Method for measuring residual quantity of organic chloride pesticides in traditional Chinese medicinal materials

A technology for pesticide residues and determination methods, which is applied in the field of determination of Chinese medicinal materials, can solve the problems of few types of residues, low efficiency, ineffective aliphatic compounds, etc., and achieves the effect of high sensitivity

Inactive Publication Date: 2014-12-03
INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

At present, the pretreatment of these documents or standard methods is mainly based on concentrated sulfuric acid sulfonation, and there are few types of organochlorine pesticide residues at one time, mainly for the detection of HCH, DDT and pentachloronitrobenzene. There are certain safety risks for personnel, and the efficiency is low; in addition, pesticides using cyclopentadiene as raw materials, such as chlordane, heptachlor, endosulfan, etc., generally cannot be sulfonated with sulfur trioxide or its hydrate, which will produce certain loss; aliphatic compounds are either inactive or oxidatively decompose fatty compounds, resulting in complex mixtures

Method used

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  • Method for measuring residual quantity of organic chloride pesticides in traditional Chinese medicinal materials
  • Method for measuring residual quantity of organic chloride pesticides in traditional Chinese medicinal materials
  • Method for measuring residual quantity of organic chloride pesticides in traditional Chinese medicinal materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Embodiment 1: the selection of extraction solvent

[0061] Take the powder of Chinese medicinal materials in a 50mL centrifuge tube, add a certain concentration of standard solution, add deionized water to soak for 20min, and add the extract to extract.

[0062] In this example, according to the characteristics of organochlorine pesticides, a one-component solvent extraction experiment was first carried out, and 25 mL of petroleum ether, n-hexane, ethyl acetate and acetone were used for extraction respectively. The experimental results are shown in Table 1, and Table 1 shows the recovery rate results of 17 kinds of organochlorine pesticides extracted by one-component solvent.

[0063] Table 1

[0064] extraction solvent

[0065] The test results showed that the recoveries of 17 kinds of organochlorine pesticides in four extraction solvents were between 60%-70%, 30%-40%, 50%-80%, and 110%-140%, respectively. According to the experimental results, it can be se...

Embodiment 2

[0073] Embodiment 2: Effect experiment of GPC purification

[0074] There are many kinds of Chinese herbal medicines, and the matrix composition of all kinds of Chinese herbal medicines is complex; therefore, purification is a very critical step for the detection of pesticide residues in Chinese herbal medicines. GPC is to remove macromolecular lipids, pigments and other matrix impurities in the extract of Chinese herbal medicines through the molecular weight difference between the target compound and impurities.

[0075] Gel permeation chromatography (GPC) conditions are as follows:

[0076] Gel chromatography purification column: 300mm×25mm(i.d);

[0077] Filler: Bio-Beads, S-X3, 38μm~75μm;

[0078] Concentration temperature: 45°C;

[0079] Mobile phase: cyclohexane-ethyl acetate (50+50, volume ratio);

[0080] Volumetric reagent: 8:2 n-hexane: acetone solution;

[0081] Flow rate: 5mL / min;

[0082] Injection volume: 5.0 mL.

[0083] Through the segmented collection o...

Embodiment 3

[0084] Embodiment 3: the selection of solid-phase extraction column (SPE) type and eluent amount

[0085] Since Chinese herbal medicines contain many and complex chemical components, GPC purification alone cannot meet the requirements of computer determination; therefore, other purification techniques such as solid-phase extraction technology are still needed for further purification. According to the characteristics of organochlorine pesticides, a single column was first selected for purification, and graphitized carbon black solid phase extraction column (GCB SPE, 250mg / 3mL) and aminopropyl column solid phase extraction (NH 2 SPE, 200mg / 3mL), Florisil solid phase extraction column (Florisil SPE, 1.5g / 3mL), neutral alumina solid phase extraction column (Al 2 o 3 SPE, 2.0g / 3mL) for purification. Using 10mL n-hexane + acetone (8:2), the elution curve of 50ng / mL organochlorine pesticide standard was studied.

[0086] The experimental results are shown in Table 4. Table 4 is g...

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Abstract

The invention provides a method for measuring residual quantity of organic chloride pesticides in traditional Chinese medicinal materials. A GPC-SPE-GC method is established, and the residual quantity of seventeen organic chloride pesticides in traditional Chinese medicinal materials is detected. The method comprises the following steps: extracting, performing preliminary GPC purification, performing solid phase extraction and binary purification, namely combining 200mg/3mL of aminopropyl column NH2SPE and 250mg/3mL of graphitized carbon black column GCB SPE, and sequentially purifying; and eluting according to a volume ratio of 8:2 of normal hexane to acetone solution. Compared with a traditional concentrated sulfuric acid purification method, the method disclosed by the invention has high sensitivity and safety, provides reliable detection means for safety production of traditional Chinese medicinal materials in China and safety supervision of exported foods and drugs and is worthy of popularization and application.

Description

technical field [0001] The invention belongs to the technical field of determination of Chinese medicinal materials, and relates to a method for determining the residual amount of organochlorine pesticides in Chinese medicinal materials, more specifically, it relates to the determination of 17 residual amounts of organochlorine pesticides in Chinese medicinal materials by using the GPC-SPE-GC method . Background technique [0002] Organochlorine pesticides are organic compounds containing organochlorine elements, which play an important role in the prevention and control of plant diseases and insect pests. They are a type of organic synthetic pesticides with the largest production volume and the most widely used area in agriculture so far. It has a series of characteristics such as low vapor pressure, low volatility, strong fat solubility and stable structure, and is not easy to be degraded by enzymes in vivo. Long-term use will cause environmental pollution and accumulate t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/08
Inventor 谢建军何曼莉陈捷陈文锐
Owner INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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