CN107843660A - It is a kind of at the same determine it is dark brownish green in 124 kinds of residues of pesticides method analysis method - Google Patents
It is a kind of at the same determine it is dark brownish green in 124 kinds of residues of pesticides method analysis method Download PDFInfo
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Abstract
The invention discloses it is a kind of and meanwhile determine it is dark brownish green in 124 kinds of residues of pesticides detection method, it is characterised in that：Comprise the following steps：A, sample pre-treatments；B, examination with computer liquid is handled：Fast qualitative quantitative detecting analysis, extract solution in A is taken, determined with liquid chromatography mass combination is utilized after dilution in acetonitrile；Accurate qualitative and quantitative detection analysis, high anhydrous sodium sulfate is added in nh 2 column, acetonitrile toluene solution prewashing post is first used before sample-adding, when liquid level reaches the top of sodium sulphate, rapid aforementioned sample extract solution of drawing is transferred on decontaminating column, again with acetonitrile toluene solution elution agricultural chemicals, all filtrates are combined in, spin concentration is done near in 45 DEG C of water-baths, nitrogen dries up at 30 35 DEG C, acetonitrile solution dissolved residue, after 0.2 μm of filtering with microporous membrane, for liquid chromatography tandem mass spectroscopy；C, mass spectroscopy：Measure liquid in step B is subjected to accurate qualitative and quantitative analysis with liquid chromatography mass combined instrument.
Description
Technical field
The present invention relates to it is a kind of and meanwhile determine it is dark brownish green in 124 kinds of residues of pesticides method analysis method, belong to agricultural product
Pesticide Residues composition detection technical field.
Background technology
In recent years, Guizhou gives full play to the advantage in resources, and increases agricultural restructuring dynamics, prominent to do a good job of it the advantages such as tealeaves spy
Color industry.6,890,000 mu of the whole province's Tea planting area in 2015, cultivated area have occupy first, the whole nation, and the comprehensive output value reaches nearly hundred
Hundred million yuan.Quality and safety of tea is the important foundation for ensureing our province Tea Industry sustainable development.Food and drug administration general bureau on
Further strengthen the notice [food medicine prison food prison (2017) 29] of quality and safety of tea supervision, it is indicated that maintain strict control over raw material and enter factory pass
Safety is closed to improve the security of tealeaves, ensures the life security of the people.
Dark brownish green is the raw material for producing tealeaves, and the dark brownish green raw material of the particularly part tea-enterprise of our province is mainly derived from tea
Blue or green trade market, dark brownish green also progressively to turn into one of the agricultural product of our province always, this also proposes one to agricultural sector and new ground
Study carefully with supervision of quality safety field, the detection for carrying out the dark brownish green Pesticide Residues of quick detection is surveyed with speed at present, but is being tested and analyzed
The middle trying situation that establishing criteria support is can not find in the presence of detection, this just hinders the supervision and detection to dark brownish green residues of pesticides,
Whether dark brownish green quality safety determines the quality safety of tealeaves, so as to ensure the quality safety of tealeaves, should strengthen dark brownish green
The residual detection of agriculture ensures quality and safety of tea.Quality and safety of tea is the important foundation for ensureing tea industry sustainable development, and dark brownish green
It is the raw material for producing tealeaves, the dark brownish green whether safe quality safety for determining tealeaves, and the sustainable development of tea industry
Property.The detection method of Chinese tea Pesticide Residues mainly has gas-chromatography-flame spectrometry and gas-chromatography-electronics to catch at present
Obtain method etc., and the detection method on the dark brownish green Pesticide Residues of tealeaves raw material is less, cause it is dark brownish green in more residues of pesticides inspection
Blank is surveyed, adds the risk of the residues of pesticides detection in sample tea.
In Tea Production, under ermal physics chemical action, using the chemical composition contained in dark brownish green as response matrix, with de-
The reaction formations such as water, hydrolysis, substitution, isomery, oxidation, reduction, original chemical composition is not only set to occur in quantity, proportion of composing
Change in upper, chemical constitution, and with the formation of a large amount of novel substances, increase detection difficulty.Due to dark brownish green and tealeaves chemistry
Composition has larger difference, significant so as to establish the detection method of a dark brownish green middle Multiple Pesticides residual.
