Method for detecting residual amount of 19 organochlorine pesticides in pseudo-ginseng

A technique for organochlorine and pesticide residues, which is applied in the field of simultaneous determination of 19 organochlorine pesticide residues in Panax notoginseng, which can solve the problems of high requirements for testing personnel, complicated preparation, and long testing time.

Active Publication Date: 2018-05-22
TIANJIN TASLY PHARMA CO LTD
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  • Description
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  • Application Information

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Problems solved by technology

The above methods are cumbersome to prepare samples, take a long time to test, use more toxic reagents such as dichloromethane, etc., column chromatography needs to be filled and processed, and require high testing personnel. These are not suitable for daily production testing.

Method used

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  • Method for detecting residual amount of 19 organochlorine pesticides in pseudo-ginseng
  • Method for detecting residual amount of 19 organochlorine pesticides in pseudo-ginseng
  • Method for detecting residual amount of 19 organochlorine pesticides in pseudo-ginseng

Examples

Experimental program
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Effect test

Embodiment 1

[0061] A method for simultaneously measuring 19 kinds of organochlorine pesticide residues in Panax notoginseng, comprising the steps of:

[0062] (1) Preparation of the test solution:

[0063] Take 1 portion of medicinal material powder, weigh it accurately, put it in a 50mL polypropylene plastic centrifuge tube, add petroleum ether 30 times the weight of the medicinal material, soak for 1 hour, filter with suction, wash the residue with petroleum ether 15 times the weight of the medicinal material, and transfer it to a 100mL circular tube. In a bottom flask, evaporate to nearly dryness in a water bath at 40°C. Reconstitute with 2 mL of n-hexane, transfer to a centrifuge tube, add 0.1 mL of concentrated sulfuric acid, shake fully for 1 min, after the reaction is complete, centrifuge at 3000 r / min for 5 min, take the supernatant, and put it into GC for testing.

[0064] (2) Preparation of mixed reference substance solution:

[0065] Precisely measure 1mL of each of the 19 ki...

Embodiment 2

[0071] According to the method of Example 1, 30 batches of Panax notoginseng medicinal materials produced in Yunnan were tested. The test results are shown in Table 4. Among them, the maximum residual amount of pentachloronitrobenzene is 0.32 mg / kg, which exceeds the limit stipulated in the 2015 edition of the Chinese Pharmacopoeia, and the remaining pesticide residues are not found to exceed the standard.

[0072] Table 4 Test result table

[0073] Tab.4 Test results

[0074]

[0075]

[0076] (Note: "-" means not detected, "+" means detected, "++" means exceeded).

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Abstract

The invention relates to a method for detecting the residual amount of 19 organochlorine pesticides in pseudo-ginseng. The method includes the following steps: (1) preparation of a test sample solution: taking a medicinal material powder, adding petroleum ether, soaking, carrying out suction filtration, carrying out fractionated washing of the residue with petroleum ether, transferring to a round-bottom flask, carrying out water bath rotary steaming at the temperature of 25-45 DEG C to be nearly dry, re-dissolving with n-hexane, adding concentrated sulfuric acid, fully jerking, after completion of the reaction, centrifuging, and taking a supernatant for standby application; (2) preparation of a mixed reference substance solution: taking 19 pesticide standard substances, placing in volumetric flasks, adding n-hexane to dilute to the scale, to obtain reserve liquids of the reference substances, respectively weighing the reserve liquids of the reference substances in a volumetric flask, diluting with n-hexane to the scale, and thus obtaining the mixed reference substance solution; and (3) detecting method: taking the test sample solution and the mixed reference substance solution, injecting into a gas chromatograph, and detecting.

Description

Technical field: [0001] The invention relates to a method for detecting pesticide residues in traditional Chinese medicines, in particular to a method for simultaneously measuring 19 kinds of organochlorine pesticide residues in Panax notoginseng. Background technique: [0002] The use of pesticides has brought great contributions to human life, and at the same time, the abuse of pesticides has also caused certain harm to human organisms. At present, with the continuous deepening of the standardized planting of Chinese medicinal materials, the problem of pesticide residues in medicinal materials has attracted more and more attention from scholars all over the world. Organochlorine pesticides were widely used in the cultivation of traditional Chinese medicine, but due to their long half-life, slow degradation, and stable chemical properties, their use was banned in the 1980s in my country, but the residual components can still be detected from water, soil, and plants. . If p...

Claims

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Application Information

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IPC IPC(8): G01N30/06
CPCG01N30/06
Inventor 李云飞佟玲李东翔段玺玉李爽
Owner TIANJIN TASLY PHARMA CO LTD
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