CN106093032A - A kind of Fast Determination of Pesticide Residue eliminates false-positive detection method - Google Patents
A kind of Fast Determination of Pesticide Residue eliminates false-positive detection method Download PDFInfo
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- G—PHYSICS
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Abstract
A kind of pesticide residues eliminate false-positive method for quick and belong to field of food safety, are specifically related to a kind of be applied to the method that Rhizoma Zingiberis Recens quickly detects with Bulbus Allii pesticide.A kind of Fast Determination of Pesticide Residue eliminates false-positive detection method, specifically includes following steps: step a, test agent are prepared, step b, sample pre-treatments, and step C, detection judge；This method sample extracting solution, through heat treated, can eliminate the interference of secondary pollutant in Rhizoma Zingiberis Recens and Bulbus Allii；Extracting solution can be by pigment and or the removing of other solid contents, the minimizing interference to testing result through centrifugal treating simultaneously；Additionally, sample processes through rubbing, extract more abundant.
Description
Technical field
A kind of pesticide residues eliminate false-positive method for quick and belong to field of food safety, are specifically related to a kind of application
In the method that Rhizoma Zingiberis Recens and Bulbus Allii pesticide quickly detect.
Background technology
In common pesticides, relatively big to people's toxicity, easily cause poisoning is insecticide, and causes poisoning thing in insecticide
What part was most is Organophosphorus and carbamate pesticides class pesticide, and this two classes pesticide uses frequency higher in actual production, and this is just
Quickly detection to Organophosphorus and carbamate pesticides class pesticide is had higher requirement.At present, conventional organophosphor and amino
Formate ester Pesticides Testing method have thin layer chromatography, gas chromatography, high performance liquid chromatography, supercritical fluid chromatography,
Hexavalent chrome bio-removal, immunoassay, inhibiting AChE etc..
Chromatographic detection precision is the highest, but its detection process is complicated, the detection time is long, vegetable wide in variety, source is wide, and
And the sale of vegetable to keep fresh, short in circulation market residence time, therefore, chromatography was difficult to before vegetable is sold complete
Become detection.And hexavalent chrome bio-removal and immunoassay are because early investment is big, experiment condition is harsh, currently also it is only used in China
Laboratory.Inhibiting AChE is high with accuracy, detection speed is fast, simple to operate, low cost and other advantages obtains extensively
General application, is the method for quick of the Organophosphorus and carbamate pesticides class pesticide that present stage is commonly used, and has become vegetable
The national standard method that middle Organophosphorus and carbamate pesticides class pesticide quickly detects.
But, enzyme inhibition rate method measures some special Determination of Pesticide Residues in Vegetable and there is false positive, and this point is marked in country
The explanation of quasi-GB/T 5009.199 2003 just explicitly points out: " Herba Alii fistulosi, Bulbus Allii, Radix Raphani, Folium Allii tuberosi, Herba Apii graveolentis, Herba Coriandri, Caulis Zizaniae caduciflorae, mushroom and
In Tomato Juice, containing plant secondary substance influential on enzyme, easily produce false positive ", interference detection results, to agricultural product
The supervision of quality safety increases difficulty.
Summary of the invention
The present invention devises a kind of Rhizoma Zingiberis Recens and the method for quick of Bulbus Allii pesticide residues, its object is to solve enzyme level
Rate method detects the false positive issue easily occurred in Rhizoma Zingiberis Recens and Bulbus Allii.
For achieving the above object, the technical solution used in the present invention is:
A kind of Fast Determination of Pesticide Residue eliminates false-positive detection method, specifically includes following steps:
Step a, test agent are prepared
The reagent preparing needs the most respectively is pH8.0 phosphate buffer, developer, substrate and acetylcholinesterase liquid,
Play collocation method as follows:
PH7.0-9.0 phosphate buffer: take 11.5-12.5g dipotassium hydrogen phosphate (K2HPO4) and 3-3.5g potassium dihydrogen phosphate
(KH2PO4), it is dissolved in 1000ml distilled water and just obtains pH7.0-9.0 phosphate buffer；
Developer: take 140-170mg sulfur for dinitrobenzoic acid (DTNB) and 14.8-16.4mg sodium bicarbonate (NaHCO3), use
The above-mentioned phosphate buffer of 17-23ml dissolves, in 2-5 DEG C of Refrigerator store.
Substrate: take 23-27mg acetylthiocholine, adds 2.6-3.3ml distilled water and dissolves, shake up and be placed on 3-6 DEG C of refrigerator
Preserve.
Acetylcholinesterase liquid: according to the activity of enzyme, with buffer solution, shake up and be placed on 2-5 DEG C of Refrigerator store.Wherein
The absorbance change of enzyme liquid 2.5-3.2min should control more than 0.3.
Step b, sample pre-treatments
(1) choose 1,2-1,5g Rhizoma Zingiberis Recens and 1,2-1,5g Bulbus Allii clear water are rinsed well, be careful not to destroy sample surface
Tissue；
(2) Rhizoma Zingiberis Recens handled well through above step 1 is rubbed with Bulbus Allii pulverizer, respectively weigh and after rubbing respectively, obtain Rhizoma Zingiberis Recens
0.8-1.2g Yu 0.8-1,2g Bulbus Allii, add the pH8.0 phosphate buffer that 5ml configures, and fully after vibration, is placed in 90-
Heat treated in 120 DEG C of water-baths, the heat treatment time-division drives row into, and the treatment conditions of Rhizoma Zingiberis Recens are 90-120 DEG C and continue 2-3min, greatly
The treatment conditions of Bulbus Allii are 80-110 DEG C and continue 1-2min；Extracting solution good for heat treatment is placed room temperature 25-28 DEG C preserve；
(3): take step 2 is positioned over room temperature 25-28 DEG C preserve sample, put in centrifuge tube, 5000 rpms from
Scheming persistently rotates 09-1.2 min, the 18-20 DEG C of preservation in addition of the clear liquid after having processed.
Step C, detection judge
(1) blank liquid test
Take test tube and add 2-3ml phosphate buffer, add 0.09-0.12ml acetylcholinesterase liquid, 0.3-0.5ml colour developing
Agent, is positioned over 35-38 DEG C of thermostat water bath and deposits 15 20min after shaking up, add 0.08-0.11ml substrate and shake up, at once
Put people's spectrophotometer to measure at 400-420nm, record the absorbance changing value Δ of reaction 2.5-3.5minΑThe number of 0
Value.
(2) sample liquid test
Take test tube and add the sample liquid handled well through step b3 of 2-3ml, add 0.09-0.12ml acetylcholinesterase liquid,
0.3-0.5ml developer, is positioned over 35-38 DEG C of thermostat water bath and deposits 15 20min, add 0.08-0.11ml after shaking up
Substrate shakes up, and puts people's spectrophotometer at once and measures at 400-420nm, records the absorbance change of reaction 2.5-3.5min
Value ΔΑThe numerical value of t.
(3) judgement is calculated
By step 1,2 record ΔΑ0 and ΔΑThe numerical value of t, calculates enzyme inhibition rate (%) by below equation
Suppression ratio (%)=[ΔΑ0 - ΔΑt]/ΔΑ0] × 100 ... ... ... (1)
(4) qualitatively judge
When the suppression ratio 50% of extracting solution, represent organophosphor or carbamate chemicals for agriculture with the presence of high dose in vegetable,
Sample is positive.
The present invention uses technique scheme, and this method sample extracting solution, through heat treated, can eliminate Rhizoma Zingiberis Recens and big
The interference of secondary pollutant in Bulbus Allii；Simultaneously extracting solution through centrifugal treating can by pigment and or other solid contents remove, reduce to inspection
Survey the interference of result；Additionally, sample processes through rubbing, extract more abundant.
Accompanying drawing explanation
Accompanying drawing explanation
Fig. 1 is Rhizoma Zingiberis Recens of the present invention and the quick overhaul flow chart of Bulbus Allii Pesticide Residues thing.