The content of the invention
The technical problem to be solved in the present invention is：A kind of method for determining dark brownish green residues of pesticides is provided, not only with sensitive
Degree is high, and accuracy is good, and analyze speed is fast, and the advantages that can analyze 124 kinds of farm chemical ingredients simultaneously, and instrument have it is very high
Detection selectivity, can solve interference of the sample impurity to testing result, with overcome the deficiencies in the prior art.
The technical scheme is that：One kind liquid chromatograph-mass spectrometer determine simultaneously it is dark brownish green in 124 kinds of agricultural chemicals it is residual
The method stayed, comprises the following steps：
A, sample pre-treatments：The dark brownish green fresh leaf powder of 10g is weighed in centrifuge tube, it is molten then to add 20mL1% acetate acetonitriles
Liquid, NaCl is added after high-speed homogenization extraction, after fully shaking mixes, centrifugation layering, take supernatant standby；
B, examination with computer liquid is handled：Fast qualitative quantitative detecting analysis, foregoing constant volume liquid 1.0mL is taken, with 1.0 mL acetonitriles
Determined after dilution using liquid chromatograph mass spectrography.Accurate qualitative and quantitative detection analysis, adds about 2cm high nothings in nh 2 column
Aqueous sodium persulfate, 5mL acetonitrile-methylbenzenes (3 are first used before being loaded:1) solution prewashing post, when liquid level reaches the top of sodium sulphate, rapidly
Aforementioned sample extract solution 4mL is drawn to be transferred on decontaminating column, then with 25mL acetonitrile-methylbenzenes (3:1) solution elution agricultural chemicals, all filters
Liquid is collected in 100mL pear shape bottles, and spin concentration is to about 0.5mL in 45 DEG C of water-baths, the nitrogen drying at 35 DEG C, and 2mL acetonitriles-
Aqueous dissolution residue, after 0.2 μm of filtering with microporous membrane, determined for liquid chromatography tandom mass spectrometry determination.
C, mass spectroscopy：Measure liquid in step B is subjected to qualitative and quantitative analysis with liquid chromatograph-mass spectrometer.
The method of the method analysis of 124 kinds of residues of pesticides during described measure is dark brownish green, it is characterised in that：Liquid chromatogram-matter
Composing the condition that combined instrument is analyzed is：Chromatographic column：Phenomenex Luna C18 (2) 100A, 3 μm, 150 mm × 2mm internal diameters；Stream
Dynamic phase and condition of gradient elution see attached list 1；Column temperature：40℃；Sample size：2μL；Ionize source module：ESI+；Atomization gas：Nitrogen；Mist
Change atmospheric pressure：60psi；Aid in gas：50psi gas curtain gas：25psi, ion spray voltage：5500V；Dry temperature degree：650℃；
Dry gas stream speed：10L/min；Fragmentation voltage is referring to table 1 in monitoring ion pair, collision gas energy and source.How anti-selective ion is
Monitoring pattern is answered to scan (SRM), the data acquisition of detector gathers for split time window.
Determined while described it is dark brownish green in 124 kinds of farm chemical ingredients method, it is characterised in that：124 kinds of agricultural chemicals, wherein
73 kinds of insecticide, 31 kinds of bactericide, 6 kinds of acaricide, 14 kinds of herbicide；35 kinds of organophosphorus insecticides, carbamates kill
20 kinds of worm agent, 6 kinds of nicotinic insecticide；Include China national standard GB2763-2016《Pesticide maximum residue limit is limited the quantity》In
To in the agricultural chemicals of Pesticide Residues in Tea finite quantity requirement except glufosinate-ammonium and glyphosate other 46 agricultural chemicals.
The beneficial effects of the invention are as follows：The present invention has the principle of high sensitivity and high selectivity using mass detector,
Disposable 124 kinds of farm chemical ingredients during fast qualitative, accurate quantitative analysis are dark brownish green simultaneously, solve it is dark brownish green in 124 kinds of agricultural chemicals it is residual
Stay the blank of detection liquid chromatography-mass spectrometry.
