CN107966339A - A kind of residual preparation method for quantitatively detecting sample of Chinese celery chlopyrifos agriculture - Google Patents
A kind of residual preparation method for quantitatively detecting sample of Chinese celery chlopyrifos agriculture Download PDFInfo
- Publication number
- CN107966339A CN107966339A CN201711169159.6A CN201711169159A CN107966339A CN 107966339 A CN107966339 A CN 107966339A CN 201711169159 A CN201711169159 A CN 201711169159A CN 107966339 A CN107966339 A CN 107966339A
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- CN
- China
- Prior art keywords
- chinese celery
- sample
- agriculture
- detection
- celery
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
Abstract
A kind of residual preparation method for quantitatively detecting sample of Chinese celery chlopyrifos agriculture, preparation including treating Chinese celery sample treatment and Chinese celery detection liquid sample, its core is sharp Chinese celery body fluid as the residual unified standard sample mother liquor quantitatively detected of agriculture, it is wherein various to wait detection essence composition identical with the concentration of composition in fresh Chinese celery body, use it as mother liquor to be detected, equivalent to measure liquid of the people by the use of blood of human body as health index, overcome different reviewers in actually detected operating process to Chinese celery mud diluted concentration not without equal, the reasons such as thinned water pollution make the defects of detection data are unstable, use Chinese celery juice, overcome the deficiency of conventional size reduction sample preparation methods, detection result is more preferable, at the same time manual weighing is eliminated to be not allowed, sample preparation is uneven, sample the deficiencies of irregular, with liquid-transfering gun it is faster more accurate move in centrifuge tube.Pre-treating method is easy to be more efficient quick, improves 35 times of work efficiency, reduces testing cost.
Description
Technical field:
The invention belongs to the residual detection technique field of agriculture, and in particular to a kind of method that Chinese celery chlopyrifos quantitatively detects.
Background technology:
At present, Chinese celery is the high-grade fresh vegetable that people are very familiar to, and is liked by people, especially Jiangsu Province's Changzhou
The geographical mark product in Jintan area --- Jintan strengthens, people without the superfine product that water-saving celery is even more in Chinese celery with the consciousness of food security
The residual problem of agriculture to all kinds of fresh vegetables extremely pay close attention to, particularly each batch of exported product has the residual detection of stringent agriculture will
Ask, if detection speed is unhappy or detection data are unreliable, vegetable farmer will be directly affected and the economic of processing and sales enterprise is imitated
Benefit, in order to further carry out service vegetable grower, must carry out scientific and technical innovation, further for being responsible for the fresh residual detection department of vegetable agriculture
Improve detection speed and detect the reliability of data.At present, for the residual problem of agriculture in relation to Chinese celery than more serious, detection speed is low, inspection
It is poor to survey data stability, censorship enterprise report is continuous, and applicant is by for a long time main the reason for researching and analysing, cause drawbacks described above
It is the making of Chinese celery detected sample, existing production program is to crush mud as detection sample using Chinese celery, different classes of
During the residual detection of agriculture, Chinese celery mud adds water to carry out uncommon pool processing after taking crushing respectively, obtains the Chinese celery solution of respective concentration, then carries out
Corresponding essence ion concentration measure, so holds that sample preparation concentration occur irregular very much, causes to test and analyze unstable result, goes out the inspection of evidence
Observe and predict announcement and secondary detection data deviation is excessive so that the registration of testing result is low, causes purchaser to return goods when serious, to agriculture
The people cause economic loss.
The content of the invention:
In order to overcome the shortcomings of the prior art, the present invention provides a kind of residual quantitatively detection sample of Chinese celery chlopyrifos agriculture
Preparation method, is made Chinese celery sample in this way, and detection speed is fast, and detection data stabilization is good, and multiplicity is high.
The technical solution that the present invention takes is as follows:
A kind of residual preparation method for quantitatively detecting sample of Chinese celery chlopyrifos agriculture, comprises the following steps:
Step 1:Chinese celery sample treatment:
After the Chinese celery sample of censorship is gone root, cleaned with clean water, then with pure water rinse, the cauline leaf of Chinese celery is cut into
The segment of 3~5 centimeter lengths, carries out centrifugal dehydration after being packed with analysis filter bag, is then placed in juice extractor and is crushed, with filter
It is spare that bag carries out filtering acquisition Chinese celery juice;
Step 2:It is prepared by Chinese celery detection liquid sample:
Chinese celery liquid sample prepared by step 1 draws 10ml Chinese celery sap sample decant(-ation)s in centrifuge tube, adds 10ml second
Nitrile, lid lid, vibrates 20min, adds Nacl and Mgso4Mixture 5g, Nacl and Mgso4Molar ratio be 1:4, hand 1min, are used
Big centrifuge centrifuges 5min under the conditions of rotating speed 6000rpm, and Aspirate supernatant is pure in 2 CNWDSPE dispersive solid-phase extractions respectively
Change in pipe, then add Mgso4 150mg、PSA 50mg、C1850mg, shakes and with small centrifuge at rotating speed 6000rpm centrifugations
2min is managed, each 1ml of liquid in two purifying pipes is drawn respectively in the small test tube of two 5ml, is blown with 60 DEG C of nitrogen and closely done,
Draw 1ml acetone constant volume, shaking in a small test tube to mix, move in sample bottle, upper machine is detected for organophosphor;Draw 1ml
N-hexane constant volume, shaking in another small test tube mix, and are filtered with hydrophilic PTFE pin types filter into sample bottle, for chrysanthemum ester
The upper machine of class detection.