Detailed description of the invention
Embodiment 1
A kind of Fast Determination of Pesticide Residue eliminates false-positive detection method, specifically includes following steps:
Step a, test agent are prepared
The reagent preparing needs the most respectively is pH8.0 phosphate buffer, developer, substrate and acetylcholinesterase liquid,
Play collocation method as follows:
PH8.0 phosphate buffer: take 11.9g dipotassium hydrogen phosphate (K2HPO4) and 3.2g potassium dihydrogen phosphate (KH2PO4), be dissolved in
1000ml distilled water just obtains pH8.0 phosphate buffer；
Developer: take 160mg sulfur for dinitrobenzoic acid (DTNB) and 15.6mg sodium bicarbonate (NaHCO3), with 17-23ml's
Above-mentioned phosphate buffer dissolves, in 4 DEG C of Refrigerator stores.
Substrate: take 25mg acetylthiocholine, adds 3ml distilled water and dissolves, shake up and be placed on 4 DEG C of Refrigerator stores.
Acetylcholinesterase liquid: according to the activity of enzyme, with buffer solution, shake up and be placed on 2-5 DEG C of Refrigerator store.Wherein
The absorbance change of enzyme liquid 3min should control more than 0.3.
Step b, sample pre-treatments
(1) the 1.3g Rhizoma Zingiberis Recens chosen is rinsed well with 1.3g Bulbus Allii clear water, be careful not to destroy sample surface tissue；
(2) Rhizoma Zingiberis Recens handled well through above step 1 is rubbed with Bulbus Allii pulverizer, respectively weigh and after rubbing respectively, obtain Rhizoma Zingiberis Recens
1g Yu 1g Bulbus Allii, adds the pH8.0 phosphate buffer that 5ml configures, and fully after vibration, is placed in 100 DEG C of water-baths and adds
Heat treatment, the heat treatment time-division drives row into, and the treatment conditions of Rhizoma Zingiberis Recens are 100 DEG C and continue 2-3min, and the treatment conditions of Bulbus Allii are 100 DEG C
Continue 1-2min；Extracting solution good for heat treatment is placed room temperature 25-28 DEG C preserve；
(3): take step 2 is positioned over room temperature 25-28 DEG C preserve sample, put in centrifuge tube, 5000 rpms from
Scheming persistently rotates 0.9-1.2 min, the 18-20 DEG C of preservation in addition of the clear liquid after having processed.
Step C, detection judge
(1) blank liquid test
Take test tube and add 2.5ml phosphate buffer, add 0.1ml acetylcholinesterase liquid, 0.4ml developer, after shaking up
It is positioned over 37 DEG C of thermostat water baths and deposits 18min, add 0.1ml substrate and shake up, put people's spectrophotometer at 412nm at once
Measure, record the absorbance changing value Δ of reaction 3minΑThe numerical value of 0.
(2) sample liquid test
Take test tube and add the sample liquid that 2.5ml handles well through step b3, add 0.1ml acetylcholinesterase liquid, 0.4ml colour developing
Agent, is positioned over 35-38 DEG C of thermostat water bath and deposits 18min after shaking up, add 0.1ml substrate and shake up, and puts people's light splitting light at once
Degree is counted and is measured at 412nm, records the absorbance changing value Δ of reaction 2.5-3.5minΑThe numerical value of t.
(3) judgement is calculated
By step 1,2 record ΔΑ0 and ΔΑThe numerical value of t, calculates enzyme inhibition rate (%) by below equation
Suppression ratio (%)=[ΔΑ0 - ΔΑt]/ΔΑ0]×100
(4) qualitatively judge
When the suppression ratio 50% of extracting solution, represent organophosphor or carbamate chemicals for agriculture with the presence of high dose in vegetable,
Sample is positive.
Embodiment 2
A kind of Fast Determination of Pesticide Residue eliminates false-positive detection method, specifically includes following steps:
Step a, test agent are prepared
The reagent preparing needs the most respectively is pH8.0 phosphate buffer, developer, substrate and acetylcholinesterase liquid,
Play collocation method as follows:
PH8.0 phosphate buffer: take 11.5g dipotassium hydrogen phosphate (K2HPO4) and 3g potassium dihydrogen phosphate (KH2PO4), be dissolved in
1000ml distilled water just obtains pH8.0 phosphate buffer；
Developer: take 140mg sulfur for dinitrobenzoic acid (DTNB) and 14.8mg sodium bicarbonate (NaHCO3), above-mentioned with 17ml
Phosphate buffer dissolves, in 2 DEG C of Refrigerator stores.