The invention is advantageous to the legitimacy of dark brownish green Detecting Pesticide, accuracy, can be dark brownish green Pesticides maximum residue limit
Formulate and substantial amounts of basic data is provided, gradual perfection China fills up domestic dark brownish green to quality and safety of tea Risk Monitoring foundation
The blank of quantitative, the accurate qualitative and quantitative detection liquid matter method of fast qualitative, is examined suitable for tealeaves raw material quality security guarantee
Survey.
The present invention is prohibited with country prohibits the use of agricultural chemicals, national standard 2763- using on agricultural chemicals, national explicit order tea tree
2016 grade foundations, select 124 kinds of pesticide varieties be research object, have respectively 73 kinds of insecticide, 31 kinds of bactericide, 6 kinds of acaricide,
14 kinds of herbicide；35 kinds of organophosphorus insecticides, 20 kinds of carbamate insecticides, 6 kinds of nicotinic insecticide；Include state of China
Mark GB2763-2016《Pesticide maximum residue limit is limited the quantity》In to Pesticide Residues in Tea finite quantity requirement agricultural chemicals in weeding
Ammonium phosphine and glyphosate other 46 agricultural chemicals.Be advantageous to improve the detection foundation of Pesticide Residues in Tea harm, strengthen to from tea place source
Supervision, detection of the head to teacup consumption, improve quality and safety of tea, ensure our province Tea Industry sustainable development.
Brief description of the drawings
Fig. 1 is that 124 kinds of concentration are 0.1ug/mL pesticide standard sample SRM chromatograms；
Fig. 2 is that dark brownish green samples add (0.1mg/kg) SRM chromatograms.
Embodiment
Embodiment 1：
First, reagent and instrument
The QTRAP of LC-20AD XR-AB 4000 (ABI-4000Q MS, American AB I company) (liquid chromatograies-mass spectrum connection
With)；Acetonitrile, methanol (chromatogram, import reagent)；124 kinds of formic acid, ammonium acetate, acetic acid (chromatographically pure, import reagent) agricultural chemicals standard specimens：
Trihydroxy carbofuran, orthene, imidacloprid, Acetochlor, Aldicarb, Aldicarb wind, Aldicarb Asia phoenix, ametryn, green bristlegrass are gone
Tianjin, AVM, azinphos-methyl, close bacterium ester, M 9834, Bian adenine phosphate, bensulfuron-methyl, Biphenthrin, bitertanol, thiazine
Ketone, first a kind of apple prestige, carbendazim, carbofuran, carbosulfan, Rynaxypyr, d ichlorbenzuron, chlorfluazuron, chlorpropham, poison with poison
Tick, chlorpyrifos-methyl, chlorsulfuron, clothianidin, Resistox, cyprodinil, cyromazine, demeton, diafenthiuron, diazinon, enemy enemy
Fear, Difenoconazole, diflubenzuron, Rogor, alkene acyl agate beautiful jade, olefin conversion, diphenylamines, emamectin-benzoate, fluorine ring
Azoles, fenvalerate, phonamiphos, etoxazole, fenamiphos, Fenarimol, fenazaquin, RH-7592, Folithion, Bassa, azoles
Mite ester, Entex, flufenoxuron, Flusilazole, hexaconazole, Hexythiazox, Acetamiprid, fly worm prestige, isazofos, isocarbophos, Mobucin,
Rice Wen Ling, ivermectin, butachlor, malathion, methiocarb, first frost phosphorus, acephatemet, methidathion, Methomyl, MTMC, first
Huang Long, nitrile bacterium azoles, Nitenpyram, omethoate, paclobutrazol, parathion, penconazole, phenthoate dimephenthoate cidial, thimet, phosmet, sulphur ring
Phosphorus, methyl ring phosphorus, Phosalone, phoxim, thimet wind, thimet Asia wind, Aphox, pretilachlor, Prochloraz, Profenofos,
The close bacterium ester of prometryn, Propamocarb, propargite, propiconazole, second pretilachlor, arprocarb, pyrrole ketone, pyrazoles, pyridaben, phonetic mould ammonium,
Quinalphos, rimsulfuron, Simanex, sulfotep, fluorine amine cyanogen polyester, Tebuconazole, terbufos, probenazole, thiacloprid, thiophene worm
Piperazine, thiophanate-methyl, Tolfenpyrad, triazolone, Triadimenol, tri-allate, Hostathion, metrifonate, tricyclazole, zoxamide agricultural
