CN105806970A

CN105806970A - Detection method for acetamiprid residual amount

Info

Publication number: CN105806970A
Application number: CN201410851635.2A
Authority: CN
Inventors: 张海燕
Original assignee: Individual
Current assignee: Individual
Priority date: 2014-12-31
Filing date: 2014-12-31
Publication date: 2016-07-27

Abstract

The invention relates to a detection method for acetamiprid in agricultural products, and the method belongs to the fields of pesticide residue analysis and agricultural product safety detection. The method is characterized by comprising the steps: extracting a to-be-measured substance with acetonitrile, homogenating at high speed with a homogenizer, then filtering, salting out with NaCl, extracting 10 ml of a filtrate, and blowing to dry; adding methanol and dichloromethane, dissolving, passing through an amino column, leaching the dissolving liquid, collecting a leacheate, blowing to dry, making the volume constant, filtering, then carrying out liquid chromatographic analysis, and achieving the detection of the acetamiprid residual amount. The method has the following excellent effects: the operation is simple and fast, the precision is high, the recovery rate is high, the detection limit is low, interference of other substances in the agricultural products on the detection of the acetamiprid residual amount is effectively reduced, and scientific basis is provided for quality safety of the agricultural products.

Description

A kind of detection method determining worm amidine residual quantity

Technical field

The present invention relates to pesticide residue analysis and agricultural product security detection technique field, be specially a kind of detection method determining worm amidine residual quantity.

Background technology

China is a large agricultural country, and the crops planting area such as Cereal, vegetable and fruit is big, and gross annual output amount is high, and Agricultural Products Trade accounts for consequence in China's export is earned foreign exchange.But the development along with agriculture industrialization, the production of agricultural product is increasingly dependent on the agrochemicals such as pesticide, pesticide while bringing huge interests to the mankind, also because management and improper use bring serious pollution problem to the ecological environment of the mankind and people necessary agricultural product of living.For this, the further strengthening supervision to pesticide producing, operation and use links, rectify and purify pesticide market, the work carrying out chemistry security monitoring is to have very important meaning.Chemistry security monitoring is an element task and the important means of implementing agricultural product quality and safety supervision.By chemistry security monitoring and evaluation project implementation, reflection agricultural product quality and safety situation more objectively, strengthen Monitoring Data and collect and the analysis of causes, hold security-hidden trouble and scope, conscientiously accomplish to avert risks in time.At present, in China mainly through pesticide is carried out residue detection, the safety in utilization of pesticide is detected.

Acetamiprid is a kind of New-type wide-spectrum, efficient, safe pesticide, belongs to Nitromethylene heterocycle compound, the class pests such as Semiptera (such as aphid, aleyrodid etc.), Lepidoptera (such as diamondback moth, Grapholita spp etc.) are had significantly high activity.But to people and animals' low toxicity, pest natural enemy lethality is little, fish toxicity is relatively low, Apis impact is little, the insect of pyrethroid, Organophosphorus and carbamate pesticides class generation resistance is also effective, useful stronger the tagging and osmosis of Acetamiprid, is one of excellent pesticidal agent of having wide application prospects at present, has had begun to promotion and application in China.It is 0.5-1.0ml/kg that China " GB2763 2012 " determines worm amidine MRL in vegetable.

High performance liquid chromatography HPLC is the novel separate analytical technique of the one grown up early 1960s, through constantly improving and development, has become the important means that the extremely wide Chemical Decomposition of application is analyzed at present.A kind of chromatography that HPLC is is mobile phase with liquid, it can separation detection polarity strong, the ion-type pesticide that molecular weight is big, is particularly suited for, to not easily gasifying or appearance labile organic agricultural chemicals detection of being heated, measuring the persticide residue in agricultural product fast and efficiently.Current Han Zhen is safe etc. by reversed phase high-performance liquid chromatography is used for measuring the residual quantity of thiacloprid after Fraxinus velutina trunk and soil pesticide, Hou Ruyan etc. report and use nicotinoids pesticide concentration in vegetables by HPLC, fruit, but the high-efficiency liquid chromatography method for detecting determining worm amidine is had no report at home.

Summary of the invention

Present invention aim at providing a kind of high-efficient liquid phase chromatogram technology, the response rate is high, and precision is high, for detecting the residual quantity determining worm amidine in crops.

Proposing to determine the concrete scheme of the worm amidine determination of residual amount according to above-mentioned purpose: by determinand through 50ml acetonitrile extraction, refiner is used after high-speed homogenization 2min filter paper filtering, 3.5gNaCl extracts 10ml filtrate after saltouing and dries up；Add 2.0ml methanol+dichloromethane to dissolve, pre-leaching nh 2 column, add liquid to be measured, after nh 2 column leacheate drip washing, collect after leacheate dries up constant volume filtration and carry out liquid-phase chromatographic analysis, it is achieved determine the mensuration of worm amidine residual quantity.

