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Detection method of pesticide residues in heart benefiting and pulse restoring particle

A granular and beneficial technology, applied in measuring devices, instruments, scientific instruments, etc., can solve problems such as pesticide residue detection not seen

Inactive Publication Date: 2017-07-04
TIANJIN TASLY PHARMA CO LTD
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  • Abstract
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  • Application Information

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Problems solved by technology

[0014] The detection of pesticide residues by gas chromatography tandem mass spectrometry mainly involves vegetables, fruits, single traditional Chinese medicines and soil, etc. The pretreatment of samples in this method includes the extraction and purification of samples. Most of the reagents are acetonitrile, ethyl acetate and acetone. So far, there has been no report on the detection of pesticide residues in traditional Chinese medicine compound preparations using this method.

Method used

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  • Detection method of pesticide residues in heart benefiting and pulse restoring particle
  • Detection method of pesticide residues in heart benefiting and pulse restoring particle
  • Detection method of pesticide residues in heart benefiting and pulse restoring particle

Examples

Experimental program
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Effect test

Embodiment 1

[0125] Embodiment 1 detects the method for 74 kinds of pesticide residues in Yixin Fumai Granules

[0126] 1. Preparation of the test solution

[0127] Accurately weigh 2.0 g of Yixin Fumai Granules into a 50 mL polyethylene centrifuge tube, add 10 mL of water to dissolve the sample completely. Add 20mL of n-hexane, vortex and mix well, put it into an ultrasonic instrument for ultrasonic extraction for 5min, add 4.0g sodium chloride and 3g sodium acetate, vortex mix, shake vigorously for 1min, and then centrifuge at 10000r / min for 5min. Accurately pipette 10.0mL supernatant into a 100mL round-bottomed flask, spin-evaporate in a water bath at 40°C until nearly dry, reconstitute with 2mL acetone, pipette 1.5mL of the extract into 50mg anhydrous magnesium sulfate, 50mg magnesium silicate and 50 mg C18 in a polyethylene centrifuge tube, vortexed to mix, and centrifuged at a rate of 12000r / min for 3min to obtain a supernatant;

[0128] 2. Preparation of matrix matching standard w...

Embodiment 2

[0145] The pesticide residue detection method of the 2015 edition of the Chinese Pharmacopoeia was adopted. For details, see the method for the determination of pesticide residues in the fourth general rule 2341 of the 2015 edition of the Chinese Pharmacopoeia—the fourth method of gas chromatography-tandem mass spectrometry to detect the samples in Example 1.

[0146] The research object of this method is medicinal materials or decoction pieces. After the samples are extracted with 1% glacial acetic acid-acetonitrile solution, N-propylethylenediamine, octadecyl bonded silica gel, silica gel and graphitized carbon black are used for impurity removal and purification. Final computer analysis.

[0147] The research object of the present invention is a compound Chinese medicine preparation——Yixin Fumai Granules. When 74 kinds of pesticide residues were detected by the method stipulated in the Pharmacopoeia, it was found that the extraction efficiency of some pesticides was not high...

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Abstract

The invention relates to a detection method of pesticide residues in a heart benefiting and pulse restoring particle. The method is gas chromatography-mass spectrography. The method comprises the following steps: preparing a sample solution, preparing a matrix matched standard working solution, and using a gas chromatograph-mass spectrograph to detect. The sample solution is prepared through the following steps: taking the heart benefiting and pulse restoring particle, adding water to dissolve the particle, adding n-hexane, carrying out ultrasonic extraction, adding sodium chloride and sodium acetate, uniformly mixing above substances, centrifuging the obtained mixture to obtain a supernatant, carrying out water-bath rotary evaporation until the supernatant is nearly dry, re-dissolving the nearly dry supernatant in acetone, adding the re-dissolved supernatant to anhydrous magnesium sulfate, a magnesium silicate adsorbent and C18, centrifuging the obtained solution, and taking the obtained supernatant.

Description

technical field [0001] The invention relates to a method for detecting pesticide residues in traditional Chinese medicine preparations, in particular to a method for detecting 74 kinds of pesticide residues in Yixin Fumai granules. Background technique [0002] The primary quality characteristic of a drug is safety. In addition to the influence of its own material base, the safety of traditional Chinese medicine is the foreign harmful substances introduced in the growth, processing, storage, production and other links, and the residual pesticide is one of them. The so-called pesticide residues refer to the parent pesticides and special derivatives with toxicological significance, such as degradation or transformation products and metabolites, which remain in the medicinal parts after being affected by the growth environment or after the use of pesticides in the process of planting, processing and storage of traditional Chinese medicines. and industrial impurities. Exogenou...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/88G01N30/02
CPCG01N30/06G01N30/02G01N30/88G01N2030/025
Inventor 佟玲孟文婷刘小勤张永志李东翔周水平
Owner TIANJIN TASLY PHARMA CO LTD
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