Environment supervision and inspection center of portion (Tianjin)；
2nd, detection method
A, sample pre-treatments：The dark brownish green fresh leaf powder of 10g is weighed in centrifuge tube, it is molten then to add 20mL1% acetate acetonitriles
Liquid, NaCl is added after high-speed homogenization extraction, after fully shaking mixes, centrifugation layering, take supernatant standby；
B, examination with computer liquid is handled：Fast qualitative quantitative detecting analysis, foregoing constant volume liquid 1.0mL is taken, with 1.0 mL acetonitriles
Determined after dilution using liquid chromatograph mass spectrography.Accurate qualitative and quantitative detection analysis, adds about 2cm high nothings in nh 2 column
Aqueous sodium persulfate, 5mL acetonitrile-methylbenzenes (3 are first used before being loaded:1) solution prewashing post, when liquid level reaches the top of sodium sulphate, rapidly
Aforementioned sample extract solution 4mL is drawn to be transferred on decontaminating column, then with 25mL acetonitrile-methylbenzenes (3:1) solution elution agricultural chemicals, all filters
Liquid is collected in 100mL pear shape bottles, and spin concentration is to about 0.5mL in 45 DEG C of water-baths, the nitrogen drying at 35 DEG C, and 2mL acetonitriles-
Aqueous dissolution residue, after 0.2 μm of filtering with microporous membrane, determined for liquid chromatography tandom mass spectrometry determination.
C, mass spectroscopy：Measure liquid in step B is subjected to qualitative and quantitative analysis with liquid chromatograph-mass spectrometer.
The condition of the liquid chromatography-mass spectrography qualitative and quantitative analysis is：The condition of liquid chromatograph-mass spectrometer analysis
For：Chromatographic column：Phenomenex Luna C18 (2) 100A, 3 μm, 150mm × 2mm internal diameters；Mobile phase and condition of gradient elution
See attached list 1；Column temperature：40℃；Sample size：2μL；Ionize source module：ESI+；Atomization gas：Nitrogen；Atomization gas pressure：60psi；It is auxiliary
Help gas：50psi gas curtain gas：25psi, ion spray voltage：5500V；Dry temperature degree：650℃；Dry gas stream speed：10L/
min；Fragmentation voltage is referring to table 1 in monitoring ion pair, collision gas energy and source.Selective ion multiple-reaction monitoring pattern scanning
(SRM), the data acquisition of detector gathers for split time window.The Mass Spectrometry Conditions and retention time of 124 kinds of agricultural chemicals are shown in Table 1,
Standard specimen chromatogram is as shown in Figure 1.
The conditions such as table 1 124 kinds of agricultural chemicals retention times, Q1, Q3, collision energies
3rd, method validation
1st, the practicality of method
Detecting Pesticide analysis is carried out using the above method is dark brownish green to tea place, market is dark brownish green, Detection results can reach
Detection demand, there is preferable practicality and generalization.
2nd, the linear measure of method
First configuration concentration is 100.0 μ g/mL pestsides synthesis standard liquids, then to be configured to gradient concentration standard molten for dilution step by step
Liquid.Standard liquid mass concentration is 0.020 μ g/mL, 0.050 μ g/mL, 0.20 μ g/mL, 0.50 μ g/mL, upper machine examination after mixing
Survey.Using agricultural chemicals peak area as ordinate, pesticide quality concentration is abscissa, and the coefficient R of each agricultural chemicals is calculated2(see
Table 2).As a result the coefficient R of each agricultural chemicals is shown2Not less than 0.983, mass concentration has in the range of 0.02~0.50 μ g/mL
There is good linear relationship.
As a result show, coefficient R2More than 0.983,124 kinds of residues of pesticides are in mass concentration 0.02~0.50
In μ g/mL content ranges, mass detector response and the concentration of corresponding 124 kinds of residues of pesticides are in good linear relationship.Simultaneously
Also showing mass spectrum has preferable sensitivity.
3rd, repeatability and determination of recovery rates
Experiment is added by adding agricultural chemicals in dark brownish green sample to evaluate method, respectively plus low concentration
(0.10mg/kg) and the concentration gradient of high concentration (0.50mg/kg) two addition recovery experiment.
10.0g sample is first accurately weighed, it is 0.10mg/kg and 0.50mg/kg agricultural chemicals standard specimens to add every kind of pesticide concentration
Solution, tested and analyzed as stated above, the results are shown in Table 2.From Table 2, it can be seen that method has reached strict quantitative standard
True property, precision and repeatability.
Method coefficient correlation (the R of table 22), quantitative limit, precision and the rate of recovery
Note：Above-mentioned average recovery rate measures average values, relative standard deviation (RSD=6) for 6 times, and concentration unit is：ug/
kg
5th, mass spectrometry is quantitative
Sample measure is carried out under the same conditions, if the retention time of the chromatographic peak of detection is consistent with standard items,
And in the sample mass spectrum after background correction, selected ion occurs, and selected abundance of ions ratio and standard
The abundance of ions of product is than meeting：Relative abundance ＞ 50%, it is allowed to ± 20% deviation；Relative abundance ＞ 20%~50%, it is allowed to ±
25% deviation；Relative abundance ＞ 10%~20%, it is allowed to ± 30% deviation；Relative abundance≤10%, it is allowed to ± 50% deviation, then
It can determine whether this agricultural chemicals in sample be present.Analyzed using peak area mass concentration standard curve quantified by external standard method.
6th, the measure of actual sample
Detecting Pesticide is carried out to 5 dark brownish green samples of collection using the present invention, every part of sample is parallel to repeat detection 3
It is secondary, relative standard deviation (RSD, n=3) is calculated to detection value, the results are shown in Table 3.As a result illustrate that actual sample detects relative standard
Deviation (RSD, n=3) is 3.2-5.2%, and method is applicable 124 kinds of pesticide residue analysis detections in dark brownish green sample.
The pesticide sample measurement result of table 3
| Farm chemical ingredients | sample1 | sample2 | sample3 | sample4 | sample5 |
| Biphenthrin | 1.2 | 1.3 | - | - | |
| Fenvalerate | 0.21 | - | - | - | |
| Acetamiprid | - | - | 0.86 | 0.16 | - |
| Imidacloprid | - | - | - | - | 0.052 |
Note：To measure average value three times, concentration unit is above-mentioned testing result：mg/kg
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to is assert
The specific implementation of the present invention is confined to these explanations.For general technical staff of the technical field of the invention,
On the premise of not departing from present inventive concept, some simple deduction or replace can also be made, should all be considered as belonging to the present invention's
Protection domain.
The mobile phase of subordinate list 1 and gradient elution
Claims (4)
1. it is a kind of at the same determine it is dark brownish green in 124 kinds of residues of pesticides detection method, it is characterised in that：Comprise the following steps：
A, sample pre-treatments：Dark brownish green fresh leaf powder is weighed in centrifuge tube, then adds 1% acetate acetonitrile solution, high-speed homogenization
NaCl is added after extraction, after fully shaking mixes, centrifugation layering, takes supernatant standby；
B, examination with computer liquid is handled：Fast qualitative quantitative detecting analysis, extract solution in A is taken, with utilizing liquid phase color after dilution in acetonitrile
Spectrum-MS；Accurate qualitative and quantitative detection analysis, high anhydrous sodium sulfate is added in nh 2 column, second is first used before sample-adding
Nitrile-toluene solution prewashing post, when liquid level reaches the top of sodium sulphate, rapid aforementioned sample extract solution of drawing is transferred to decontaminating column
On, then with acetonitrile-methylbenzene solution agricultural chemicals is eluted, combine in all filtrates, spin concentration is near dry in 45 DEG C of water-baths, in 30-35
Nitrogen dries up at DEG C, acetonitrile-aqueous solution dissolved residue, after 0.2 μm of filtering with microporous membrane, is surveyed for liquid chromatography-tandem mass spectrometry
It is fixed；
C, mass spectroscopy：Measure liquid in step B is subjected to accurate qualitative and quantitative analysis with liquid chromatograph-mass spectrometer.
