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Method for detecting pesticide residue in white paeony root crude drug

A technology for pesticide residues and peony materials is applied to the field of simultaneous detection of 23 kinds of pesticide residues in white peony materials, which can solve the problems of large environmental pollution, time-consuming impurities, poor universality, etc., and achieve simple sample processing, good repeatability, Universal effect

Inactive Publication Date: 2011-09-14
ZHEJIANG UNIV
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  • Description
  • Claims
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Problems solved by technology

Solid-phase extraction technology requires a large amount of solvent for column activation and elution, which causes great environmental pollution, is time-consuming and has many impurities, and the recovery rate of pesticides is not high
In addition, the existing methods for the analysis of pesticide residues in Radix Paeoniae Alba are mainly gas chromatography-electron capture detection or gas chromatography-flame photometry, and gas chromatography is not suitable for the detection of non-volatile and thermally unstable pesticides.
Moreover, the existing method only detects organochlorine and organophosphorus pesticides, which is not universally applicable

Method used

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  • Method for detecting pesticide residue in white paeony root crude drug
  • Method for detecting pesticide residue in white paeony root crude drug
  • Method for detecting pesticide residue in white paeony root crude drug

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Experimental program
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Effect test

Embodiment 1

[0018] 23 organochlorine, organophosphorus and organonitrogen pesticides were analyzed by liquid chromatography-mass spectrometry.

[0019] Preparation of standard solution: Take an appropriate amount of each pesticide standard, weigh it accurately, and dissolve it in methanol. As a standard stock solution. Low concentration standard solutions were obtained by diluting the stock solutions with an appropriate amount of methanol.

[0020] Liquid chromatography conditions: Agilent ZORBAX SB-C18 (4.6 mm × 250 mm, 5 μm); mobile phase A: 20% methanol-water solution containing 5 mmol / L ammonium formate, mobile phase B: containing 5 mmol / L ammonium formate methanol solution, the elution procedure is as follows: 0-5 min, 26%B~52%B; 5~15 min, 52%B~70%B; 15~45 min, 70%B~83%B; 45~ 46 min, 83% B ~ 100% B; 46 ~ 65 min, 100% B; analysis time 65 min, equilibration time 20 min. Flow rate: 0.5 mL / min, column temperature: 20 ℃, injection volume: 20 μL.

[0021] Mass spectrometry conditions: ...

Embodiment 2

[0026] The medicinal materials of Radix Paeoniae Alba added with 23 kinds of pesticides were analyzed by liquid chromatography-mass spectrometry.

[0027] Sample pretreatment: crush the Radix Paeoniae Alba sample, pass it through a sieve with a pore size of 200 μm, take 5.0 g of Radix Paeoniae Alba sample powder, accurately weigh it in a 50 mL Corning polypropylene centrifuge tube, add 0.5 mL of the mixed reference solution, and then add 20 Mix mL of acetonitrile by vortexing for 1 min, let stand for 20 min, centrifuge at 4000 r / min for 10 min at 20°C, and take the supernatant; add 10 mL of acetonitrile to the centrifuge tube, and repeat the above operation once. Combine the two extracts, add 60 mg PSA and 180 mg anhydrous magnesium sulfate, vortex mix for 1 min, centrifuge at 4000 r / min at 20 °C for 10 min, take the supernatant, and evaporate to dryness with a rotary evaporator at 40 °C , the residue was precisely dissolved in 0.5 mL of methanol, centrifuged, and the supernat...

Embodiment 3

[0030] Application of liquid chromatography-mass spectrometry for the analysis of Radix Paeoniae Alba.

[0031] Sample pretreatment: Pulverize the Radix Paeoniae Alba sample, pass it through a sieve with a pore size of 200 μm, take 5.0 g of Radix Paeoniae Alba sample powder, accurately weigh it in a 50 mL Corning polypropylene centrifuge tube, add 20 mL of acetonitrile, and vortex mix for 1 min. Let stand for 20 minutes, centrifuge at 4000 r / min at 20°C for 10 minutes, and take the supernatant; then add 10 mL of acetonitrile to the centrifuge tube, and repeat the above operation once. Combine the two extracts, add 60 mg PSA and 180 mg anhydrous magnesium sulfate, vortex mix for 1 min, centrifuge at 4000 r / min at 20 °C for 10 min, take the supernatant, and evaporate to dryness with a rotary evaporator at 40 °C , the residue was precisely dissolved by adding 0.5 mL of methanol, centrifuged, and the supernatant was collected for later use.

[0032] Sample analysis: the same chro...

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Abstract

The invention provides a method for detecting pesticide residue in a white paeony root crude drug, comprising the following steps of: extracting powder of the white paeony root crude drug with acetonitril in oscillation, then, performing dispersed purification by using N-propyl ethylene diamine as a dispersion purifying agent and using anhydrous magnesium sulfate as a drying agent; evaporating solvent of the extract to dry at 40 DEG C in a rotary evaporators; and taking liquid chromatogram as a separation means and taking mass spectrum as a detection means after dissolving the residual again. The method provided by the invention can simultaneously detect 23 kinds of pesticide residues of organic chloride, organic phosphor and organic nitrogen types. By using the method provided by the invention to analyze the pesticide residue in the white paeony root crude drug, the sample is simply and conveniently processed, rate of recovery is high, and universality is high, so that the method has better application prospect.

Description

technical field [0001] The invention belongs to the technical field of limited detection of harmful substances in traditional Chinese medicinal materials, and relates to a method for detecting pesticide residues in samples of traditional Chinese medicinal materials, in particular to a method for simultaneously detecting 23 kinds of pesticide residues in white peony medicinal materials. Background technique [0002] The problem of drug safety is directly related to people's livelihood. In order to reduce the amount of pesticide residues in Chinese medicinal materials and improve the competitiveness of Chinese traditional medicine products in the international market, the detection and analysis of pesticide residues is a very important part. Radix Paeoniae Alba is a commonly used traditional Chinese medicine in my country, and it is necessary to detect and analyze pesticide residues in it. Currently, the commonly used pretreatment techniques for Radix Paeoniae Alba samples are ...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 王书芳李云飞邵青程翼宇
Owner ZHEJIANG UNIV
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