Described drying up refers to: under 80 DEG C of water-baths, nitrogen dries up；

Described methanol+dichloromethane mixed liquor refers to: the volume ratio of methanol and dichloromethane is 5:95；

Described leacheate refers to: dichloromethane；

Described pre-leaching refers to: uses 5ml eluent methylene chloride nh 2 column, and is repeated once；

Described drip washing refers to: uses 5ml eluent methylene chloride nh 2 column, and is repeated once；

Described constant volume refers to: with methanol+water constant volume 5.0ml (first add 2.0ml methanol, then be settled to 5.0ml with water)；

Described filtration refers to: with 0.45 μm of membrane filtration；

Described liquid-phase chromatographic analysis refers to: adopts Agilent1100 type chromatograph of liquid, joins VWD detector chromatographic column: Eclipse4.6 × 250mm × 5.0 μm；Post flow: 0.8ml/min；Mobile phase: methanol: water (40:60)；Sampling volume: 10 μ L；Relative retention time: under above-mentioned liquid phase chromatogram condition, Acetamiprid relative retention time is 4.90min.

Minimum detectable activity and minimal detectable concentration is adopted to represent sensitivity.Acetamiprid minimum detectable activity is 3.0 × 10-11g, and the minimal detectable concentration of Acetamiprid is 0.025mg/kg, it was shown that the present invention is highly sensitive, and detection limit is low, and method is simple, and the response rate is high, and selectivity is good.

Accompanying drawing explanation

Fig. 1 determines worm amidine standard solution chromatogram

Fig. 2 pakchoi blank sample chromatogram

Fig. 3 pakchoi actual measurement chromatogram

Detailed description of the invention

Below the implementation of the present invention being described in detail, this example is carried out under premised on technical solution of the present invention, gives detailed embodiment and concrete operating process.

Example 1

Pakchoi sample

Pretreatment: weigh 25.0g pakchoi sample sample, adds 50ml acetonitrile, refiner uses filter paper filtering after high-speed homogenization 2min；After 3.5gNaCl saltouts, extracting 10ml filtrate, 80 DEG C of water-baths, nitrogen dries up；Add 2.0ml methanol+dichloromethane (5+95) dissolved residue, to be clean.

Measure: by nh 2 column 5ml dichloromethane pre-leaching, and be repeated once, when solvent liquid level arrives post adsorption layer surface, add liquid to be clean immediately, then with 5.0ml leacheate drip washing, and come again.The 80 DEG C of water-baths of filtrate that will collect, nitrogen blows near dry, with methanol+water constant volume 5.0ml (first add 2.0ml methanol, then be settled to 5.0ml with water), with 0.45 μm of membrane filtration, to be measured.

Assay recovery data such as following table:

As it is shown in figure 1, for determine worm amidine standard solution chromatogram, in figure: the chromatographic peak that 4.9min occurs is the characteristic peak determining worm amidine.

As in figure 2 it is shown, be pakchoi blank sample chromatogram, in figure: the chromatographic peak that 3.3min, 4.1min, 4.4min, 4.6min and 5.3min place occurs is impurity peaks, and chromatographic peak does not occur in 4.9min, illustrates in pakchoi blank sample without determining worm amidine.

As it is shown on figure 3, pakchoi adds determines worm amidine chromatogram, in figure: contrast with pakchoi blank sample chromatogram, at 4.9min, chromatographic peak occurs, illustrate this sample can detect that and determine worm amidine.

Claims

1. the detection method determining worm amidine residual quantity, it is characterised in that: first after 50ml acetonitrile extraction, concussion 30min, determinand being used filter paper filtering, 3.5gNaCl extracts 10ml filtrate after saltouing and dries up；Add 2.0ml methanol+dichloromethane to dissolve, pre-leaching nh 2 column, add liquid to be measured, after nh 2 column leacheate drip washing, collect after leacheate dries up constant volume filtration and carry out liquid-phase chromatographic analysis, it is achieved determine the detection of worm amidine residual quantity.

2. the detection method determining worm amidine residual quantity according to claim 1, is characterized in that, described drying up refers to: under 80 DEG C of water-baths, nitrogen dries up.

3. the detection method determining worm amidine residual quantity according to claim 1, is characterized in that, described methanol+dichloromethane mixed liquor refers to: the volume ratio of methanol and dichloromethane is 5:95.

4. the detection method determining worm amidine residual quantity according to claim 1, is characterized in that, described pre-leaching refers to: uses 5ml eluent methylene chloride nh 2 column, and is repeated once.

5. the detection method determining worm amidine residual quantity according to claim 1, is characterized in that, described leacheate refers to: dichloromethane.

6. the detection method determining worm amidine residual quantity according to claim 1, is characterized in that, described drip washing refers to: uses 5ml eluent methylene chloride nh 2 column, and is repeated once.

7. the detection method determining worm amidine residual quantity according to claim 1, is characterized in that, described constant volume refers to: with methanol+water constant volume 5.0ml (first add 2.0ml methanol, then be settled to 5.0ml with water).

8. the detection method determining worm amidine residual quantity according to claim 1, is characterized in that, described filtration refers to: with 0.45 μm of membrane filtration.

9. the detection method determining worm amidine residual quantity according to claim 1, is characterized in that, described liquid-phase chromatographic analysis refers to: adopts Agilent1100 type chromatograph of liquid, joins VWD detector chromatographic column: Eclipse4.6 × 250mm × 5.0 μm；Post flow: 0.8ml/min；Mobile phase: methanol: water (40:60)；Sampling volume: 10 μ L；Relative retention time: under above-mentioned liquid phase chromatogram condition, Acetamiprid relative retention time is 4.90min.