CN105806971A

CN105806971A - Method for detecting procymidone residual amount

Info

Publication number: CN105806971A
Application number: CN201410851681.2A
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 method for detecting procymidone in agricultural products, and the method belongs to the fields of pesticide residue analysis and agricultural product safety detection. The method comprises the steps: extracting a to-be-measured substance with acetonitrile, homogenating at high speed with a homogenizer, then filtering, salting out with 5-7 g of sodium chloride, extracting 10.0 mL of a filtrate, and blowing to dry; dissolving with n-hexane, leaching with a Florida silicon column, collecting a leacheate, blowing to dry, making the volume constant, then carrying out gas chromatographic analysis, and achieving the detection of the procymidone residual amount. The method has the advantages of high sensitivity, low detection limit, simple method, relatively small relative standard deviation, good stability and extremely strong practical value.

Description

A kind of determination of residual amount method of procymidone

Technical field

It is an object of the invention to provide a kind of determination of residual amount method of procymidone, belong to pesticide residue analysis and agricultural product security detection category.

Background technology

China is a large agricultural country, 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.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.

Nineteen fifty-two James and Martin proposes gas liquid chromatography, have also been invented first gas chromatography detector simultaneously, the sixties in 20th century and the seventies, development due to gas chromatographic technique, post effect greatly improves, the development of the subjects such as environmental science, it is proposed that the requirement of trace analysis, occurs in that again some high sensitivity, high selective detector successively.Simultaneously as the development of electronic technology, great improvement done again by original detector in structure and circuit, as TCD occurs in that weighing apparatus electric current, horizontal hot-wire temperature and weighing apparatus hot-wire temperature's testing circuit；There is weighing apparatus frequency time-dependent current, weighing apparatus current impulse modulation detection circuit etc. in ECD, so that performance increases again.The eighties in 20th century, quick extensive use due to fused-silica capillary column, detector is proposed that volume is little, it is fast, highly sensitive to respond, selectivity is good requirement, the particularly development of computer and software, making TCD, FID, the sensitivity of ECD and NPD and stability all improve a lot, the detection cell volume of TCD and ECD is substantially reduced.Entering the nineties in 20th century, owing to developing rapidly of electronic technology, computer and software makes MSD production cost and complexity decline, and stability and ruggedness increase, thus one of becoming the most general gas chromatography detector.

Procymidone (Procymidone); it is that a kind of wide spectrum systemic fungicide has protection and therapeutical effect; the gray mold of various crops, the sclerotiniose that occur when to low temperature and high relative humidity have notable preventive effect; Botrytis and Sclerotinia there is specially good effect; in recent years; for preventing and treating food gray mold (Botrytis gray mold), procymidone is widely used.Procymidone belongs to low toxicity antibacterial, and general only have stimulation to skin and eye, and animal has no teratogenesis, mutagenesis, carcinogenesis under test conditions.But, procymidone is widely used simultaneously as its chloride structure and residue problem in the environment attract attention as a kind of efficient antibacterial, and therefore in agricultural product, the mensuration of rotten enzyme profit residual quantity increasingly comes into one's own.

Summary of the invention

It is an object of the invention to provide a kind of efficiently gas phase detection technique, for detecting the residual quantity of procymidone.

The concrete scheme of the procymidone determination of residual amount is proposed: by determinand through 50.0mL acetonitrile extraction according to above-mentioned purpose, high-speed homogenization 2min on refiner, filtering, 5～7g sodium chloride is saltoutd, and extracts 10.0mL filtrate and dries up, add 2.0mL n-hexane to dissolve, add liquid to be measured after pre-leaching Fu Luoli silicon post, and collect filtrate again with leacheate drip washing Fu Luoli silicon post, collect leacheate, filtrate and leacheate are dried up the laggard circulation of qi promoting analysis of hplc of constant volume, it is achieved the mensuration of procymidone residual quantity.

Described drying up refers to: under 50 DEG C of water-baths, nitrogen dries up；

Described pre-leaching refers to: successively with 5.0ml acetone+normal hexane (10:90) and 5.0mL normal hexane drip washing；

Described leacheate refers to: acetone+normal hexane volume ratio is 10:90；

Described drip washing refers to: uses 5.0mL acetone+normal hexane (10+90) drip washing Fu Luoli silicon post, and is repeated once；

Described constant volume refers to: be settled to 5.0ml with normal hexane；

Described gas chromatographic analysis refers to: Agilent6890 gas chromatograph, joins ECD detector；Chromatographic column: DB-130m × 0.53mm × 0.25 μm；Post flow: 4.0ml/min (constant current mode)；Injector temperature: 220 DEG C；Sample introduction pattern: Splitless injecting samples；Detector temperature: 280 DEG C；Sampling volume: 1 μ L；Under above-mentioned chromatographic condition, the retention time of procymidone is 7.181min.

The computing formula of described procymidone residual quantity is:

Wherein R-sample Pesticide Residues (mg/kg)；C_Mark-concentration of standard solution (mg/L)；V_Mark-standard solution sampling volume (mL)；V_EventuallyThe final constant volume of-sample solution (mL)；V_Sample-sample solution sampling volume (mL)；S_MarkThe peak area (Hz*s) of-injection standard solution；S_SampleThe peak area (Hz*s) of-injecting sample solution；W-claims sample weight (g).

Minimum detectable activity of the present invention is 1.0 × 10^-10G, minimum concentrations is 0.01mg/kg, highly sensitive, and detection limit is low, and method is simple, and relative standard deviation is less, good stability.

Accompanying drawing explanation

Fig. 1 procymidone standard solution chromatogram

Fig. 2 Fructus Cucumidis sativi blank sample chromatogram

Fig. 3 Fructus Cucumidis sativi actual measurement chromatogram

Detailed description of the invention

Example 1

Fructus Cucumidis sativi sample

Pretreatment: by Fructus Cucumidis sativi sample through 50.0mL acetonitrile extraction, uses filter paper filtering on refiner after high-speed homogenization 2min, 5～7g sodium chloride is saltoutd, make acetonitrile phase and aqueous phase layering, extract 10.0mL filtrate, dry up with Nitrogen evaporator under 50 DEG C of water-baths, add 2.0mL n-hexane.

Measure: by Fu Luoli silicon post successively with 5.0ml acetone+normal hexane (10+90) and 5.0mL normal hexane pre-leaching, when solvent liquid level arrives post absorbed layer surface, solution collect filtrate after pouring above-mentioned pretreatment immediately into, again with 5.0mL acetone+normal hexane (10+90) drip washing Fu Luoli silicon post, and be repeated once, collect leacheate, by filtrate and leacheate, nitrogen under 50 DEG C of water-baths dries up, it is settled to 5.0ml with normal hexane, carries out gas chromatographic analysis.

Assay recovery result data is as shown in the table:

As it is shown in figure 1, be procymidone standard solution chromatogram, in figure: the characteristic peak that chromatographic peak is procymidone that 7.181min occurs.

As in figure 2 it is shown, be Fructus Cucumidis sativi blank sample chromatogram, in figure: the chromatographic peak that 1.614min, 1.686min and 6.745min occur is impurity peaks, and chromatographic peak does not occur in 7.181min, illustrates in Fructus Cucumidis sativi blank sample without procymidone.

As it is shown on figure 3, Fructus Cucumidis sativi adds procymidone chromatogram, in figure: contrasting with Fructus Cucumidis sativi blank sample chromatogram, chromatographic peak occurs in 7.181min, illustrates to can detect that procymidone in this sample.

Claims

1. the method for a procymidone determination of residual amount, it is characterized in that: by determinand through 50.0mL acetonitrile extraction, high-speed homogenization 2min on refiner, filter, 5～7g sodium chloride is saltoutd, extract 10.0mL filtrate to dry up, add 2.0mL n-hexane and dissolve, after pre-leaching Fu Luoli silicon post, add liquid to be measured, and collect filtrate again with leacheate drip washing Fu Luoli silicon post, collect leacheate, filtrate and leacheate are dried up the laggard circulation of qi promoting analysis of hplc of constant volume, it is achieved the mensuration of procymidone residual quantity.

2. the assay method of procymidone residual quantity according to claim 1, is characterized in that, described drying up refers to: under 50 DEG C of water-baths, nitrogen dries up.

3. saying according to right and require the assay method of procymidone residual quantity described in 1, it is characterized in that, described pre-leaching refers to: successively with 5.0ml acetone+normal hexane (10:90) and 5.0mL normal hexane drip washing.

4. the assay method of procymidone residual quantity according to claim 1, is characterized in that, described leacheate refers to: acetone+normal hexane volume ratio is 10:90.

5. the assay method of procymidone residual quantity according to claim 1, is characterized in that, described drip washing refers to: with 5.0mL acetone+normal hexane (10+90) drip washing Fu Luoli silicon post, and is repeated once.

6. the assay method of procymidone residual quantity according to claim 1, is characterized in that, described constant volume refers to: be settled to 5.0ml with normal hexane.

7. the assay method of procymidone residual quantity according to claim 1, is characterized in that, described gas chromatographic analysis refers to: Agilent6890 gas chromatograph, joins ECD detector；Chromatographic column: DB-130m × 0.53mm × 0.25 μm；Post flow: 4.0ml/min (constant current mode)；Injector temperature: 220 DEG C；Sample introduction pattern: Splitless injecting samples；Detector temperature: 280 DEG C；Sampling volume: 1 μ L；Under above-mentioned chromatographic condition, the retention time of procymidone is 7.181min.