The beneficial effects of the present invention are:
Present invention improves over sample preparation technology and theory, is detected using the javan waterdropwort juice for determining concentration ecosystem as unification
Mother liquor, wherein various wait detection essence composition identical with the concentration of composition in fresh Chinese celery body, uses it as mother to be detected
Liquid, equivalent to measure liquid of the people by the use of blood of human body as health index, overcomes different reviewers in actual inspection
To survey in operating process to Chinese celery mud diluted concentration not without equal, the reason such as thinned water pollution makes the defects of detection data are unstable,
Using Chinese celery juice, the deficiency of conventional size reduction sample preparation methods is overcome, detection result is more preferable, while eliminates manual weighing
Inaccurate, sample preparation is uneven, samples the deficiencies of irregular, with liquid-transfering gun it is faster more accurate move in centrifuge tube.Pre-treating method simplicity is more
Efficient quick, improves 3-5 times of work efficiency, reduces testing cost.
Embodiment:
Illustrate the embodiment of the present invention below:
Embodiment 1:A kind of residual preparation method for quantitatively detecting sample of Chinese celery chlopyrifos agriculture, comprises the following steps:
Step 1:Chinese celery sample treatment:
After the Chinese celery sample of censorship is gone root, cleaned with clean water, then with pure water rinse, the cauline leaf of Chinese celery is cut into
The segment of 3~5 centimeter lengths, carries out centrifugal dehydration after being packed with analysis filter bag, is then placed in juice extractor and is crushed, with filter
It is spare that bag carries out filtering acquisition Chinese celery juice;
Step 2:It is prepared by Chinese celery detection liquid sample:
Chinese celery liquid sample prepared by step 1 draws 10ml Chinese celery sap sample decant(-ation)s in centrifuge tube, adds 10ml second
Nitrile, lid lid, vibrates 20min, adds Nacl and Mgso4Mixture 5g, Nacl and Mgso4Molar ratio be 1:4, hand 1min, are used
Big centrifuge centrifuges 5min under the conditions of rotating speed 6000rpm, and Aspirate supernatant is pure in 2 CNWDSPE dispersive solid-phase extractions respectively
Change in pipe, then add Mgso4 150mg、PSA 50mg、C1850mg, shakes and with small centrifuge at rotating speed 6000rpm centrifugations
2min is managed, each 1ml of liquid in two purifying pipes is drawn respectively in the small test tube of two 5ml, is blown with 60 DEG C of nitrogen and closely done,
Draw 1ml acetone constant volume, shaking in a small test tube to mix, move in sample bottle, upper machine is detected for organophosphor;Draw 1ml
N-hexane constant volume, shaking in another small test tube mix, and are filtered with hydrophilic PTFE pin types filter into sample bottle, for chrysanthemum ester
The upper machine of class detection.
Claims (1)
1. a kind of residual preparation method for quantitatively detecting sample of Chinese celery chlopyrifos agriculture, it is characterized in that:Comprise the following steps:
Step 1:Chinese celery sample treatment:
After the Chinese celery sample of censorship is gone root, cleaned with clean water, then with pure water rinse, the cauline leaf of Chinese celery is cut into 3~5
The segment of centimeter length, with analysis filter bag pack after carry out centrifugal dehydration, be then placed in juice extractor and crushed, with filter bag into
It is spare that row filtering obtains Chinese celery juice;
Step 2:It is prepared by Chinese celery detection liquid sample:
Chinese celery liquid sample prepared by step 1 draws 10ml Chinese celery sap sample decant(-ation)s in centrifuge tube, adds 10ml acetonitriles, lid lid
Son, vibrates 20min, adds Nacl and Mgso4Mixture 5g, Nacl and Mgso4Molar ratio be 1:4, hand 1min, with big centrifugation
Machine centrifuges 5min under the conditions of rotating speed 6000rpm, and Aspirate supernatant is purified in pipe in 2 CNWDSPE dispersive solid-phase extractions respectively,
Plus Mgso then4150mg、PSA 50mg、C1850mg, shakes and with small centrifuge in rotating speed 6000rpm centrifugal treating 2min,
Each 1ml of liquid in two purifying pipes is drawn respectively in the small test tube of two 5ml, and near dry, absorption 1ml is blown with 60 DEG C of nitrogen
Acetone constant volume, shaking in a small test tube mix, and move in sample bottle, and upper machine is detected for organophosphor;Draw 1ml n-hexanes in
Constant volume, shaking mix in another small test tube, are filtered with hydrophilic PTFE pin types filter into sample bottle, in the detection of chrysanthemum esters
Machine.
Priority Applications (1)
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CN201711169159.6A CN107966339A (en) | 2017-11-22 | 2017-11-22 | A kind of residual preparation method for quantitatively detecting sample of Chinese celery chlopyrifos agriculture |
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CN201711169159.6A CN107966339A (en) | 2017-11-22 | 2017-11-22 | A kind of residual preparation method for quantitatively detecting sample of Chinese celery chlopyrifos agriculture |
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CN107966339A true CN107966339A (en) | 2018-04-27 |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108426756A (en) * | 2018-05-15 | 2018-08-21 | 常州市金坛区农产品质量检验检测中心 | A kind of differential speed change broken wall filtering all-in-one machine of fruits and vegetables sample homogenization |
-
2017
- 2017-11-22 CN CN201711169159.6A patent/CN107966339A/en active Pending
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108426756A (en) * | 2018-05-15 | 2018-08-21 | 常州市金坛区农产品质量检验检测中心 | A kind of differential speed change broken wall filtering all-in-one machine of fruits and vegetables sample homogenization |
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Application publication date: 20180427 |
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