CN108287201A - The detection method of bromine cyanogen insect amide and metabolin J9Z38 in pork - Google Patents
The detection method of bromine cyanogen insect amide and metabolin J9Z38 in pork Download PDFInfo
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- G—PHYSICS
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Abstract
The present invention provides a kind of detection method of bromine cyanogen insect amide and metabolin J9Z38 in pork, including：Extraction purifies, and measures, is added recovery test, obtains bromine cyanogen insect amide and the TIANZHU XINGNAO Capsul and relative standard deviation of J9Z38（RSDs）；Detect the minimum detectable activity of bromine cyanogen insect amide and J9Z38；Obtain the minimal detectable concentration of bromine cyanogen insect amide, J9Z38 in pork.The present invention establishes the analyzing detecting method of bromine cyanogen insect amide and its metabolin J9Z38 in pork；It is extracted using acetonitrile, n-hexane removes the impurity such as fat, protein in pork, purification separation effect is good, the pretreatment process of this method is relatively easy, the rate of recovery is high, and reproducible, purification separation effect is good, and minimal detectable concentration is relatively low, is suitable for the analysis detection of bromine cyanogen insect amide and metabolin J9Z38 in pork.
Description
Technical field
The present invention relates to the detection method of Pesticides Testing more particularly to bromine cyanogen insect amide and metabolin J9Z38 in pork.
Background technology
Bromine cyanogen insect amide (Cyantraniliprole) is another Novel ortho of E.I.Du Pont Company after Rynaxypyr
Aminobenzamide insecticides.It has efficiently, low toxicity, mechanism of action it is novel, to non-target organism safety, to existing desinsection
The features such as agent no interactions resistance.Bromine cyanogen insect amide especially has excellent preventive effect to sucking pest, has wide answer
With foreground, cause the extensive concern of people.
The chemical name of bromine cyanogen insect amide is the bromo- 1- of 3- (3- chloro-2-pyridyls)-N- { 4- cyano -2- methyl -6- [(first
Base amino) carbonyl] phenyl } -1H- pyrazoles -5- formamides；Chemical structural formula is
Molecular formula C19H14BrClN6O2, molecular weight 473.7.Bromine cyanogen insect amide is white powder, 168~173 DEG C of fusing point,
Relative density (20 DEG C) 1.387g/cm3, not volatile.Solubility (20 DEG C) 0~20 mg/L in water, the dissolving in other solvents
Degree, 2.383g/L (methanol), 5.965g/L (acetone), 0.576g/L (toluene), 5.338g/L (dichloromethane), 1.728g/L
(acetonitrile).
Exemplary metabolites object of the bromine cyanogen insect amide in plant and animal body is J9Z38, and structural formula is：
Molecular formula is C19H12BrClN6O, molecular weight 457.
Currently, the report in relation to bromine cyanogen insect amide detection method has：Bromine cyanogen insect amide cereal (rice, wheat, corn),
Plant sources agricultural product, the soil such as vegetables (cucumber, tomato, pakchoi, capsicum, cowpea, romaine lettuce), fruit (apple, grape, citrus)
With the detection method in water.But it is had not been reported about the detection method of bromine cyanogen insect amide and metabolin J9Z38 in pork.
Invention content
Technical problem to be solved by the invention is to provide a kind of inspection of bromine cyanogen insect amide and metabolin J9Z38 in pork
Survey method can be detected bromine cyanogen insect amide in pork and metabolin J9Z38, meet in pesticide residue analysis to accurate
The requirement of degree, precision and sensitivity.
Technical solution is used by the present invention solves above-mentioned technical problem：A kind of bromine cyanogen insect amide and metabolin J9Z38
Detection method in pork, includes the following steps：
(1) it extracts：Pork sample 2g is weighed, is placed in 50mL centrifuge tubes, 0.1% formic acid waters of 2mL and 20mL extractions is added
Liquid is homogenized 30s under the conditions of 6000rpm, and 1g anhydrous sodium acetates and 2g anhydrous magnesium sulfates is added, is aggressively shaken 30s,
5min is centrifuged under the conditions of 4000rpm；
(2) it purifies：It pipettes extracting solution 10mL in centrifuge tube to be placed in separatory funnel, 30mL scavenging solutions is added for the first time, it is acute
Strong shake 1min stands 20min, after liquid layered in separatory funnel, discards lower layer's scavenging solution, adds for second in separatory funnel
Enter 30mL scavenging solutions, be aggressively shaken 1min, stands 20min and discard lower layer's scavenging solution after liquid layered in separatory funnel, receive
Collect the extracting solution in separatory funnel in boiling flask, concentrates and do under the conditions of 40 DEG C, be settled to 5mL, crossing 0.22 μm has eedle
Formula filter, it is to be determined；
(3) it measures：Preparation 0.005,0.01,0.05,0.1,0.2,0.5, the bromine cyanogen insect amide of 1.0mg/L and J9Z38 marks
Quasi- solution, 1 μ L of sample introduction, obtain the response of UPLC-MS/MS respectively, and it is molten to draw bromine cyanogen insect amide standard with concentration-peak area
Liquid curve and J9Z38 standard solution curves；
(4) when setting bromine cyanogen insect amide adds a concentration of 0.02,0.1 and 10.0mg/kg in pork, it is added recycling
Rate is tested, and the TIANZHU XINGNAO Capsul and relative standard deviation (RSDs) of bromine cyanogen insect amide and J9Z38 are respectively obtained；
(5) minimum detectable activity of ultra performance liquid chromatography tandem mass spectrometer detection bromine cyanogen insect amide and J9Z38 is used；
(6) response condition according to bromine cyanogen insect amide and J9Z38 on ultra performance liquid chromatography tandem mass spectrometer and pig
The sample that bromine cyanogen insect amide and J9Z38 are added by minimum addition concentration in meat response on instrument is all higher than 3 times of letters of instrument
Number noise ratio, obtains the minimal detectable concentration of bromine cyanogen insect amide, J9Z38 in pork.
Extracting solution is acetonitrile homogenate.
Scavenging solution is n-hexane liquid.
Ultra performance liquid chromatography condition is：
Chromatographic column：Waters acquityBEH C18 (1.7 μm, 2.1 × 100mm)；
Mobile phase：Aqueous formic acid=80/20 of acetonitrile/0.1%；
Flow velocity：0.2mL/min；
Column temperature：40℃；
Sample size：1μL；
Mass Spectrometry Conditions are：
Ion source：ESI+；
Quantitative model：MRM patterns；
Capillary voltage：4.0KV；
Atomization gas flow：3.0L/min；
Heat throughput：10.0L/min；
Interface temperature：300℃；
DL temperature：250℃；
Heat Block temperature：400℃；
Dry gas stream amount：10L/min；
Bromine cyanogen insect amide quota ion pair：475.10>286.00, qualitative ion pair：475.10>444.10；
J9Z38 quota ion pairs：456.80>188.00；Qualitative ion：456.80>299.00.
The beneficial effects of the invention are as follows：The present invention establishes the analysis of bromine cyanogen insect amide and its metabolin J9Z38 in pork
Detection method；It is homogenized and is extracted using acetonitrile, the distribution of n-hexane liquid liquid removes the impurity such as fat, protein, purification separation in pork
Effect is good (core of invention), and pretreatment process of the invention is relatively easy, and the rate of recovery is high, reproducible, purification separation effect
It is good, and minimal detectable concentration is relatively low, is suitable for the analysis detection of bromine cyanogen insect amide and metabolin J9Z38 in pork.
Description of the drawings
Fig. 1 is bromine cyanogen insect amide and the TIANZHU XINGNAO Capsul and relative standard deviation of J9Z38.
Fig. 2 is the canonical plotting of bromine cyanogen insect amide.
