Method for determining residual quantity of myclobutanil by SPE-GC/ECD (Solid Phase Extraction-Gas Chromatography-Electron Capture Detector)

A technology of myclobutanil and residual amount, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve problems such as easy to cause errors, complicated operation, increase operation steps, etc., achieve good accuracy and precision, optimize detection conditions, The effect of high extraction efficiency

Inactive Publication Date: 2013-06-19
TOBACCO RES INST CHIN AGRI SCI ACAD
View PDF3 Cites 7 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The detection practice found that although this residue analysis method has high extraction efficiency, it has the following disadvantages: 1) Since acetone and methanol are used as extraction agents, impurities such as sugars, fats, and proteins are also easily extracted. There is a large interference in the detection. Although dichloromethane is used for multiple extractions, the operation steps are increased, which not only increases the workload, but also easily causes errors.
2) It is difficult to separate the extractant and the water phase, making the extraction and purification process relatively cumbersome
3) The method of column chromatography is not only complicated to operate, but also has poor reproducibility. It is not suitable for tobacco samples containing a lot of pigments, oils, and impurities. Improper purification, impurity peaks can easily interfere with the detection results
[0004] However, if the current detection method is used to detect the residual amount of myclobutanil in tobacco leaves, the defect is that there are many interferences, especially impurities such as nicotine and proteins are likely to interfere with the detection of myclobutanil residues.
Although the above method is easy to operate, it cannot effectively remove impurities such as nicotine and protein in tobacco leaves.
During the detection, the existence of nicotine and protein is easy to form interference peaks, which affects the detection accuracy of the target

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for determining residual quantity of myclobutanil by SPE-GC/ECD (Solid Phase Extraction-Gas Chromatography-Electron Capture Detector)
  • Method for determining residual quantity of myclobutanil by SPE-GC/ECD (Solid Phase Extraction-Gas Chromatography-Electron Capture Detector)
  • Method for determining residual quantity of myclobutanil by SPE-GC/ECD (Solid Phase Extraction-Gas Chromatography-Electron Capture Detector)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Embodiment one: detection of myclobutanil residues in fresh tobacco leaves

[0051] 1. Extraction

[0052] Weigh 10.0g of fresh tobacco leaf sample into a 250mL ground-mouth Erlenmeyer flask, add 80mL of acidic acetonitrile, shake and extract for 1h with a rotary oscillator, add 10-15g of sodium chloride, and continue to shake for 15min. After filtering, the filtrate was dehydrated with anhydrous sodium sulfate, and 40 mL was taken, and concentrated to near dryness under reduced pressure on a rotary evaporator, and the residue was dissolved with 2 mL of acetone / n-hexane (2:8, V / V) and purified.

[0053] 2. Purification and separation

[0054] Use Florisil SPE column (1g / 6mL) to pre-wash with 5mL acetone / n-hexane (2:8, V / V), the sample concentrated solution is passed through the column at a speed of 1-2 drops / second, 18mL acetone / Wash the bottle with n-hexane (2:8, V / V) for 3 times and then rinse. Collect the eluent in a 100mL flat-bottomed flask, concentrate it on a ...

Embodiment 2

[0081] Example two: detection of myclobutanil residues in dried tobacco leaves

[0082] 1. Extraction

[0083] Weigh 4.0 g of dry tobacco leaf sample into a 250 mL ground-neck Erlenmeyer flask, add 80 mL of acidic acetonitrile, oscillate and extract with an orbital shaker for 1 h, add 10-15 g of sodium chloride, and continue shaking for 15 min. After filtering, the filtrate was dehydrated with anhydrous sodium sulfate, and 40 mL was taken, and concentrated to near dryness under reduced pressure on a rotary evaporator, and the residue was dissolved with 2 mL of acetone / n-hexane (2:8, V / V) and purified.

[0084] 2. Purification

[0085] Florisil SPE column (1g / 6mL) was pre-washed with 5mL acetone / n-hexane (2:8, V / V), the sample concentrate was passed through the column at a speed of 1-2 drops / second, and 18mL acetone / n-hexane Wash the bottle with alkanes (2:8, V / V) for 3 times and then rinse. Collect the eluate in a 100mL flat-bottomed flask, concentrate it on a rotary evapora...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention provides a method for determining residual quantity of myclobutanil by SPE-GC / ECD (Solid Phase Extraction-Gas Chromatography-Electron Capture Detector). The method comprises the following steps of: (1) preparation of a standard liquid: weighing a myclobutanil standard substance and dissolving by an organic solvent to set volume so as to prepare a standard storage liquid; stepwise diluting the myclobutanil standard storage liquid to prepare standard working liquid with series of concentrations; (2) extracting residue in a sample; (3) purification: dissolving by an acetone-normal hexane mixed liquid, then, transferring to a Florisil solid phase column pre-sprayed by the acetone-normal hexane mixed liquid and spraying by the acetone-normal hexane mixed liquid; (4) detecting the residual quantity of myclobutanil in the sample by gas chromatography; (5) establishing a standard curve; and (6) calculating the residual quantity of myclobutanil. The detection method provided by the invention has the characteristics of simpleness and rapidness, and accuracy and reliability, and is of significant value to control the residual quantity of myclobutanil in tobacco for guiding safe and reasonable use of myclobutanil in tobacco.

Description

technical field [0001] The invention belongs to the technical field of trace analysis, and in particular relates to a method for measuring the residual amount of myclobutanil in tobacco by using SPE-GC / ECD. Background technique [0002] Myclobutanil is a triazole fungicide, which can inhibit the biosynthesis of pathogenic bacteria epikeratosterol. It has strong systemic property, high drug efficacy, safety to crops and long-lasting effect. It is mainly used to prevent and control various diseases caused by pathogenic bacteria such as ascomycetes and basidiomycetes. It has good control effects on powdery mildew, rust, scab, gray spot and brown spot, and is a promising fungicide . In recent years, with the extensive application of myclobutanil at home and abroad, its residue problems in the environment and agricultural products have become increasingly prominent, and have attracted great attention. [0003] At present, there have been relevant reports on the residue analysis...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 王秀国李义强王凤龙孔凡玉徐金丽徐光军孙惠青郑晓
Owner TOBACCO RES INST CHIN AGRI SCI ACAD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap