Method for detecting difenoconazole and azoxystrobin in garlic

A technology for azoxystrobin and difenoconazole, which is applied in the field of pesticide residue detection, can solve the problems of long detection time, complicated pretreatment process, inability to meet trace analysis requirements, etc., achieves optimization of instrument detection conditions, and improves instrument sensitivity and resolution. Ability, the effect of shortening the analysis and detection time

Pending Publication Date: 2020-12-18
安徽华辰检测技术研究院有限公司
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  • Abstract
  • Description
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Problems solved by technology

The quantitative limit of the gas chromatography instrument is relatively high, which cannot meet the requirements of trace analysis. The gas chromatography-mass spectrometry method has a complicated and cumbersome pretreatment process, and the detection time of the two methods is very long
There are no domestic reports on the detection methods of difenoconazole and azoxystrobin in various garlic matrices. In order to study the changes of difenoconazole and azoxystrobin residues in garlic matrices, it is necessary to explore a garlic matrix A convenient and accurate method for the detection of difenoconazole and azoxystrobin

Method used

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  • Method for detecting difenoconazole and azoxystrobin in garlic
  • Method for detecting difenoconazole and azoxystrobin in garlic
  • Method for detecting difenoconazole and azoxystrobin in garlic

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Experimental program
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Effect test

Embodiment 1

[0065] A method for detecting difenoconazole and azoxystrobin in garlic, using liquid chromatography tandem mass spectrometer LCMS-8040 from Shimadzu Corporation, Japan, wherein the high performance liquid chromatography conditions are: the chromatographic column is Shim-pack XR -ODSⅡ chromatographic column (2mm I.D. * 75mm), mobile phase A is the formic acid aqueous solution of 0.1% by volume fraction, and mobile phase B is acetonitrile, and elution mode is isocratic elution, and the volume ratio of mobile phase A and mobile phase B is 20:80, the flow rate is 0.3mL / min; the column temperature is 35°C, the injection volume is 1μL, and the HPLC acquisition time is ≤3min;

[0066] The mass spectrometry conditions are: the ion source is an electrospray ion source under atmospheric pressure, a triple quadrupole mass analyzer, the ion source is in positive ion mode, the interface voltage is 4.5kv, the DL tube temperature is 250°C, the heating block temperature is 400°C, and the fog ...

Embodiment 2

[0119] Embodiment 2 garlic recovery rate test

[0120] By adding a sample of known concentration, the residual amount of difenoconazole and azoxystrobin in the sample was detected according to the method and detection conditions of Example 1, and the recovery rate was calculated.

[0121] experiment procedure:

[0122] Take the garlic blank matrix, weigh 6 parts, weigh 5.000g for each part, numbered A, B, C, D, E, F, G, H, and then take the standard stock solution of difenoconazole and azoxystrobin (Same as Example 1) Dilute to different concentrations respectively, add to A, B, C, D, E, F, G, H garlic blank matrix, mix evenly, make difenoconazole, pyrimidine in A, B samples The added concentrations of strytostrobin were 0.02mg / kg and 0.01mg / kg respectively; the added concentrations of difenoconazole and azoxystrobin in C and D samples were 0.2mg / kg and 0.1mg / kg respectively; E and F samples The added concentrations of difenoconazole and azoxystrobin were 2mg / kg and 1mg / kg r...

Embodiment 3

[0137] Embodiment 3 Garlic shoot recovery rate test

[0138] Garlic sprout samples were used for the addition recovery test, so that the added concentrations of difenoconazole and azoxystrobin in samples A and B were 0.02mg / kg and 0.01mg / kg respectively; The added concentration of strytostrobin was 0.2mg / kg and 0.1mg / kg respectively; the added concentrations of difenoconazole and azoxystrobin in samples E and F were 2mg / kg and 1mg / kg respectively; The added concentrations of diemeconazole and azoxystrobin were both 4 mg / kg; then the recovery rate was detected and calculated according to the method of Example 2, and the results are shown in Table 11-13.

[0139] Table 11 Linear regression equation of difenoconazole in garlic sprouts

[0140]

[0141]

[0142] Table 12 Linear regression equation of azoxystrobin in garlic sprouts

[0143]

[0144] The recoveries of difenoconazole and azoxystrobin in garlic sprouts were calculated according to the linear regression equa...

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Abstract

The invention discloses a method for detecting difenoconazole and azoxystrobin in garlic, a high performance liquid chromatography-mass spectrometry method is adopted for detection, addition and recovery tests are carried out in garlic bulbs, green garlic and young garlic shoots, the recovery rate of difenoconazole on the garlic bulbs is 80%-104%, and RSD is 1%; the recovery rate of difenoconazoleon green garlic is 87%-103%, and RSD is 1%-3%; the recovery rate of difenoconazole on young garlic shoots is 92%-107%, and RSD is 1%-9%; the recovery rate of azoxystrobin on garlic bulbs is 79%-95%,and RSD is 2%-4%; the recovery rate ofazoxystrobin on green garlic is 93%-117%, and RSD is 1%-3%; the recovery rate of azoxystrobin on young garlic shoots is 83%-105%, and RSD is 2%-6%. The blank thatdifenoconazole and azoxystrobin in three matrixes of garlic cannot be detected at the same time through an existing method is filled up.

Description

technical field [0001] The invention relates to the technical field of pesticide residue detection, in particular to a method for detecting difenoconazole and azoxystrobin in garlic. Background technique [0002] Both difenoconazole and azoxystrobin belong to plant fungicides, which are often used in combination as compound pesticides, and are widely used in various crops to prevent and control various diseases. Nowadays, there are more and more reports on food safety problems caused by the abuse of fungicides. Both at home and abroad have formulated the maximum limit values ​​of difenoconazole and azoxystrobin for supervision. Among the detection methods of difenoconazole and azoxystrobin reported in the existing literature, gas chromatography and gas chromatography are more, and liquid chromatography and mass spectrometry are rarely reported. The quantitative limit of gas chromatography is relatively high, which cannot meet the requirements of trace analysis. The pretreat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/34G01N30/30G01N30/72G01N30/60G01N30/16G01N30/32G01N30/86
CPCG01N30/02G01N30/06G01N30/14G01N30/34G01N30/30G01N30/72G01N30/60G01N30/16G01N30/32G01N30/86G01N2030/062G01N2030/324
Inventor 王小明乔琳张辉周风达
Owner 安徽华辰检测技术研究院有限公司
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