Fig. 3 is the canonical plotting of J9Z38.
Fig. 4 is bromine cyanogen insect amide (0.1mg/L), J9Z38 (0.1mg/L) standard solution chromatogram.
Specific implementation mode
The invention discloses a kind of detection method of bromine cyanogen insect amide and metabolin J9Z38 in pork, this method is adopted
The key instrument and chemical reagent used have：
Ultra performance liquid chromatography tandem mass spectrometer UPLC-MS/MS (Ultra Performance Liquid Chromatography instrument model LC-30AD, mass spectrum
Instrument model LCMS-8050, Shimadzu Corporation),
SPS 402F type electronic balances：(Mettler-Toledo (Changzhou) Measurement Technology Co., Ltd.),
IKA T18 types disperser (the German laboratories IKA),
The desk-top Bradytelic centrifugation of the large capacity machine of TD5A-WS types (Jin Nan instrument manufacturings Co., Ltd),
R-201 types rotary evaporator (Shanghai Shen Sheng Bioisystech Co., Ltd),
HH-4 types thermostat water bath (Jiangnan instrument plant of Community of Jin Tan County city),
SHZ-D (III) type circulating water type vacuum pump (Yuhua Instrument Co., Ltd., Gongyi City),
II A types oscillators of TYZD- (Tian Yi Electron equipment Co., Ltd of Jiangyan City),
Methanol (analyzing pure 500mL, Tianjin great Mao chemical reagent factories),
Ethyl acetate (analyzing pure 500mL, Tianjin great Mao chemical reagent factories),
Acetonitrile (analyzing pure 500mL, Shanghai Ling Feng chemical reagent Co., Ltd),
Anhydrous sodium acetate (analyzing pure 500g, chemistry materials factory of Wenzhou City),
Anhydrous magnesium sulfate (analyzing pure 500g, Tianjin good fortune morning chemical reagent factory),
N-hexane (analyzing pure 500mL, Sinopharm Chemical Reagent Co., Ltd.),
Cleanert MAS-Q purification pipes (2mL, PSA 50mg, C1850mg, PC 50mg, MgSO4150 mg, model
MS-9PP0250, Tianjin Bonaaijieer Technology Co., Ltd),
Cleanert NANO CARB purification pipes (150mg/1mL, model IC-NN1510-S, Tianjin Beaune Ai Jieerke
Skill Co., Ltd),
Oasis HLB 3cc pillars (60mg/3mL, model WAT094226, Waters company),
Cleanert NH2- SPE pillars (500mg/6mL, model NH5006, the limited public affairs of Tianjin Beaune Ai Jieer science and technology
Department),
Acetonitrile (chromatographically pure 4L, Moke Stock Limited Partnership),
Formic acid (chromatographically pure 500mL, U.S. ROE Scientific Inc),
Organic pin type filter (0.22 μm, model TQP-61322, Tian Yuan scientific ＆ technical corporation),
Syringe (2mL, Changzhou Yue Kang medical equipments Co., Ltd).
Wherein, the condition of instrument is：
Ultra performance liquid chromatography condition：
Chromatographic column：Waters acquityBEH C18 (1.7 μm, 2.1 × 100mm)；
Mobile phase：Aqueous formic acid=80/20 of acetonitrile/0.1%；
Flow velocity：0.2mL/min；
Column temperature：40℃；
Sample size：1μL.
Mass Spectrometry Conditions：
Ion source：ESI+；
Quantitative model：MRM patterns；
Capillary voltage：4.0KV；
Atomization gas flow：3.0L/min；
Heat throughput：10.0L/min；
Interface temperature：300℃；
DL temperature：250℃；
Heat Block temperature：400℃；
Dry gas stream amount：10L/min；
Bromine cyanogen insect amide quota ion pair：475.10>286.00, qualitative ion pair：475.10>444.10；
J9Z38 quota ion pairs：456.80>188.00；Qualitative ion：456.80>299.00.
The specific detection operation of the present invention is as follows：
Extraction：Sample 2g (being accurate to 0.01g) is weighed to be placed in 50mL centrifuge tubes, be added 0.1% formic acid waters of 2mL and
20mL analyzes pure acetonitrile, and (IKA T18 types disperser) 30s is homogenized under the conditions of 6000rpm.Be added 1g anhydrous sodium acetates and 2g without
Water magnesium sulfate is aggressively shaken 30s.(the desk-top Bradytelic centrifugation of the large capacity machine of TD5A-WS types) 5min is centrifuged under the conditions of 4000rpm.
Methanol mechanical shaking extraction, ethyl acetate mechanical shaking extraction, acetonitrile mechanical shaking extraction, acetonitrile are homogenized can be as the present invention's
The recovery rate point of extracting solution, but the extraction efficiency of 4 kinds of extracting solutions difference, methanol mechanical shaking extraction bromine cyanogen insect amide and J9Z38
Not Wei 38% and 46%, recovery rate does not reach requirement.The recovery rate of ethyl acetate mechanical shaking extraction bromine cyanogen insect amide and J9Z38 are distinguished
For 72% and 82%, recovery rate can reach requirement.The recovery rate of acetonitrile mechanical shaking extraction bromine cyanogen insect amide and J9Z38 is respectively
71% and 85%, recovery rate can reach requirement.The recovery rate of acetonitrile homogenate extraction bromine cyanogen insect amide and J9Z38 are 82% He
89%, recovery rate can reach requirement.Ethyl acetate mechanical shaking extraction, acetonitrile mechanical shaking extraction and acetonitrile homogenate 3 kinds of conditions of extraction, bromine
Cyanogen insect amide and J9Z38 recovery rates can reach requirement, consider the factors such as recovery rate, extraction time, and acetonitrile homogenate carries
Optimal extraction conditions are taken as, accordingly, it is determined that extraction side of the acetonitrile homogenate extraction as bromine cyanogen insect amide and J9Z38 in pork
Method.
Purification：It accurately pipettes acetonitrile 10mL in centrifuge tube to be placed in separatory funnel, 30mL n-hexanes is added for the first time, it is acute
Strong shake 1min stands 20min.After liquid layered in separatory funnel, lower layer's n-hexane is discarded.Add for second in separatory funnel
Enter 30mL n-hexanes, be aggressively shaken 1min, stands 20min.After liquid layered in separatory funnel, lower layer's n-hexane is discarded, is received
Collect the acetonitrile in separatory funnel in boiling flask, is concentrated under the conditions of 40 DEG C and do (R-201 types rotary evaporator), use chromatographically pure
Acetonitrile is settled to 5mL, crosses 0.22 μm of organic pin type filter (model TQP-61322), to be determined.
In selected scavenging solution, NH is compared2- SPE pillars, HLB pillars, Cleanert MAS-Q purification pipes (2mL, C18
50mg, PSA 50mg, PC 50mg, MgSO4150mg), IC-NN1510-S types Cleanert NANO CARB purifications pipe
Shadow of the 5 kinds of purification conditions such as (150mg/1mL), n-hexane liquid liquid distribution to bromine cyanogen insect amide in pork and J9Z38 clean-up effects
It rings.The result shows that by NH5006 type Cleanert NH2- SPE pillars (500mg/6mL) purification after, bromine cyanogen insect amide and
The rate of recovery of J9Z38 is respectively 53% and 66%, and the rate of recovery does not reach requirement.It is small by WAT094226 type Oasis HLB 3cc
After column (60mg/3mL) purification, the rate of recovery of bromine cyanogen insect amide and J9Z38 are respectively 47% and 70%, and the rate of recovery, which is not achieved, to be wanted
It asks.By MS-9PP0250 type Cleanert MAS-Q purification pipes (2mL, PSA 50mg, C18 50mg, PC 50mg, MgSO4
After 150mg) purifying, the rate of recovery of bromine cyanogen insect amide and J9Z38 are respectively 72% and 79%, and the rate of recovery can reach requirement.Through
After crossing IC-NN1510-S type Cleanert NANO CARB purification pipe (150mg/1mL) purification, bromine cyanogen insect amide and J9Z38's
The rate of recovery is respectively 67% and 74%, and the rate of recovery does not reach requirement.By n-hexane liquid liquid distribution purification after, bromine cyanogen insect amide and
The rate of recovery of J9Z38 is respectively 105% and 91%, and the rate of recovery can reach requirement；And liquid is colourless after purifying, and goes to clean
The effect of matter is fine, considers the rate of recovery, the removal factors such as impurity effect and operating process, n-hexane liquid liquid is assigned as optimal
Purification condition, accordingly, it is determined that n-hexane liquid liquid distributes the purification method as bromine cyanogen insect amide and J9Z38 in pork.
Prepare 0.005 with trifluoroacetic acid aqueous solution, 0.01,0.05,0.1,0.2,0.5, the bromine cyanogen insect amide of 1.0mg/L and
J9Z38 standard solution, 1 μ L of sample introduction, obtain the response of UPLC-MS/MS respectively, and bromine cyanogen insect amide is drawn with concentration-peak area
Standard solution curve is shown in that Fig. 2, regression equation are y=9835407.97x+24039.88 (R2=0.9999)；J9Z38 standards
Solution curve is shown in that Fig. 3, regression equation are y=1601429.98x+2065.58 (R2=1.0000).
According to the response feelings of bromine cyanogen insect amide, J9Z38 on ultra performance liquid chromatography tandem mass spectrometer (UPLC-MS/MS)
Condition, bromine cyanogen insect amide, J9Z38 set 3 grades of addition concentration (0.02,0.1 and 10mg/kg), every grade of addition in pork sample
Concentration sets 5 repetitions.
By said extracted, purification and determination step, it is added recovery test.Obtain bromine cyanogen worm acyl in pork sample
Amine, the TIANZHU XINGNAO Capsul of J9Z38 and relative standard deviation (RSDs), are shown in Fig. 1.
As shown in Figure 1, it is average to recycle when bromine cyanogen insect amide adds a concentration of 0.02,0.1 and 10.0mg/kg in pork
Rate is respectively 107%, 102% and 96%, and relative standard deviation is respectively 3.7%, 3.5% and 3.6%.J9Z38 is in pork
When adding a concentration of 0.02,0.1 and 10.0mg/kg, average recovery rate is respectively 93%, 88% and 93%, relative standard deviation
Respectively 3.1%, 4.0% and 5.3%.
Ultra performance liquid chromatography tandem mass spectrometer (UPLC-MS/MS) is equal to the minimum detectable activity of bromine cyanogen insect amide, J9Z38
For 5 × 10-12g.
According in response condition on ultra performance liquid chromatography tandem mass spectrometer of bromine cyanogen insect amide, J9Z38 and pork
The sample of the minimum addition concentration 0.02mg/kg of bromine cyanogen insect amide, J9Z38 response on instrument is all higher than 3 times of signals of instrument
Noise ratio obtains：The minimal detectable concentration of bromine cyanogen insect amide, J9Z38 in pork is 0.02mg/kg.
The present invention establishes the analyzing detecting method of bromine cyanogen insect amide and its metabolin J9Z38 in pork, this method bromine cyanogen
Insect amide and metabolin J9Z38 are in good linear relationship in 0.005~1.0mg/L concentration ranges；Bromine cyanogen insect amide is in pig
Average recovery rate is 96%~101% in meat, and relative standard deviation is 5.0%~13.8%.J9Z38 is averagely returned in pork
Yield is 93%~97%, and relative standard deviation is 2.9%~11.0%.The minimum inspection of bromine cyanogen insect amide, J9Z38 in pork
It is 0.02mg/kg to survey concentration, and the present invention is easy to operate, accurately and reliably, can meet the requirement of pesticide residue analysis, and can be used for
The quick detection of a large amount of samples.
Claims (5)
1. the detection method of bromine cyanogen insect amide and metabolin J9Z38 in pork, characterized in that include the following steps：
(1) it extracts：Pork sample 2g is weighed, is placed in 50mL centrifuge tubes, 0.1% formic acid waters of 2mL and 20mL extracting solutions is added,
It is homogenized 30s under the conditions of 6000rpm, 1g anhydrous sodium acetates and 2g anhydrous magnesium sulfates is added, 30s is aggressively shaken, in 4000rpm items
5min is centrifuged under part；
(2) it purifies：It pipettes extracting solution 10mL in centrifuge tube to be placed in separatory funnel, 30mL scavenging solutions is added for the first time, acutely shake
Dynamic 1min, stands 20min, after liquid layered in separatory funnel, discards lower layer's scavenging solution, is added for second in separatory funnel
30mL scavenging solutions are aggressively shaken 1min, stand 20min and discard lower layer's scavenging solution after liquid layered in separatory funnel, collect
Extracting solution in separatory funnel concentrates under the conditions of 40 DEG C and does, be settled to 5mL, cross 0.22 μm of organic pin type in boiling flask
Filter, it is to be determined；
(3) it measures：It is molten to prepare 0.005,0.01,0.05,0.1,0.2,0.5, the bromine cyanogen insect amide of 1.0mg/L and J9Z38 standards
Liquid, 1 μ L of sample introduction, obtain the response of UPLC-MS/MS respectively, and it is bent to draw bromine cyanogen insect amide standard solution with concentration-peak area
Line；
(4) it sets bromine cyanogen insect amide and metabolin J9Z38 adds a concentration of 0.01,0.2 and 8.0mg/kg in pork, added
Add recovery test, respectively obtains the TIANZHU XINGNAO Capsul and relative standard deviation (RSDs) of bromine cyanogen insect amide and J9Z38；
(5) minimum detectable activity of ultra performance liquid chromatography tandem mass spectrometer detection bromine cyanogen insect amide and J9Z38 is used；
(6) in the response condition according to bromine cyanogen insect amide and J9Z38 on ultra performance liquid chromatography tandem mass spectrometer and pork
3 times of signals that the sample that bromine cyanogen insect amide and J9Z38 are added by minimum addition concentration response on instrument is all higher than instrument are made an uproar
Signal to noise ratio obtains the minimal detectable concentration of bromine cyanogen insect amide, J9Z38 in pork.
2. detection method according to claim 1, characterized in that extracting solution is acetonitrile homogenate.
3. detection method according to claim 1, characterized in that scavenging solution is n-hexane liquid.
4. detection method according to claim 1, characterized in that the chromatographic condition of ultra performance liquid chromatography tandem mass spectrometer
It is：
Chromatographic column：Waters acquityBEH C18 (1.7 μm, 2.1 × 100mm)；
Mobile phase：Aqueous formic acid=80/20 of acetonitrile/0.1%；
Flow velocity：0.2mL/min；
Column temperature：40℃；
Sample size：1μL.
5. detection method according to claim 1, characterized in that the Mass Spectrometry Conditions of ultra performance liquid chromatography tandem mass spectrometer
It is：
Ion source：ESI+；
Quantitative model：MRM patterns；
Capillary voltage：4.0KV；
Atomization gas flow：3.0L/min；
Heat throughput：10.0L/min；
Interface temperature：300℃；
DL temperature：250℃；
Heat Block temperature：400℃；
Dry gas stream amount：10L/min；
Bromine cyanogen insect amide quota ion pair：475.10>286.00, qualitative ion pair：475.10>444.10；J9Z38 quota ions
It is right：456.80>188.00；Qualitative ion：456.80>299.00.
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