Substrate: take 23mg acetylthiocholine, adds 2.6ml distilled water and dissolves, shake up and be placed on 3 DEG C of Refrigerator stores.
Acetylcholinesterase liquid: according to the activity of enzyme, with buffer solution, shake up and be placed on 2 DEG C of Refrigerator stores.Wherein enzyme
The absorbance change of liquid 2.5min should control more than 0.3.
Step b, sample pre-treatments
(1) the 1.2g Rhizoma Zingiberis Recens chosen is rinsed well with .1.2g Bulbus Allii clear water, be careful not to destroy sample surface tissue；
(2) Rhizoma Zingiberis Recens handled well through above step 1 is rubbed with Bulbus Allii pulverizer, respectively weigh and after rubbing respectively, obtain Rhizoma Zingiberis Recens
0.8g Yu 0.8g Bulbus Allii, adds the pH8.0 phosphate buffer that 5ml configures, and fully after vibration, is placed in 90 DEG C of water-baths
Heat treated, the heat treatment time-division drives row into, and the treatment conditions of Rhizoma Zingiberis Recens are 90 DEG C and continue 2min, and the treatment conditions of Bulbus Allii are 80 DEG C and hold
Continuous 1min；Extracting solution good for heat treatment is placed room temperature 25-28 DEG C preserve；
(3): take step 2 is positioned over room temperature 25-28 DEG C preserve sample, put in centrifuge tube, 5000 rpms from
Scheming persistently rotates 0.9-1.2 min, the 18-20 DEG C of preservation in addition of the clear liquid after having processed.
Step C, detection judge
(1) blank liquid test
Take test tube and add 2ml phosphate buffer, add 0.09ml acetylcholinesterase liquid, 0.3ml developer, put after shaking up
It is placed in 35 DEG C of thermostat water baths and deposits 15min, add 0.08ml substrate and shake up, put people's spectrophotometer at 400nm at once
Measure, record the absorbance changing value Δ of reaction 2.5minΑThe numerical value of 0.
(2) sample liquid test
Take test tube and add the sample liquid that 2ml handles well through step b3, add 0.09ml acetylcholinesterase liquid, 0.3ml colour developing
Agent, is positioned over 35-38 DEG C of thermostat water bath and deposits 15min after shaking up, add 0.081ml substrate and shake up, and puts people's light splitting at once
Photometer measures at 400nm, records the absorbance changing value Δ of reaction 2.5minΑThe numerical value of t.
(3) judgement is calculated
By step 1,2 record ΔΑ0 and ΔΑThe numerical value of t, calculates enzyme inhibition rate (%) by below equation
Suppression ratio (%)=[ΔΑ0 - ΔΑt]/ΔΑ0]×100
(4) qualitatively judge
When the suppression ratio 50% of extracting solution, represent organophosphor or carbamate chemicals for agriculture with the presence of high dose in vegetable,
Sample is positive.
Embodiment 3
A kind of Fast Determination of Pesticide Residue eliminates false-positive detection method, specifically includes following steps:
Step a, test agent are prepared
The reagent preparing needs the most respectively is pH8.0 phosphate buffer, developer, substrate and acetylcholinesterase liquid,
Play collocation method as follows:
PH8.0 phosphate buffer: take 12.5g dipotassium hydrogen phosphate (K2HPO4) and 3.5g potassium dihydrogen phosphate (KH2PO4), be dissolved in
1000ml distilled water just obtains pH8.0 phosphate buffer；
Developer: take 170mg sulfur for dinitrobenzoic acid (DTNB) and 16.4mg sodium bicarbonate (NaHCO3), above-mentioned with 23ml
Phosphate buffer dissolves, in 2-5 DEG C of Refrigerator store.
Substrate: take 27mg acetylthiocholine, adds 3.3ml distilled water and dissolves, shake up and be placed on 6 DEG C of Refrigerator stores.
Acetylcholinesterase liquid: according to the activity of enzyme, with buffer solution, shake up and be placed on 5 DEG C of Refrigerator stores.Wherein enzyme
The absorbance change of liquid 3.2min should control more than 0.3.
