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Method for determining residual amount of thiediazole copper in dendrobium officinale

A technology of Dendrobium officinale and an analytical method, applied in the field of analysis of thiophanate copper residues in Dendrobium officinale, can solve the problems of matrix interference, unsatisfactory purification effect, low sensitivity and the like, and achieves less impurity interference, avoiding matrix interference, and recovery rate. high effect

Active Publication Date: 2018-06-08
ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the complex matrix of Dendrobium officinale, the high-efficiency liquid phase method is used for detection, the purification effect is not ideal, the matrix interference is serious, and the sensitivity is low. It is impossible to use the liquid phase method to accurately measure the residual amount of thiobacterium copper in Dendrobium candidum. It is necessary to develop a more effective detection method. method

Method used

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  • Method for determining residual amount of thiediazole copper in dendrobium officinale
  • Method for determining residual amount of thiediazole copper in dendrobium officinale
  • Method for determining residual amount of thiediazole copper in dendrobium officinale

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Embodiment 1

[0046] (1) Derivation: Weigh 5 g of Dendrobium officinale sample, put it in a stoppered Erlenmeyer flask, add 20 mL of 0.1 mol / L sodium sulfide solution, heat to 30°C, and shake for 30 minutes;

[0047] (2) Extraction: add 20 mL of acetonitrile, shake at room temperature for 1 hour, filter with suction after shaking, and use 1 mol / L H 2 SO 4 Adjust the pH to 4-5;

[0048](3) Extraction: Transfer the above solution to a separatory funnel, add 50 mL of ethyl acetate for extraction, take the upper organic phase, dry over anhydrous sodium sulfate, filter, and concentrate the filtrate to near-dryness under reduced pressure in a constant temperature water bath at 40 °C, add 2.0 mL of petroleum ether: acetone (1:1, v:v) dissolved, to be purified;

[0049] (4) Purification: take Florisil solid-phase column, activate with petroleum ether, take the above-mentioned extract to be purified and load it, elute with petroleum ether: acetone (1:1, v:v), collect eluent, reduce Concentrate un...

Embodiment 2

[0053] (1) Derivation: Weigh 10 g of Dendrobium officinale sample, put it in a stoppered Erlenmeyer flask, add 60 mL of 0.1mol / L sodium sulfide solution, heat to 60°C, and shake for 30 minutes;

[0054] (2) Extraction: add 60 mL of acetonitrile, shake at room temperature for 2 hours, filter with suction after shaking, and use 1 mol / L H 2 SO 4 Adjust the pH to 4-5;

[0055] (3) Extraction: Transfer the above solution to a separatory funnel, add 100 mL of ethyl acetate for extraction, take the upper organic phase, dry over anhydrous sodium sulfate, filter, and concentrate the filtrate to near-dryness under reduced pressure in a constant temperature water bath at 40 °C, add 2.0 mL of petroleum ether: acetone (1:1, v:v) dissolved, to be purified;

[0056] (4) Purification: take Florisil solid-phase column, activate with petroleum ether, take the above-mentioned extract to be purified and load it, elute with petroleum ether: acetone (1:1, v:v), collect eluent, reduce Concentrate...

Embodiment 3

[0060] (1) Derivation: Weigh 7.5 g of Dendrobium officinale sample, put it in a stoppered Erlenmeyer flask, add 20-60 mL of 0.1mol / L sodium sulfide solution, heat to 40°C and shake for 30 minutes;

[0061] (2) Extraction: Add 40 mL of acetonitrile, shake at room temperature for 1.5 hours, filter with suction after shaking, and use 1 mol / L H for the filtrate 2 SO 4 Adjust the pH to 4-5;

[0062] (3) Extraction: Transfer the above solution to a separatory funnel, add 70 mL of ethyl acetate for extraction, take the upper organic phase, dry over anhydrous sodium sulfate, filter, and concentrate the filtrate to near-dryness under reduced pressure in a constant temperature water bath at 40 °C, add 2.0 mL of petroleum ether: acetone (1:1, v:v) dissolved, to be purified;

[0063] (4) Purification: take Florisil solid-phase column, activate with petroleum ether, take the above-mentioned extract to be purified and load it, elute with petroleum ether: acetone (1:1, v:v), collect eluent...

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Abstract

The invention provides a method for determining the residual amount of thiediazole copper in dendrobium officinale. The method comprises adding a sodium sulfide solution into a dendrobium officinale sample so that the thiediazole copper is derived and transformed into a metabolite thiadiazole, carrying out extraction with acetonitrile, adding an acid into the extract to adjust pH, adding ethyl acetate into the extract, carrying out liquid-liquid distribution, carrying out concentration drying through an organic phase through a rotary evaporator, removing interfering substances in the extract through a solid phase extraction method and carrying out detection through an ultra-high performance liquid chromatography-mass spectrometer / mass spectrometer. The method can effectively prevent samplematrix interference and has good results. The method has high accuracy, precision and sensitivity, has a high recovery rate and small interference of impurities and can effectively determine the content of thiediazole copper in the dendrobium candidum.

Description

technical field [0001] The invention belongs to the technical field of determination of pesticide residues, and in particular relates to an analysis method for the residual amount of thiabactin in dendrobium officinale. Background technique [0002] Thiobacterium copper is a patented product developed by Zhejiang Longwan Chemical Co., Ltd. Its chemical name is 2-amino-5-mercapto-1, 3, 4-thiadiazole copper complex, and its main metabolite is thiadiazole. It is a highly effective Broad-spectrum systemic fungicide. The bactericidal mechanism is unique, not only the unique effect of thiazole group on bacteria, but also the control effect of copper ions on fungi and bacteria. It can be widely used in the prevention and control of more than 60 kinds of bacterial and fungal diseases in more than 20 kinds of crops. At present, it has been applied to the control of soft rot, leaf spot, bacterial blight and other diseases on Chinese cabbage, tomato, citrus, cucumber, rice, watermelon...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/047G01N2030/062
Inventor 俞建忠许振岚何红梅吴珉张春荣何开雨张昌朋朱亚红胡秀卿赵华
Owner ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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