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A method for analyzing residues of polyoxin in ginseng

A technology for analysis of polyoxin and residues, which is applied in the direction of analysis of materials, material separation, and measuring devices. strong effect

Active Publication Date: 2017-09-01
JILIN AGRICULTURAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, our device, high performance liquid chromatography, capillary electrophoresis-electrochemiluminescence (CE-ECL), etc., but these methods generally have low recovery rate and poor reproducibility when applied to ginseng matrix, so there is no reference Therefore, the determination of polyoxin fungicide residues in ginseng has become a difficult point in the current residue analysis

Method used

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  • A method for analyzing residues of polyoxin in ginseng
  • A method for analyzing residues of polyoxin in ginseng
  • A method for analyzing residues of polyoxin in ginseng

Examples

Experimental program
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Effect test

Embodiment 1

[0075] Example 1: Determination of polyoxin in ginseng plants

[0076] Weigh 5.0 g of the ginseng plant sample and put it into a beaker, add 20 mL of 0.3% formic acid aqueous solution, adjust the pH range to 2-5, homogenate for about 2 min, filter under reduced pressure in a Buchner funnel covered with filter aid, and remove all the filtrate Collect in a stoppered measuring cylinder, draw part of the filtrate into a centrifuge tube, centrifuge at 12000rpm for 5min, pass through a 0.22μm filter membrane, and wait for detection by liquid chromatography-mass spectrometry. Figure 5-Figure 6 ,From Figure 5 , Figure 6 It can be seen that the recovery rate is significantly improved after acid addition.

[0077] The assay result of polyoxin in the ginseng plant of embodiment 1

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Embodiment 2

[0082] Embodiment 2: the mensuration of polyoxin in ginseng soil

[0083] Weigh 5.0 g of the soil sample into a stoppered Erlenmeyer flask, add 20 mL of 0.3% formic acid aqueous solution, adjust the pH range to 2-5, shake and extract for 1 h, vacuum filter under reduced pressure in a Buchner funnel covered with filter aid, and remove all the filtrate Collect in a stoppered measuring cylinder, draw part of the filtrate into a centrifuge tube, centrifuge at 12000rpm for 5min, pass through a 0.22μm filter membrane, and wait for detection by liquid chromatography-mass spectrometry. Figure 7-Figure 8 ,From Figure 7 , Figure 8 It can be seen that the recovery rate is significantly improved after acid addition.

[0084] The assay result of polyoxin in embodiment 2 soil

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Embodiment 3

[0089] Embodiment 3: Determination of polyoxin in fresh ginseng

[0090] Weigh 5.0g of fresh ginseng sample and put it into a beaker, add 20mL of 0.3% formic acid aqueous solution, adjust the pH range to 2-5, homogenate for about 2min, filter under reduced pressure in a Buchner funnel covered with filter aid, and filter all the filtrate Collect in a stoppered measuring cylinder, draw part of the filtrate into a centrifuge tube, centrifuge at 12000rpm for 5min, pass through a 0.22μm filter membrane, and wait for detection by liquid chromatography-mass spectrometry. Figure 9-Figure 10 ,From Figure 9 , Figure 10 It can be seen that the recovery rate is significantly improved after acid addition.

[0091] The assay result of polyoxin in embodiment 2 soil

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Abstract

The invention provides a method for analyzing residues of polyoxin on ginseng, establishes a method for analyzing residues of polyoxin on ginseng, and uses an aqueous solution containing formic acid to homogeneously extract residual polyoxin in a sample, After passing through the membrane, liquid chromatography mass spectrometry-mass spectrometry (HPLCMS-MS) detection, a calibration standard curve was established using a blank matrix solution without the pesticide to be tested, and the external standard method was used for quantification. The pretreatment is simple and less organic reagents are used, the recovery rate meets the requirements of the pesticide residue guidelines, and the method meets the current environmental protection requirements. Moreover, the accuracy and precision of the detection method meet the technical requirements of residue analysis, and the detection limit meets the requirements of domestic and foreign technical regulations and limit standards. The average recovery rate of the present invention is 74.6%-94.7%, the average relative standard deviation (RSD) is 1.3%-7.8%, and the detection limit is lower than 0.06mg / kg. Good performance, qualitative and quantitative accuracy.

Description

technical field [0001] The invention provides a residue analysis method of polyoxin on ginseng, which is an improvement on the existing residue analysis method and belongs to the technical field of chemical analysis of Chinese herbal medicines. Background technique [0002] Polyoxin is an actinomycete isolated from the soil in Sojunbo, Kumamoto Prefecture by Dr. Saburo Suzuki from the Institute of Physical and Chemical Research of Japan in 1963. It is a broad-spectrum antibiotic fungicide with endogenous suction conduction. It has been put into production and application in my country since 1982. It is mainly used to control wheat powdery mildew, ginseng black spot, tobacco red spot, cucumber downy mildew, melon wilt, rice sheath blight, apple leaf spot, strawberry and grape gray mold disease, tree dead sheath disease and other fungal diseases. Its unique mechanism of action can interfere with the biosynthesis of cell wall chitin. Some fungi, germ tubes, and mycelia of the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 侯志广逯忠斌王秀梅逯洲赵晓峰潘普群侯新港刘亚娟刘良月张浩王鑫宏
Owner JILIN AGRICULTURAL UNIV