Step b, sample pre-treatments
(1) by the 1.5g Rhizoma Zingiberis Recens chosen with. 1.5g Bulbus Allii clear water is rinsed well, be careful not to destroy sample surface tissue；
(2) Rhizoma Zingiberis Recens handled well through above step 1 is rubbed with Bulbus Allii pulverizer, respectively weigh and after rubbing respectively, obtain Rhizoma Zingiberis Recens
1.2g Yu 1.2g Bulbus Allii, adds the pH8.0 phosphate buffer that 5ml configures, and fully after vibration, is placed in 120 DEG C of water-baths
Middle heat treated, the heat treatment time-division drives row into, and the treatment conditions of Rhizoma Zingiberis Recens are 120 DEG C and continue 3min, and the treatment conditions of Bulbus Allii are 110
DEG C continue 2min；Extracting solution good for heat treatment is placed room temperature 25-28 DEG C preserve；
(3): take and step 2 is positioned over the sample that room temperature 28 DEG C preserves, put in centrifuge tube, the centrifuge of 5000 rpms
Persistently rotate 1.2 min, the 18-20 DEG C of preservation in addition of the clear liquid after having processed.
Step C, detection judge
(1) blank liquid test
Take test tube and add 3ml phosphate buffer, add 0.12ml acetylcholinesterase liquid, 0.5ml developer, put after shaking up
It is placed in 35-38 DEG C of thermostat water bath and deposits 20min, add 0.11ml substrate and shake up, put people's spectrophotometer in 420nm at once
Place measures, and records the absorbance changing value Δ of reaction 2.5-3.5minΑThe numerical value of 0.
(2) sample liquid test
Take test tube and add the sample liquid handled well through step b3 of 2-3ml, add 0.09-0.12ml acetylcholinesterase liquid,
0.3-0.5ml developer, is positioned over 35-38 DEG C of thermostat water bath and deposits 15 20min, add 0.08-0.11ml after shaking up
Substrate shakes up, and puts people's spectrophotometer at once and measures at 400-420nm, records the absorbance change of reaction 2.5-3.5min
Value ΔΑThe numerical value of t.
(3) judgement is calculated
By step 1,2 record ΔΑ0 and ΔΑThe numerical value of t, calculates enzyme inhibition rate (%) by below equation
Suppression ratio (%)=[ΔΑ0 - ΔΑt]/ΔΑ0]×100
(4) qualitatively judge
When the suppression ratio 50% of extracting solution, represent organophosphor or carbamate chemicals for agriculture with the presence of high dose in vegetable,
Sample is positive.
Detection is analyzed
According to the mode of above 3 embodiments, do following experimental data comparison.
Variable concentrations pesticide liquid test checking: under conditions of boiling water bath is 3min heat time heating time, verify variable concentrations agriculture
Medicine buffer and the pesticide buffer test result without heat treated, according to the detection process of step c, under the conditions of verifying two kinds
To result of determination concordance；As shown in the table to 5 kinds of Organophosphorus and carbamate pesticides class pesticide the results.Result shows, two
In the case of Zhong, the testing result to suppression ratio has no significant effect, and completely the same in the qualitative judgement line result of 50% suppression ratio,
Therefore qualitative judgement is had no significant effect by 3min heat treatment time.
Note: * represents consistent ,-represent inconsistent
Extraction Rhizoma Zingiberis Recens and each 5 batches of Bulbus Allii respectively, each batch takes the process sample of 3 different embodiments, according to the present invention
Detection method, T1, T2, T3 respectively embodiment 1, the detection method of embodiment 2 embodiment 3, testing result and GB GB/
T5009-2003 " the quick detection of Organophosphorus and carbamate pesticides pesticide residue amount in vegetable " enzyme inhibition rate is sent out contrast, and is used
Gas chromatography does quantitative verification；By 30 groups of Rhizoma Zingiberis Recenss and the Bulbus Allii data of the inventive method detection, do not occur through chromatography checking
Cross false positive results, and 11 false positive results (as shown in the table) occurs in GB rule.
Note :-represent feminine gender ,+representing the positive ,/expression does not detects.