2. it is according to claim 1 at the same determine it is dark brownish green in 124 kinds of residues of pesticides method analysis method, its feature exists
In：After dark brownish green sample is extracted with 1% acetate acetonitrile high-speed homogenization, fast qualitative quantitative analysis after extract solution dilution in acetonitrile；With
After SPE amino column purification, liquid chromatography mass instrument accurate quantitative analysis qualitative analysis is utilized.
3. it is according to claim 1 at the same determine it is dark brownish green in 124 kinds of residues of pesticides method analysis method, its feature exists
In：Liquid chromatograph-mass spectrometer analysis condition be：Chromatographic column：Phenomenex Luna C18(2)100A,3μm,
150mm × 2mm internal diameters；Mobile phase and condition of gradient elution see attached list 1；Column temperature：40℃；Sample size：2μL；Ionize source module：
ESI+；Atomization gas：Nitrogen；Atomization gas pressure：60psi；Aid in gas：50psi gas curtain gas：25psi, ion spray voltage：
5500V；Dry temperature degree：650℃；Dry gas stream speed：10L/min；Selective ion multiple-reaction monitoring pattern scans (SRM),
The data acquisition of detector gathers for split time window.
4. it is according to claim 1 at the same determine it is dark brownish green in 124 kinds of farm chemical ingredients method, it is characterised in that：Described 124
Kind agricultural chemicals, wherein 73 kinds of insecticide, 31 kinds of bactericide, 6 kinds of acaricide, 14 kinds of herbicide；35 kinds of organophosphorus insecticides, amino
20 kinds of formate ester insecticide, 6 kinds of nicotinic insecticide；Include China national standard GB2763-2016《The maximum residual of Pesticide
Amount limitation》In in the agricultural chemicals of Pesticide Residues in Tea finite quantity requirement except glufosinate-ammonium and glyphosate other 46 agricultural chemicals.
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| CN109738564A (en) * | 2019-01-23 | 2019-05-10 | 中国农业科学院饲料研究所 | The method of 19 kinds of pesticide residues in liquid chromatography-tandem mass spectrometry clover |
| CN109932461A (en) * | 2019-01-31 | 2019-06-25 | 刘军虎 | A kind of pesticide residue method in QuEChERS pretreatment technology combination gas Chromatographic Determination tealeaves |
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| CN115128179A (en) * | 2022-05-30 | 2022-09-30 | 天津市农业生态环境监测与农产品质量检测中心 | Method for simultaneously determining residue of prometryn, abamectin and ivermectin in non-standard medicines for aquaculture and application |
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| YALIN CAO 等: "A novel method based on MSPD for simultaneous determination of 16 pesticide residues in tea by LC-MS/MS", 《JOURNAL OF CHROMATOGRAPHY B》 * |
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| CN109738564A (en) * | 2019-01-23 | 2019-05-10 | 中国农业科学院饲料研究所 | The method of 19 kinds of pesticide residues in liquid chromatography-tandem mass spectrometry clover |
| CN109932461A (en) * | 2019-01-31 | 2019-06-25 | 刘军虎 | A kind of pesticide residue method in QuEChERS pretreatment technology combination gas Chromatographic Determination tealeaves |
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| CN113009063A (en) * | 2021-02-22 | 2021-06-22 | 山东国投鸿基检测技术股份有限公司 | Method for rapidly detecting pesticide residues in traditional Chinese medicinal materials and decoction pieces thereof |
| CN115128179A (en) * | 2022-05-30 | 2022-09-30 | 天津市农业生态环境监测与农产品质量检测中心 | Method for simultaneously determining residue of prometryn, abamectin and ivermectin in non-standard medicines for aquaculture and application |
| CN115128179B (en) * | 2022-05-30 | 2023-09-05 | 天津市农业生态环境监测与农产品质量检测中心 | Method for simultaneously determining prometryn, abamectin and ivermectin residues in non-standard medicines for aquaculture and application thereof |
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