEG C；Column oven temperature programming: 82 DEG C keep 5min, then with 9 DEG C/min temperature programming extremely
280 DEG C, keep 10min；Carrier gas: helium, overall flow rate: 30.0mL/min；Column flow rate: 1.75mL/min；Ion source temperature: 200
℃；GC/MS interface temperature: 250 DEG C；Solvent delay time: 9.5min；Detection voltage: 0.79KV；Mass Spectrometer Method pattern: select
Ion monitoring SIM, every kind of compound selects 1 quota ion, 2 qualitative ions respectively.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106370758A (en) * | 2016-11-30 | 2017-02-01 | 中国检验检疫科学研究院 | Chinese herbal medicine improved QuEChERS filler bag and application thereof in detection of Chinese herbal medicine pesticide residues |
| CN106770841A (en) * | 2017-03-23 | 2017-05-31 | 西北师范大学 | The method that fruit Pesticides Testing sample is processed using QuEChERS abstraction techniques |
| CN108226343A (en) * | 2018-01-08 | 2018-06-29 | 中国检验检疫科学研究院综合检测中心 | Multiple Pesticides method for detecting residue in a kind of vegetables and fruits |
| CN108414493A (en) * | 2018-01-18 | 2018-08-17 | 上海海洋大学 | A kind of method of quick detection Flusilazole |
| CN109470809A (en) * | 2018-12-13 | 2019-03-15 | 浙江工业大学 | Method for analyzing triazole pesticide residues in water |
| CN112229929A (en) * | 2020-10-10 | 2021-01-15 | 贵阳海关综合技术中心(贵州国际旅行卫生保健中心、贵阳海关口岸门诊部) | Method for on-line GPC-GC-MS/MS non-target rapid screening of pesticide residues in tea |
| CN114252311A (en) * | 2021-10-27 | 2022-03-29 | 上海市农产品质量安全中心 | Method for carrying out in-situ rapid detection pretreatment on pesticide residues in vegetables and fruits |
| CN115236221A (en) * | 2022-06-29 | 2022-10-25 | 江苏康达检测技术股份有限公司 | Method for detecting dihydric alcohol compound in environmental medium |
| CN115656395A (en) * | 2022-08-17 | 2023-01-31 | 山东省产品质量检验研究院 | Method for measuring multiple pesticide residues in soil by using dispersed solid phase extraction |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106370758A (en) * | 2016-11-30 | 2017-02-01 | 中国检验检疫科学研究院 | Chinese herbal medicine improved QuEChERS filler bag and application thereof in detection of Chinese herbal medicine pesticide residues |
| CN106770841A (en) * | 2017-03-23 | 2017-05-31 | 西北师范大学 | The method that fruit Pesticides Testing sample is processed using QuEChERS abstraction techniques |
| CN108226343A (en) * | 2018-01-08 | 2018-06-29 | 中国检验检疫科学研究院综合检测中心 | Multiple Pesticides method for detecting residue in a kind of vegetables and fruits |
| CN108414493A (en) * | 2018-01-18 | 2018-08-17 | 上海海洋大学 | A kind of method of quick detection Flusilazole |
| CN109470809A (en) * | 2018-12-13 | 2019-03-15 | 浙江工业大学 | Method for analyzing triazole pesticide residues in water |
| CN112229929A (en) * | 2020-10-10 | 2021-01-15 | 贵阳海关综合技术中心(贵州国际旅行卫生保健中心、贵阳海关口岸门诊部) | Method for on-line GPC-GC-MS/MS non-target rapid screening of pesticide residues in tea |
| CN114252311A (en) * | 2021-10-27 | 2022-03-29 | 上海市农产品质量安全中心 | Method for carrying out in-situ rapid detection pretreatment on pesticide residues in vegetables and fruits |
| CN115236221A (en) * | 2022-06-29 | 2022-10-25 | 江苏康达检测技术股份有限公司 | Method for detecting dihydric alcohol compound in environmental medium |
| CN115656395A (en) * | 2022-08-17 | 2023-01-31 | 山东省产品质量检验研究院 | Method for measuring multiple pesticide residues in soil by using dispersed solid phase extraction |
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