Claims (1)
1. a Fast Determination of Pesticide Residue eliminates false-positive detection method, it is characterised in that specifically include following steps:
Step a, test agent are prepared
The reagent preparing needs the most respectively is pH8.0 phosphate buffer, developer, substrate and acetylcholinesterase liquid,
Play collocation method as follows:
PH8.0 phosphate buffer: take 11.5-12.5g dipotassium hydrogen phosphate (K2HPO4) and 3-3.5g potassium dihydrogen phosphate
(KH2PO4), it is dissolved in 1000ml distilled water and just obtains pH8.0 phosphate buffer；
Developer: take 140-170mg sulfur for dinitrobenzoic acid (DTNB) and 14.8-16.4mg sodium bicarbonate (NaHCO), use
The above-mentioned phosphate buffer of 17-23ml dissolves, in 2-5 DEG C of Refrigerator store；
Substrate: take 23-27mg acetylthiocholine, adds 2.6-3.3ml distilled water and dissolves, shake up and be placed on 3-6 DEG C of Refrigerator store；
Acetylcholinesterase liquid: according to the activity of enzyme, with buffer solution, shake up and be placed on 2-5 DEG C of Refrigerator store；
Wherein the absorbance change of enzyme liquid 2.5-3.2min should control more than 0.3；
Step b, sample pre-treatments
(1) the 1.2-1.5g Rhizoma Zingiberis Recens chosen is rinsed well with .1.2-1.5g Bulbus Allii clear water, be careful not to destroy sample surface
Tissue；
(2) Rhizoma Zingiberis Recens handled well through above step 1 is rubbed with Bulbus Allii pulverizer, respectively weigh and after rubbing respectively, obtain Rhizoma Zingiberis Recens
0.8-1.2g Yu 0.8-1.2g Bulbus Allii, adds the pH8.0 phosphate buffer that 5ml configures, and fully after vibration, is placed in 90-
Heat treated in 120 DEG C of water-baths, the heat treatment time-division drives row into, and the treatment conditions of Rhizoma Zingiberis Recens are 90-120 DEG C and continue 2-3min, greatly
The treatment conditions of Bulbus Allii are 80-110 DEG C and continue 1-2min；Extracting solution good for heat treatment is placed room temperature 25-28 DEG C preserve；
(3): take step 2 is positioned over room temperature 25-28 DEG C preserve sample, put in centrifuge tube, 5000 rpms from
Scheming persistently rotates 0.9-1.2 min, the 18-20 DEG C of preservation in addition of the clear liquid after having processed；
Step C, detection judge
(1) blank liquid test
Take test tube and add 2-3ml phosphate buffer, add 0.09-0.12ml acetylcholinesterase liquid, 0.3-0.5ml colour developing
Agent, is positioned over 35-38 DEG C of thermostat water bath and deposits 15 20min after shaking up, add 0.08-0.11ml substrate and shake up, at once
Put people's spectrophotometer to measure at 400-420nm, record the absorbance changing value Δ of reaction 2.5-3.5minΑThe number of 0
Value；
(2) sample liquid test
Take test tube and add the sample liquid handled well through step b3 of 2-3ml, add 0.09-0.12ml acetylcholinesterase liquid,
0.3-0.5ml developer, is positioned over 35-38 DEG C of thermostat water bath and deposits 15 20min, add 0.08-0.11ml after shaking up
Substrate shakes up, and puts people's spectrophotometer at once and measures at 400-420nm, records the absorbance change of reaction 2.5-3.5min
Value ΔΑThe numerical value of t；
(3) judgement is calculated
By step 1,2 record ΔΑ0 and ΔΑThe numerical value of t, calculates enzyme inhibition rate (%) by below equation
Suppression ratio (%)=[ΔΑ0 - ΔΑt]/ΔΑ0] × 100 ... ... ... (1)
(4) qualitatively judge
When the suppression ratio 50% of extracting solution, represent organophosphor or carbamate chemicals for agriculture with the presence of high dose in vegetable,
Sample is positive.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108444805A (en) * | 2018-02-13 | 2018-08-24 | 广州聚佰生物科技有限公司 | A kind of purifying tablets for rapid detection for pesticide residue pre-treatment |
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