Method for treating pesticide residue sample in Chinese medicinal material before measurement

A treatment method and pesticide residue technology, which is applied in the field of determination of Chinese herbal medicines, can solve the problems of low degree of automation, low efficiency of extraction and purification, environmental pollution, etc.

Inactive Publication Date: 2010-10-06
CENT LAB TIANJIN ACADEMY OF AGRI SCI +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most analysis units in my country still use traditional solvent ext

Method used

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  • Method for treating pesticide residue sample in Chinese medicinal material before measurement
  • Method for treating pesticide residue sample in Chinese medicinal material before measurement
  • Method for treating pesticide residue sample in Chinese medicinal material before measurement

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] (1) Crush the coix seed sample, pass through a 60-mesh sieve, dry at 60°C, and store in a desiccator;

[0051] (2) Accurately weigh 3 samples of 2.0g Coix seed, one of which is added with 0.1ml of 60 kinds of pesticides mixed standard, and let stand for 10 minutes, then mix the sample with 1g of diatomaceous earth evenly, add a piece of fiber to the bottom of the 11ml extraction cell Prime filter membrane, and then load the mixed sample from the bottom for accelerated solvent extraction;

[0052] (3) Static extraction at a temperature of 100°C, acetone:n-hexane (1:9, v / v), and a pressure of 1500psi for 5 minutes, and extraction for 2 cycles;

[0053] (4) Wash the extraction tank with a solvent equivalent to 60% of the extraction tank, and finally purge it with nitrogen for 60s. Collect the extract, concentrate on a rotary evaporator to near dryness, blow nitrogen to dryness, add 2ml of acetonitrile to dissolve for purification.

[0054] (5) Purification: Weigh 0.2g PSA, 0.2g C...

Embodiment 2

[0056] (1) Crush the sample of Atractylodes japonicus, pass a 100-mesh sieve, dry at 80°C, and store in a desiccator;

[0057] (2) Accurately weigh 3 2.0g atractylodes samples, one of which is added with 0.1ml of 60 kinds of pesticide mixed standards, and let it stand for 10 minutes, then mix the sample with 1g diatomaceous earth evenly, and add a piece of cellulose at the bottom of the 11ml extraction cell Filter membrane, and then load the mixed sample from the bottom for accelerated solvent extraction;

[0058] (3) Static extraction for 10 minutes at a temperature of 100°C, acetone:n-hexane (1:9, v / v) and a pressure of 2000 psi, and extraction for 4 cycles;

[0059] (4) Wash the extraction tank with 75% solvent equivalent to the extraction tank, and finally purge it with nitrogen for 60s. The extract was collected, concentrated to near dryness on a rotary evaporator, nitrogen was blown to dryness, and 2ml of solvent (volume ratio of acetone to n-hexane 1:1) was added to dissolve ...

Embodiment 3

[0062] 1. Accelerated solvent extraction: accurately weigh out 3 2.0g ginseng samples, one of which is added with 0.1ml of 60 kinds of pesticide mixed standards, and let stand for 10 minutes, then mix the sample with 1.5g diatomaceous earth evenly, 11ml extraction cell at the bottom Add a piece of cellulose filter membrane, and then load the mixed sample from the bottom. Then perform accelerated solvent extraction. Static extraction is carried out at a temperature of 80°C, acetone:n-hexane (1:9, v / v), and a pressure of 2000psi for 8 minutes. The extraction is carried out for 3 cycles. The extraction tank is washed with a solvent equivalent to 70% of the extraction tank, and finally Purge with nitrogen for 60 s. The extract was collected, concentrated to near dryness on a rotary evaporator, nitrogen was blown to dryness, and 2ml of a mixed solvent of acetone and n-hexane (1:1) was added to dissolve it for purification.

[0063] Purification: Weigh 0.2g PSA, 0.2g C18, 0.3g anhydro...

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Abstract

The invention discloses a method for treating a pesticide residue sample in a Chinese medicinal material before measurement. The method comprises the following steps of: accurately weighing the treated Chinese medicinal material sample and uniformly mixing with diatomite; adding a cellulose filter membrane at the bottom of an extraction tank; charging the mixed sample from the bottom for accelerated solvent extraction; statically extracting for 5 minutes under the conditions that the temperature is 100 DEG C, the volume ratio of the acetone to the normal hexane is 1:9 (v/v) and the pressure is 1,500psi, and extracting for 2 circulations; collecting the extract, concentrating to nearly dry, and blowing nitrogen to dry; adding the mixed solution of the acetone and normal hexane or an acetonitrile organic solvent for dissolving; and performing purification treatment to obtain supernatant, and fixing the volume for later measurement. Due to the adoption of the technology of accelerated solvent extraction, the method has the advantages of short detection flow, convenient operation, recovery rate of 70 to 110 percent, and high sensitivity, can detect 60 pesticide residues in the medicinal material simultaneously, and has good application prospects.

Description

Technical field [0001] The invention belongs to the technical field of determination of Chinese medicinal materials, and relates to a method for rapid detection of pesticide residues in samples of Chinese medicinal materials. More specifically, it uses accelerated solvent extraction to pre-treat samples of 60 pesticides in Chinese herbal medicines. Background technique [0002] With the continuous development of traditional Chinese medicine, the role of traditional Chinese medicine and its preparations in disease prevention and treatment worldwide has been re-recognized, the inherent quality of traditional Chinese medicine preparations has been improved, and the control of pesticide residues in traditional Chinese medicines is very necessary to formulate reasonable quality control standards. As we all know, Chinese medicinal materials are special products for disease prevention, treatment and health care. The Chinese medicinal materials that people take should first be non-toxic ...

Claims

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Application Information

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IPC IPC(8): G01N1/34B01D11/02G01N30/06G01N30/02
Inventor 郭永泽程奕张玉婷刘磊邵辉李辉宋淑荣
Owner CENT LAB TIANJIN ACADEMY OF AGRI SCI
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